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BIOCHEMISTRY RESEARCH TRENDS

GAS CHROMATOGRAPHY
ANALYSIS, METHODS
AND PRACTICES

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contained herein. This digital document is sold with the clear understanding that the publisher is not engaged in
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GAS CHROMATOGRAPHY
ANALYSIS, METHODS
AND PRACTICES

VALERIE WARREN
EDITOR

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Published by Nova Science Publishers, Inc. † New York

Preface vii
Chapter 1 An Analysis of Toxic Alkaloids
of Forensic Interest via Gas Chromatography 1
Ana Claudia Fernandes Amaral,
Aline de Souza Ramos, José Luiz Pinto Ferreira,
Maria Athana Mpalantinos da Silva,
Vinicius Vaz Cabral Nery,
Thamiris de Almeida de Souza,
Igor de Almeida Rodrigues,
Francimilton Rabelo Rodrigues and
Jefferson Rocha de Andrade Silva
Chapter 2 The Influence of Surfactant Monolayer(s)
on the Evaporation of Liquid Pollutants,
Studied by Reverse-Flow Gas Chromatography 45
H. H. Mohammad, Rashid Atta Khan
and Khalisanni Khalid
Chapter 3 The Application of Headspace: Solid-Phase
Microextraction (HS-SPME) Coupled with
Gas Chromatography/Mass Spectrometry
(GC/MS) for the Characterization of Polymers 69
Peter Kusch

Chapter 4 Sampling of the Postmortem Specimen

for the Analysis of Volatile or Gaseous
Substances in Forensic Practice 105
Hiroshi Kinoshita, Naoko Tanaka, Ayaka Takakura,
Mostofa Jamal, Asuka Ito, Mitsuru Kumihashi,
Shoji Kimura, Kunihiko Tsutsui, Shuji Matsubara
and Kiyoshi Ameno
Bibliography 121
Related Nova Publications 191
Index 197

Many members of plant and fungi kingdoms have toxic alkaloids that
are highly poisonous. Chapter One explores how gas chromatography is
used to analyze some classes of these alkaloids. In Chapter Two, the
effect of surfactants on gas-liquid interfaces by using reverse-flow gas
chromatography (RF-GC). Chapter Three describes the application of Solid-
Phase Microextraction (SPME) for identifying volatile organic compounds
(VOCs), additives and degradation products in industrial plastics, rubber, and
packaging materials. And in Chapter Four, the authors discuss sampling
procedures for the analysis of volatile and gaseous substances used in daily life
and in forensic medicine.
Chapter 1 - Many members of plant and fungi kingdoms have toxic
alkaloids highly poisonous. One of the most frequent forms of poisoning is by
ingestion but can be also by contact, absorption and inhalation with these
toxins. The toxic alkaloids belong to the class of pyrrolizidine, piperidine,
tropane and others. Analysis of these toxic compounds may be realized by
some chromatographic techniques to help a rapid and efficient diagnosis of a
possible poisoning, for example. Gas chromatography is commonly used as
choice technique to analyze some class of alkaloids and that fact will be
explored in this chapter together with other related topics.
Chapter 2 - Reverse-flow gas chromatography (RF-GC) was been utilized
to compare the effect of Triton-X monolayer(s) on the evaporation of
methanol and ethanol. Evaporation rates and diffusion coefficients for the
respective liquid pollutants have been determined at 333.15 K in nitrogen.
The precision and accuracy of the method has confirmed the presented
methodology as suitable to be used in studying the retardation effect of
surfactants on the evaporation rates of volatile organic liquids. The

evaporation rates has been compared successfully with the available published
literature values, while the diffusion coefficients with compare well with
Fuller-Schettler-Giddings, affirming the validity of the presented
methodhology. The suppressing of the evaporation rates of methanol and
ethanol become significant (>40%) at amounts of surfactant corresponding to
more than two monolayers. The reduction of the evaporation rate of the
studied liquids is due to the formation of densely packed surface monolayers
or to the formation of an insoluble monolayer.
Chapter 3 - Solid-Phase Microextraction (SPME) is a very simple and
efficient, solventless sample preparation method, invented by Pawliszyn and
co-workers at the University of Waterloo (Canada) in 1989. This method has
been widely used in different fields of analytical chemistry since its first
applications to environmental and food analysis. SPME integrates sampling,
extraction, concentration and sample introduction into a single solvent-free
step. The method saves preparation time, disposal costs and can improve
detection limits. It has been routinely used in combination with gas
chromatography (GC) and gas chromatography/mass spectrometry (GC/MS)
and successfully applied to a wide variety of compounds, especially
for the extraction of volatile and semi-volatile organic compounds from
environmental, biological and food samples.
Since the last twenty years, SPME in headspace (HS) mode is used as a
valuable sample preparation technique for identifying degradation products in
polymers and for determination of rest monomers and other light-boiling
substances in polymeric materials. For more than ten years, the authors’
laboratory has been involved in projects focused on the application of HS-
SPME-GC/MS for the characterization of polymeric materials from many
branches of manufacturing and building industries. This book chapter
describes the application examples of this technique for identifying volatile
organic compounds (VOCs), additives and degradation products in industrial
plastics, rubber, and packaging materials.
Chapter 4 - Postmortem samples for toxicological examination are
routinely collected at forensic autopsy. Usually the authors collected various
biological specimens such as blood, urine, stomach contents, cerebrospinal
fluid or tissues (brain, liver, lung, kidney, muscle). The analysis of volatile and
gaseous chemical compounds in those biological samples is commonly
performed by the gas chromatography (GC) and gas chromatography-mass
spectrometry (GC/MS) in combination with head-space (HS) method. The HS
method has some advantages such as simple procedure, less time consuming
and without contamination of non-volatile component in the sample matrix.

The HS-GC or HS-GC/MS is useful not only for the quantification of volatile
and gaseous chemicals, but also for the screening of industrial products
containing volatiles used as solvents.
In the present paper, the authors discuss about the routine and additional
sampling procedure for analysis of volatile and gaseous substances used in
daily life in forensic medicine.

EBSCO Publishing : eBook Collection (EBSCOhost) - printed on 10/3/2018 2:19 PM via UNIVERSIDAD DE
ANTIOQUIA
AN: 1540094 ; Warren, Valerie.; Gas Chromatography : Analysis, Methods and Practices
Account: s1175444
In: Gas Chromatography ISBN: 978-1-53611-990-9
Editor: Valerie Warren © 2017 Nova Science Publishers, Inc.

Chapter 1

AN ANALYSIS OF TOXIC ALKALOIDS OF

FORENSIC INTEREST VIA
GAS CHROMATOGRAPHY

Ana Claudia Fernandes Amaral1,*,

Aline de Souza Ramos1, José Luiz Pinto Ferreira1,
Maria Athana Mpalantinos da Silva1,
Vinicius Vaz Cabral Nery2,
Thamiris de Almeida de Souza1,
Igor de Almeida Rodrigues3,
Francimilton Rabelo Rodrigues4
and Jefferson Rocha de Andrade Silva4
1
Laboratory of Medicinal Plants and Derivatives, PN1, Department of
Natural Products, Farmanguinhos, FIOCRUZ, Manguinhos, RJ, Brazil
2
Laboratory of Mass Spectromettry, PMA, Farmanguinhos, FIOCRUZ,
Manguinhos, RJ, Brazil
3
Laboratory of Antimicrobial Prospection, Department of Natural Products
and Food, School of Pharmacy, UFRJ, Rio de Janeiro, RJ, Brazil
4
Laboratory of Chromatography, Department of Chemistry, UFAM,
Setor Sul, Japiim, Manaus, AM, Brazil

*
Corresponding Author address. Email: [email protected]; [email protected].

ABSTRACT
Many members of plant and fungi kingdoms have toxic alkaloids
highly poisonous. One of the most frequent forms of poisoning is by
ingestion but can be also by contact, absorption and inhalation with these
toxins. The toxic alkaloids belong to the class of pyrrolizidine, piperidine,
tropane and others. Analysis of these toxic compounds may be realized
by some chromatographic techniques to help a rapid and efficient
diagnosis of a possible poisoning, for example. Gas chromatography is
commonly used as choice technique to analyze some class of alkaloids
and that fact will be explored in this chapter together with other related
topics.

Keywords: alkaloid, gas chromatography, poisoning, mass fragmentogram,

biological sample

INTRODUCTION
Gas chromatography (GC) is one of the most applied techniques in
analytical chemistry for separation, identification and quantification of
different kind of samples from many areas, such as food, flavors, natural
products, environmental, forensics and others. There are different reports of
poisonings with alkaloids and the analyzed samples by GC are mainly from
animals and humans (body fluids and tissues), plant (extracts, medicines,
wrong botanical identification) and food (contamination). The types of
detectors commonly used, alone or combined; in the analyses of toxic
alkaloids are flame ionization (FID), nitrogen-phosphorus (NPD), alkali-flame
(AFD) or alkali flame ionization (AFID), and mass spectrometer (MS).
Alkaloids represent the largest group of secondary metabolites that
contain one or several nitrogen atoms. Depending on the ring structures, they
are subdivided into pyrrolidine, acridone, steroid alkaloids, quinolizidine,
monoterpene indole, protoberberine, aporphine, morphinane, quinoline,
piperidine, indole, isoquinoline, diterpene, and pyrrolizidine. Intoxication
linked to wrong ingestion, homicide, suicide and poisoning due to abuse for
hallucinogenic reasons with alkaloids of the last five classes have been
analyzed by GC. In this context, the chapter describes the application of the
GC technique in analyses of some toxic alkaloids.

SOURCE OF TOXIC ALKALOIDS

Alkaloids are widely distributed in the plant kingdom (Angiosperms),
especially in the botanical families Lauraceae, Annonaceae, Ranunculaceae,
Solanaceae, Apocynaceae, Menispermaceae, Rutaceae, Magnoliaceae,
Loganiaceae, Rubiaceae, Papaveraceae and Fumariaceae. On the other hand,
in bacteria they are extremely rare, and in fungi they are relatively rare. In
Pteridophytes they are also very scarce, mainly occurring in Lycopodiales and
Equisetales. Similarly, plants belonging to the Gymnosperm division are rare
in this group of natural products, occurring mainly in the Taxales and Gnetales
orders [1].
The most commonly cited alkaloids with severe toxic effects are those
containing pyrrolizidine, indole, diterpene, isoquinoline and steroid nucleus,
covering mainly the Fabaceae, Asteraceae, Ranunculaceae, Boraginaceae,
Papaveraceae and Apiaceae families. These families are related to some
natural sources of alkaloids that have high toxicity when accidentally ingested
by man, whether as food, or by overdosage in therapeutic use, or deliberately,
e.g., criminal intent or for suicidal purposes. Many of these botanical sources
also cause severe economic losses due to poisoning of animals, particularly
beef cattle or dairy cattle [1].
In this context, in relation to the botanical genera and alkaloids, it is worth
emphasizing:
Lupinus (lupanine, 5,6-dehydrolupanine, ammodendrine, anagyrine) [2];
Aconitum (aconitine, hypaconitine, mesaconitine, yunaconitine, crassicauline
A) [3, 4]; Symphytum (echimidine, symphytine, lycopsamine) [5, 6]; Senecio
(senkirkine, integerrimine, platyphylline, retrorsine, riddeline, sarracine,
senecionine, seneciphylline, otosenine) [7-9]; Crotalaria (monocrotaline,
fulvine) [10]; Nicotiana (nicotine, anabasine) [11], Narcissus (galanthamine,
haemanthamine, lycorine) [12, 13]; Eupatorium (lycopsamine, echinatine)
[14]; Conium (coniine, gamma-coniceine) [15]; Sanguinaria (chelerythrine)
[16]; Strychnos (strychnine, brucine) [17]; Colchicum (colchicine) [18];
Psychotria (N,N-dimethyltryptamine, 5-methoxydimethyltryptamine) [19, 20];
Physostigma (eserine) [21]; Banisteriopsis (harmine, harmaline) [18];
Heliotropium (heliotridine esters, lasiocarpine) [22, 23]; Tabernanthe
(ibogaine) [24]; Rauwolfia (reserpine) [25]; Pausinystalia (yoimbine) [26].

TOXICITY EFFECTS
Cases of poisoning by alkaloids are common, as toxic alkaloids are
present in a wide diversity of plant species, including those used as traditional
remedies or even as food. The pyrrolizidine alkaloids (PAs) are known
mainly for its hepatotoxic effects in humans, which may lead to serious
hepatic conditions such as hepatic sinusoidal obstruction syndrome [27]. Since
most pyrrolizidine alkaloid bioactivation occurs in the liver, there is a
consensus that the formation of pyrrole-protein adducts are responsible for the
hepatotoxic affects. However, it is worth mentioning that only pyrrolizidine
alkaloids with an unsaturated necine base (retronecine-type and otonecine-
type) undergo metabolic activation to generate pyrrole-protein adducts
associated with toxicity [28].
Interestingly, it has been demonstrated that hepatocyte cytochromes P450
play a critical role in the extrahepatic toxic effects of the dehydropyrrolizidine
alkaloids generated. Dehydromonocrotaline (DHM) is the activated form of
monocrotaline (PA) responsible for the toxic effects observed in multiple
organs, including the liver, lung and kidney [29]. In addition, even at the non-
cytotoxic dose (100μM), heliotrine, echimidine, senkirkine and senecionine
are able to induce changes in human hepatocyte gene expression, including
those responsible for cytochrome P450 expression. The up- and
downregulation of these genes provided strong evidence that PAs might
interfere in their own uptake, distribution, metabolism and excretion [30].
Despite the use of plants belonging to the Aconitum genus in traditional
Eastern medicine, the diester-diterpenoid alkaloid content of these plants can
lead to serious health problems or even death. Among the toxic alkaloids
present in this genus, aconitine has been described as the most toxic one,
affecting neural cells and cardiac tissue. The toxicity of this alkaloid has been
attributed to its ability to bind to the neurotoxin binding site 2 of the Na+
channel protein α-subunit, leading to neurotoxic and cardiotoxic effects [31].
However, aconitine as well as its derivatives benzoylaconine and aconine,
could be useful in a combined drug therapy, as they are able to up regulate the
expression of P-glycoprotein, an efflux pump responsible for pumping
chemicals, including aconitine itself, out of the epithelial cells of different
tissues [32].
Colchicine is an anti-inflammatory drug usually prescribed to combat
familial Mediterranean fever and gout. Nevertheless, long-term treatment with
colchicine may cause serious side effects, including gastrointestinal disorders
and musculoskeletal conditions such as myopathy and rhabdomyolysis. The

mode of action of colchicine relies on its inhibitory effect over cellular

mytosis. More precisely, the alkaloid binds to cellular tubulin avoiding
microtubules polymerization and elongation, leading to an uncompleted
mitotic process where cells remain in metaphase (G2/M) [33]. It is worth
mentioning that the minimal lethal doses of oral colchicine may vary between
7 and 26mg, and the high fatality rate of this alkaloid has been reported after
acute ingestion dosages higher than 0.5mg/kg [34].
Conium maculatum (poison hemlock) is extremely toxic due its alkaloid
contents. Coniine, a piperidine alkaloid, displays both toxic and teratogenic
effects. The mechanism of action of this alkaloid is not fully understood, but it
is known that coniine is a nicotinic acid agonist. Symptoms include movement
problems, dilated pupils, slow and weak pulse, heavy salivation and nausea
[35]. In animal models this alkaloid produces multiple congenital contracture
abnormalities in the offspring of pregnant cows. It has been postulated that the
teratogenic effects of piperidine alkaloid are due the persistent desensitization
of fetal muscle-type nAChRs [36].
The use of harmine and harmaline as therapeutic drugs is limited by their
toxicity. They are able to inhibit the monoamine oxidase (MAO), which may
contribute to the psychotropic effect of another indole alkaloid; N,N-
dimethyltryptamine (DMT). In the Amazon region, both alkaloids are often
consumed together, in a beverage known as Ayahuasca, which contains
Banisteriopsis caapi (rich in β-carboline alkaloids) and Psychotria viridis (rich
in DMT), natural sources of these alkaloids. MAO inhibition promoted by β-
carboline alkaloids prevents first-pass metabolism of DMT, allowing its access
to the systemic circulation and then to the central nervous system (CNS). After
reaching the CNS, DMT binds to 5-hydroxytryptamine (5-HT) 2A receptors,
acting as an agonist and causing hallucinogen effects [37]. Tryptamines have
been used as recreational drugs due the lack of legal concerns over their
commercialization in some countries. Another natural derivate of tryptamine
that is closely related to DMT − 5-methoxy-N,N-dimethyltryptamine (5-MeO-
DMT) − is a potent short-duration hallucinogen in humans, and has high
affinity for the 5-HT 1A receptor, causing many physiological and behavioral
changes. Therefore, high doses of MAO inhibitors and 5-MeO-DMT have
been reported as a fatal combination, due the exacerbated serotonergic effect
or serotonin toxicity [38].
Brucine and strychnine are the major alkaloids (over 70%) identified
on extracts obtained from dried seed of Strychnos nuxvomica L., and are
responsible for its pharmacological (analgesic and anti-inflammatory
activities) and toxic effects. Both alkaloids are rapidly absorbed after ingestion

and are distributed to various tissues, especially the renal tissue. In vitro assays
showed that strychnine and brucine present cytotoxic effect against kidney
cells (VERO cells) at concentrations above 450μM and 900μM, respectively.
In addition, brucine showed the ability to bind to the DNA of these cells
[17]. Strychnine has been reported as a convulsing agent, as it acts as an
antagonist of the receptors (GlyRs), binding to the inhibitory neurotransmitter
glycine. Strychnine binding sites are identified at high levels in the spinal
cord and motoneurons. Symptoms such as hyperactivity of the sensory and
motor functions are very common in cases of intoxication. Higher doses of
strychnine may also lead to death by respiratory or spinal paralysis, or by
cardiac arrest [39].
Eserine (also known as physostigmine) is a reversible inhibitor of
acetylcholinesterase, an enzyme responsible for acetylcholine hydrolysis in the
synaptic cleft of the neuromuscular junction. This alkaloid is used
therapeutically to treat anticholinergic delirium. However, high doses of
eserine can lead to excessive cholinergic activity, followed by serious adverse
effects, including seizures and occasional cardiotoxicity [40].

METHODOLOGY
This chapter gives a broad overview of publications in which poisoning by
alkaloids from plants can be identified by gas chromatography (GC). Due to
the extremely high number of toxic alkaloids, analysis by GC restricted the
number of alkaloids to around 100. Of these, only plant-derived alkaloids have
been used for presentation in this chapter. An initial search was conducted
of the scientific databases Scopus and Scifinder, using the search terms
“alkaloids” and “fatal poisoning”, which resulted in 99 compounds. Based on
these results, a new search was conducted on the database Google Scholar,
searching only on alkaloids derived from plant sources, using the search terms
“toxic alkaloids” and “gas chromatography analysis”. This search yielded 35
alkaloids, which are listed in Table 1 and which form the basis this chapter.

SEPARATION, DETECTION AND METHODS

The presence of toxic alkaloids has been investigated by gas
chromatography on a wide variety of samples, including plant extracts [14, 41-

53], herbal medicines and pharmaceutical preparations [54-58], foods [59-63],

and biological samples, such as blood, urine, brain, liver, kidney, heart, lung
and gastric contents [3, 64-77]. In the published studies, samples are mostly
subjected to an acid-base extraction, exploiting the characteristics of the
basicity of alkaloids prior to separation [7, 12, 13, 15, 46, 48-50, 55, 71, 73,
78-83]. In general, fractionation is preceded by extraction in methanol,
ethanol, hydroalcoholic solution or acidic aqueous solution, by methods
involving maceration [43, 45, 84], ultrasonication [10, 13, 26, 54] or a Soxhlet
apparatus [9, 59], with or without pH control. However, there are situations in
which alkaloids may be analyzed by GC directly after maceration in methanol,
such as in the analysis of senecionine and seneciophyline in Senecio alpinus
[85] or submitted to partition with increasing polarity solvents, hexane,
dichloromethane and ethyl acetate [86].
Pyrrolizidine alkaloids are frequently found in nature as N-oxides, which
are difficult to analyze by GC. For this reason, it is necessary to carry out
reduction of N-oxide function with Zn dust in acidic aqueous solution, to
obtain the corresponding tertiary alkaloid [8, 9,59-63, 87-92].
Many alkaloids can be directly analyzed and identified by GC coupled
to mass spectrometry (MS). However, some alkaloids, such as aconitine,
eserine and haemanthamine, may suffer thermal degradation under GC
conditions, and exhibit different mass fragmentation [41, 69, 93]. Toxic
alkaloids are frequently identified without derivatization using GC-MS, but
derivatization can improve resolution and peak shape and minimize thermal
decomposition in the injector. The most frequently used derivatives are the
trimethylsilyl ethers formed by the reaction with N,O-bis(trimethylsilyl)
trifluoroacetamide (BSTFA) in pyridine [41, 69, 79, 94-97], or N-methyl-N-
trimethylsilylfluoroacetamide (MSTFA) [61, 63, 67, 68]. Indole alkaloids
can also be derivatized using heptafluorobutyrylimidazole (HFBI) [98],
acetylated with acetic anhydride in pyridine [65, 66] or methylated with
trimethylanilinium hydroxide in methanol [99].
Regarding chromatographic columns, it is observed that older studies
analyzing the indole alkaloids strychnine, brucine, eserine, DMT and 5-MeO-
DMT employ as columns glass tubes with internal diameter (id) of about 3 to
4mm and length of about 0.6 to 4m. These studies employ stationary phases
(1-3%) on a silane-treated support (Gas Chrom Q, Chromosorb W, among
others). The stationary phase with low polarity methylpolysiloxane (known
commercially as OV-1, OV-101, SE-30) is used for the analyses of reserpine,
strychnine, eserine, brucine, DMT and 5-MeO-DMT [93, 100-106]; the phase
50% phenyl 50% polymethylsiloxane (OV-17) is used for the analysis of DMT

and strychnine [99, 104, 107]; the phase 20% phenyl 70% methylpolysiloxane
(OV-7) is used for the analysis of 5-methoxydimethyltryptamine [108]; and
5% phenyl 95% methylpolysiloxane (SE-52) is used for the analysis of DMT
[107]. In these studies, carrier gas He or N2 flow vary from 20mL/min [105] to
100mL/min [101]. Column oven temperatures, applied as gradient or isotherm,
vary from 110 to 280ºC [101, 108-110].
The development of capillary gas chromatography led to the virtual
abandonment of the use of glass columns of 3-4mm in diameter. The use of
capillary columns of several meters in length (5 to 60m) [50, 111], with
internal diameter of about 0.2 to 0.5 mm [70, 111-114], makes it possible to
increase the separation efficiency, with a drastic reduction in carrier gas flow
(He, H2 or N2), which now varies between 0.9 and 3mL/min [7, 45, 115],
reaching up to 12mL/min [111, 112]. The injector port temperature is usually
set between 250 and 300°C [55, 56, 88, 103, 116, 117].
However, there are situations in which the analysis of thermally labile or
low volatility compounds may be favored by the use of reduced length
columns, increasing the carrier gas flow rate and lowering the temperature
programming rate, as described by Fialkov and coworkers [118]. Various
classes of substances can be analyzed by a technique called “supersonic GC-
MS”, including the thermally labile alkaloid reserpine (608 Daltons). The
authors use a column of 1m length, 0.25mm id, 0.1µm DB-XLB film (mid
polarity) and 100mL/min helium column flow rate. The column temperature
programming rate is 30ºC/min from 100 to 280ºC. The transfer line and nozzle
temperatures are 280ºC. An optic PTV injector is used, programmed from 100
to 280ºC at 5ºC/s. This procedure reduces intra-injector degradation and
provided reasonably good chromatography, well-defined peak shapes, and
high quality mass spectra, with little loss in the GC resolution.
In regard to detection, the flame ionization detector (FID) is the most
widely used GC detection method [119]. Its high sensitivity, linearity and
robustness make this technique highly suitable for quantitative analysis of
toxic alkaloids in a wide variety of samples. However, FID only gives the
retention time to help with the identification of the substance. The FID
operating temperature in the analysis of toxic alkaloids is approximately 230
to 350ºC [9, 78, 88, 92, 105, 106, 108, 120, 121].
Nitrogen-phosphorus detectors (NPD) are often used in GC alkaloid
analysis, to explore its selective effect on nitrogen in alkaloid structures [45,
59, 77, 87, 91, 111, 112, 115, 120, 122-130]. This detector has high sensitivity
towards nitrogen and phosphorus compounds and excludes others from the

resulting gas chromatograms, such as lipids and cholesterol esters from

biological samples [119, 126].
The MS detector, with electron impact ionization (70eV) or positive
chemical ionization, is widely used for the rapid identification of toxic
alkaloids, being especially useful in qualitative analyses. The MS detector can
be used in scan mode or in selective ion monitoring mode, to detect the
selective ion of the desired alkaloid. The most used MS conditions for the
analysis of toxic alkaloids are: transfer line 250-320ºC, scan range 40-650
Daltons, and ion source 150-230ºC [10, 54-59, 84, 88, 131].
It is possible to use dual column capillary chromatography associated with
two detectors [129, 129, 130]. Watts & Simonick [129, 130] employed the
nonpolar column Ultra-I methylsilicone or Ultra-2, 5% phenyl methyl silicone
(Hewlett-Packard), and the polar column HP-17, 50% phenylmethylsilicone
(Hewlett-Packard), placed in the same injection port with dual NP detectors to
analyze basic and neutral substances in biological samples and solutions in one
injection, with simultaneous NP detection. A two-holed 100% graphite ferrule
sealed the two capillary columns into the injection port. Perrigo and coworkers
[127] also describe this technique to analyze strychnine and many other
substances in solution with the dual-column configuration, but with two
different detectors: a flame ionization detector and a nitrogen-phosphorus
detector. The two identical columns, DB-l, 15m × 0.32mm id, film thickness
of 0.25µm (Agilent J&W) are inserted into the same injection port using a
graphite ferrule with an enlarged single hole.
Table 1 shows summarized information on the gas chromatographic
techniques applied to the analysis of toxic alkaloids frequently related to oral
intoxication in a wide variety of samples. Currently, a wide range of marketed
capillary columns can be used for the analysis of toxic alkaloids. The most
frequently used columns are: DB-1 (15m × 0.25mm, 0.2µm); DB-5ms (30m ×
0.25mm, 0.25µm); DB-5 (15m or 30m × 0.25mm, 0.1µm); HP-5 (25m ×
0.2mm, 0.33µm); Ultra 2-HP (12m × 0.2mm, 0.33µm); DB-5 (15m or 30m ×
0.25mm, 0.1µm); ZB-1 (30m × 0.25mm, 0.25µm); HP-5ms (30m × 0.25mm,
0.25μm); SE-54 (30m × 0.25 mm, 0.33µm); and CP-Sil 8 CB (30m × 0.25mm
id, 0.25μm). In regard to detection, the flame ionization detector (FID),
nitrogen-phosphorus detector (NPD) and mass spectrometry detector (MS) are
the mostly frequently used.

ANALYSIS OF BIOLOGICAL SAMPLES

The action mechanism of toxic alkaloids is variable and their toxicity
affects different physiological processes. Determining the origin of a particular
fatality is a challenge for the analyst, which must be focused on the detection
of the compound responsible for the poisoning. Table 1 shows a large amount
of GC methods used to detect a particular toxic alkaloid in biological samples.
Laboratory analyses of blood, tissues or urine are the only way to determine
the diagnosis of poisonings. Pre-treatment of these samples may include
methods of extraction, clean-up, derivatization and analysis.
Biological samples, such as blood and tissues, require separation of
proteins, which can be done by precipitation, through the addition of ethanol,
methanol or acetone and centrifugation [24, 69, 97, 103]. Some extractions
of alkaloids from urine sample require addition of an alkaline solution
and chloroform or only organic solvent, followed by ultrasound. After
centrifugation of the sample solution, the organic layer is transferred and dried
for further analysis.
Some samples that contain pyrrolizidine alkaloids in complex matrix
alkaloids, such as plant extracts, animal fluids and tissues, honey and herbal
medicines, can be pretreated by adsorption in a resin of solid phase extraction
(SPE), using C18, SI (silica gel) or weak and strong cation exchange
cartridges. Some of the cartridges frequently used are: C18 SPE column [111],
Oasis hydrophilic/lipophilic mixed-bed SPE columns from Waters corporation
[132, 133], the weak ion exchange LC-SCX cartridge from Supelco [134], the
strong cation exchange SPE FocusTM column, from Agilent Technologies [65,
66], Chem Elut cartridges for solid supported liquid-liquid extraction,
from Agilent Technologies [135], Bond Elut LRC cartridge from Agilent
Technologies [59], Bond Elut SI cartridge from Agilent Technologies
[97], and Bond Elut C18 cartridge from Agilent Technologies [72]. The solid
phase microextraction (SPME) using CarbowaxTM/Divinylbenzene fiber
and headspace SPME with polydimethylsiloxane/divinylbenzene fiber is
successful in strychnine analysis in blood and DMT analysis in Ayahuasca
beverage, respectively [136, 137]. The SPME technique is practical and avoids
the use of toxic solvents.

Alkaloid Sample analyzed Method and Stationary phase used Limit of detection Ref.
ionization mode (LOD)/Limit of
quantification
(LOQ)
Aconitine Human material (urine GC-MS-EI; GC- CC*: DB-5 (15m × 0.25mm, 0.25 μm); LOD (GC-MS): [3, 67-69,
(diterpene) and blood); animal TOF-MS-EI DB-5ms (30m × 0.25mm, 0.25 μm); TC-1 10pg/injection [3, 96, 96, 97]
material (urine, plasma, (15m × 0.25 mm., 0.1μm). 97]; 0.05ng/mL [69]
blood and tissues); plant
(methanol extract)
Brucine Standard solution; GC-FID; GC-MS- Glass column: 1% SE-30 on Anakrom [57, 70, 71,
(indole) human material (fluids EI; Py-GC-MS- ABS 80-100 mesh (1m × 3mm); 3.0% OV- 93, 101,
and tissues); animal EI; GC-Argon β- 1 (0.91m × 6.4mm od); glass U-tubes 1% 106, 138-
material (urine, serum, ionization detector SE-30 on Gas-Chrom P 100-140 mesh (4 142]
gastric contents); plant to 6ft × 3 mm). CC*: cross-linked methyl
(acetone extract; silicone film (12.5 m × 0.2 mm); DB-5
benzene-ethanol extract; (15m × 0.53mm); DB-5 (30m × 0.25mm);
tincture; herbal DB-5ms (30m x 0.25mm); CP-Sil 8 CB
medicine) (30m × 0.25mm, 0.25μm).
Colchicine Human urine; plant GC-MS-EI CC*: SPB-5 (15m × 0.25mm); HP5-ms [44, 143,
(phenetyl- tissue (30m × 0.25mm, 0.25 µm). 144]
isoquinoline)
Coniine Plant (tissues and acidic GC-MS; GC- CC*: HP-1 (12m × 0.2mm, 0.33µm); DB-5 LOD (GC-NPD): [15, 111,
(piperidine) methanol extract); NPD; GC-FID (5m × 0.53mm, 1.0µm); EC-1 (30m × 0.1ppm [112]; LOD 112]
animal material (fluids, 0.23mm); HP-5ms (30m × 0.25mm, (GC-MS): 1ppm
tissues, eggs) 0.25µm). [112]

Alkaloid Sample analyzed Method and Stationary phase used Limit of detection Ref.
ionization mode (LOD)/Limit of
quantification
(LOQ)
N,N- DMT Plant (ethanol extract, GC-MS-EI; GC- Glass column: 3% SE-52 on Gas Chrom Q LOD (GC-NPD): [19, 20, 53-
(indole) 80% methanol extract, NPD; GC-MS- 80-100 mesh (2m × 4mm); 3% OV-17 Gas 30ng/L [107]; 56, 75, 76,
methanol extract, PCI; GC-surface Chrom Q 100-120 mesh (2m × 2mm); OV- 0.01mg/mL [122]; 95, 98, 99,
tissues, beverage, ionization 17 on Chromosorb WHP 80-100 mesh (2m 0.5ng/mL [123]; 102, 107,
capsules and tablets); detection; HT- × 6mm od); spiral glass column 5% F- LOD (GC-surface 115, 122,
human material GC-MS-EI 60/1.5% SE-30 on Gas Chrom P 80-100 ionization detection): 123, 137,
(plasma, blood, urine); mesh (2ft × 3mm). CC*: DB-5ms (30m × 0.5ng/mL [115]; 145-150]
standard solutions 0.25mm, 0.25µm); HP-5ms (30m × LOD (GC-MS):
0.25mm, 0.25µm); SE-30 (18m × 0.1ppm [55];
0.33mm); HP Ultra-2 (25m or 12m × 10ng/mL [76];
0.2mm, 0.33μm); VF-5ms (30m × 10pg/mL [95];
0.25mm, 0.25μm); DB-1; ZB-1 (30m × 0.5ng/mL [102];
0.25mm, 0.25µm); CP-Sil 8 (30m × 0.78mg/L [137];
0.25mm, 0.25µm); SLB-5ms (30m × 0.5-6ng/mL [148];
0.25mm, 0.25µm); WCOT cross-linked 0.12mg/g [150];
methyl silicone 12 (36m × 0.2mm); DB-5 LOQ (GC-NPD):
(15m × 0.25mm, 0.1µm); Rtx-5MS (30m × 0.02mg/mL [122];
0.25mm id, 0.25µm); BP-l (25m × 5ng/mL [123];
1.6ng/mL [124];
0.22mm); SPB-1 (30m × 0.20mm); SE-54
LOQ (GC-MS):
(30m × 0.25mm).
9.5mg/L [137]
Echimidine Plant (ethanol extract, GC-MS-EI; GC- CC*: Rtx-5 (30m × 0.25mm, 0.25µm); LOD (GC-NPD): [43, 87]
(pyrrolizidine) aqueous extract) NPD DB-1 (30m, 0.25µm). 0.1-0.4 ng/µL [87]

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Alkaloid Sample analyzed Method and Stationary phase used Limit of detection Ref.
ionization mode (LOD)/Limit of
quantification
(LOQ)
Echinatine Plant (acidic aqueous GC-FID; GC-MS- CC*: DB1- 30W (30m × 0.317mm); DB-1 [14, 151,
(pyrrolizidine) extract, methanol EI; GC-NP-TSD (30m × 0.32mm, 0.25µm); CP Sil 5 (25m 152]
alkaloid extract); × 0.32mm).
animal material
(methanol extract)
Eserine or Standard solution; GC-FID; GC- Glass U-tubes 3.8% SE-30 on Diatoport S, [100, 135,
physostigmine human material ATD; GC-MS-EI 80-100 mesh (4ft × 3mm). CC*: SE-54 153]
(indole) (urine) (15m × 0.32mm, 0.25µm); SE-54 (25m ×
0.3mm, 0.17µm).
Fulvine Plant (methanol GC-MS-EI CC*: DB-5ms (30m × 0.25mm). [10]
(pyrrolizidine) extract)
Haemanthamine Plant (alcohol extract; GC-MS-EI; GC- CC*: HP-5ms (30m × 0.25mm, 0.25μm); [12, 13, 46-
(indole) acidic aqueous MS-FAB; GC- DB-5; DB-1 (15m × 0.25mm, 0.2μm); DB- 49, 79-81,
extract; shoot culture) MS-CI; GC-FID; 5ms column (30m × 0.25mm, 0.25μm). 120, 154]
GC-NPD
Harmaline Plant (ethanol extract, GC-MS-EI; GC- CC*: CP–Sil 8CB-MS (30m × 0.25mm, LOD (GC-MS): [19, 50, 54,
(indole) beverage, herbal NPD 0.25μm); HP1-MS (30m × 0.25mm, 0.05µg/mL [58]; 56, 58, 122]
products); standard 0.25μm); HP Ultra-2 (25m × 0.2mm, LOD (GC-NPD):
solution 0.33μm); ZB-5MSi (60m × 0.25mm, 0.01mg/mL [122];
0.25μm); DB-5ms (30m × 0.25mm, LOQ (GC-MS):
0.25μm). 0.1µg/mL [58]; LOQ
(GC-NPD):
0.02mg/mL [122].

Alkaloid Sample analyzed Method and Stationary phase used Limit of detection Ref.
ionization (LOD)/Limit of
mode quantification
(LOQ)
Harmine Plant (ethanol extract, GC-MS-EI; CC*: DB-5ms (30m × 0.25mm, 0.25μm); LOD (GC-MS): [19, 50, 54,
(indole) acidic methanol extract, GC-NPD SE-30 (30m × 0.53mm, 1.2μm); ZB-5MSi 0.05µg/mL [58]; 56, 58, 72,
beverage, herbal (60m × 0.25mm, 0.25μm); Rtx-5MS (30m × LOD (GC-NPD): 73, 122]
products); human 0.25mm, 0.25μm); HP1-ms, 30m × 0.25mm, 0.01mg/mL [122];
material (hair); standard 0.25μm); HP Ultra-2 (25m × 0.2mm× LOQ (GC-MS):
solutions 0.33μm); CP-SIL 8CB-ms (30m × 0.25mm, 0.05µg/mL [58];
0.25μm). LOQ (GC-NPD):
0.02mg/mL [122].
Heliotridine Plant material (methanol GC-MS-EI; CC*: DB-1 (30m × 0.32mm) [92, 155,
(pyrrolizidine) extract, acidic aqueous GC-FID 156]
extract)
Ibogaine Plant (acidic aqueous GC-MS-EI; CC*: Rtx-5MS (15m × 0.25mm, 0.25μm); LOD (GC-MS): [21, 22, 24,
(indole) extract); human material GC-MS-PCI; DB-1 (15m × 0.32mm, 0.25μm); DB-1 (30m 0.5µg/mL [82]; 74, 82, 110,
(fluids); animal material GC-FID; GC- × 0.25mm, 0.25μm); DB-5 (15m × 0.25mm, 20ng/mL [21]; 157-160]
(tissues, fluids), standard AFID 0.1 μm); DB-5ms (30m × 0.25mm, 0.1μm); 5ng/mL [22];
solutions 5% phenyl, 95% methylsiloxane (30m × 10ng/mL [24];
0.25mm, 0.50μm); 2% SE- 52. 1ng/mL [74]; LOQ
(GC-MS):
1.0µg/ml [82];
Integerrimine Plant (acidic chloroform GC-MS-EI; CC*: DB-5MS (30m × 0.25mm); Rtx-5 LOD (GC-FID): [6, 25, 45,
(pyrrolizidine) extract, acidic aqueous GC-MS-CI; (30m × 0.32mm, 0.1µm); HP-5ms (30m × 0.4-0.5µg/g [25]; 86, 131,
extract, methanol extract, GC-NPD; 0.25mm, 0.25µm); HP-1 (30m × 0.25μm); LOD (GC-MS): 0.1 161, 162]
basic chloroform- GC-FID SE-30 (30m × 0.25mm, 0.25µm); RSL-200 ppm [6]; LOQ
methanol extract) (50m × 0.32mm). (GC-NPD): 30µg/g
[45]

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Alkaloid Sample analyzed Method and Stationary phase used Limit of detection Ref.
ionization (LOD)/Limit of
mode quantification
(LOQ)
Lasiocarpine Plant (acidic aqueous GC-MS-EI CC*: Rtx-5MS (30m × 0.25mm, 0.5µm); [23, 163]
(pyrrolizidine) extract), animal material HP-5 (50m × 0.32mm, 0.17μm)
(eggs); culture medium
containing lasiocarpine
Lycopsamine Plant material (methanol GC-MS-EI; CC*: CP-Sil 5 CB (25m × 0.32mm); RSL- LOD (GC-MS): [6, 14, 151,
(pyrrolizidine) extract; basic GC-MS-CI; 200 (50m × 0.32mm); DB-1 (30m × 0.32mm, 0.1 ppm [6] 155, 164,
chloroform-methanol GC-NPD 0.25µm); ZB-1ms (30m × 0.25mm, 0.25μm); 165]
extract, acidic aqueous DB-5 (15m × 0.53mm).
extract), animal material
(larvae,nd eggs)
Lycorine Plant (methanol extract, GC–MS/MS- CC*: DB-1 (15m × 0.25mm, 0.2mm); HP- [12, 41, 42,
(indole) basic methanol extract, EI; GC-MS- 1ms (30m × 0.25mm, 0.25μm); HP-5ms 47-49,
ethanol extract, EI; GC-FID; (30m × 0.25mm, 0.25µm); DB-5ms (30m × 51, 52,
chloroform extract, GC-NPD 0.25mm, 0.25µm); AT-1 (25m × 0.32mm, 79-81,
acidic aqueous extract); 0.30μm); Sapiens-X5ms (30m × 0.25mm, 83, 120,
liquids from shoot 0.25µm). 166-170]
culture (methanol
extract)
5-MeO-DMT Plant (basic methanol GC-MS-EI; Glass column: 2% OV-7 on Chromosorb W LOD (GC-MS): [20,
(indole) extract, aqueous basic GC-FID; CI- AW-DMCS 100-120 mesh (2m × 2mm); 0.1ppm [55]; 54-56,
solution, herbal products, IT-MS/MS CC*: SE-30 (18m × 0.33mm); DB-5ms (30m 0.03µg [66]; 0.5- 65, 66, 95,
beverage); standard × 0.25mm, 0.25µm); VF-5 (30m × 0.25mm, 6µg/mL (Wang et 98, 108,
solutions, human 0.25μm); HP-5ms (30m × 0.25mm, 0.25μm; al., 2008) 147, 148,
material (fluids), animal BP-l (25m × 0.22mm); SPB-1 (30m × 171]
material (urine) 0.20mm); HP-1ms (30m × 0.25mm,
0.25µm).

Alkaloid Sample analyzed Method and Stationary phase used Limit of Ref.
ionization detection
mode (LOD)/Limit of
quantification
(LOQ)
Monocrotaline Plant (methanol extract), GC-MS-EI; CC*: DB-5ms (30m × 0.25mm); DB-1 (30m); [10, 61,
(pyrrolizidine) honey, animal material GC-MS-FAB; DB-1ms (30m × 0.32mm, 0.25m). 172]
(microsomal liver) GC-MS-PCI;
HRGC-MS-
EI
Otosenine Plant (acidic aqueous GC-MS-EI; CC*: DB-1 (15m × 0.317mm, 0.25µm); DB-1 [8, 78, 90,
(pyrrolizidine) extract; acidic methanol GC-FID; GC- (15m × 0.25mm); OV-1 (30m × 0.25mm, 131]
extract) NPD 0.25µm); DB-5ms (30m × 0.25mm); ZB1 or
ZB5 (30m × 0.32mm).
Platyphylline Plant (acidic aqueous GC-MS-EI; CC*: HP-5ms (30m × 0.25mm, 0.25µm); SA-5 [7, 84, 85,
(pyrrolizidine) extract, methanol extract, GC-MS-PCI; (30m × 0.25mm, 0.25µm); SE-54; DB-5 (30m 88, 116,
ethanol extract, animal GC-FID; GC- × 0.32 mm); ZB-1 (30m × 0.32 mm, 0.25 µm). 173]
material insects and NPD
fluids)
Reserpine Standard solution; Supersonic Glass column 1%OV 1 on Gas Chrom Q 100- [103, 105,
(indole) pharmaceutical GC-MS; GC- 120 mesh (40m × 4mm); glass tube 3% OV- 118, 135]
preparations (tablets, MS-EI; GC- 101 on Gas-Chrom Q l00-120 mesh (1.82m ×
ampoules, capsules); FID 0.4 mm). CC*: DB-XLB (1m × 0.25mm,
human urine; animal 0.1µm); SE-54 (25m × 0.3mm, 0.17µm).
material (brain)
Retronecine Plant (acidic aqueous GC-MS-EI; CC*: DB-5 (30m × 0.32mm); ZB-1 (30m × LOD (GC-FID): [62, 63, 84,
(pyrrolizidine) extract); animal material GC-FID; 0.32mm, 0.25µm); DB-1 (30m); DB1-30W 0.02 µg/mL 92, 94, 121]
(rumen fluid, insects), HRGC-MS- (30m × 0.317mm); ZB-5ms (30m × 0.25mm, [121]
bacterial growth media, EI 0.25µm); Rtx-5 (30m × 0.25mm, 0.25µm)

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Alkaloid Sample analyzed Method and Stationary phase used Limit of Ref.
ionization detection
mode (LOD)/Limit of
quantification
(LOQ)
foods (honey, pollen
containing foods)
Retrorsine Plant (acidic aqueous GC-NPD; CC*: HP-1 (30m, 0.25μm); DB-5ms (30m × [8, 10, 45,
(pyrrolizidine) extract, methanol extract, GC-MS-EI; 0.25mm); HP-5ms (30m × 0.25mm, 0.25µm); 59, 60, 61,
chloroform extract, herbal GC-MS-PCI; SA-5 (30m × 0.25mm, 0.25µm); OV-1 (30m × 78,
medicines), animal GC-FID; 0.25mm, 0.25µm); DB-1ms (30m × 0.32mm, 89, 90, 94,
material (fluids, tissues); HRGC-MS- 0.25µm); DB-1 (15m × 0.25mm, 0.25µm); DB- 111, 131,
foods (honey, pollen EI; HRGC- 5 (5m × 0.53mm, 1.0µm); HP-5 (30m × 132, 155,
products) FID/NPD 0.32mm, 0.25µm); ZB-1 and ZB-5 (30m × 174, 175]
0.32mm); HP-1 (12m × 0.2mm, 0.33µm).
Riddeline Plant (ethanol extract, GC-MS-EI; CC*: HP-5ms (30m × 0.25mm, 0.25µm); SA-5 [7, 45, 78]
(pyrrolizidine) acidic aqueous extract) GC-FID; GC- (30m × 0.25mm, 0.25µm); HP-1 (30m,
NPD; HRGC- 0.25μm); OV1 (30m × 0.25mm, 0.25µm).
MS
Sarracine Plant (methanol extract); GC-MS-EI, CC*: ZB1 (30m × 0.32mm); DB-17 (20m × [84, 176]
(pyrrolizidine) animal material (insects) GC-FID 0.18mm, 0.3µm).
Senecionine Plant (methanol extract, GC-MS- PCI; CC*: Duran 50 glass PS 264 - 7% diphenyl, LOQ (GC-NPD): [8, 9, 23,
(pyrrolizidine) acidic methanol extract, GC-MS-NCI; 1% vinyl polydimethylsiloxane (30m × 0.3μm); 30µg/g [45]; 45, 59-61,
acidic aqueous extract, GC-MS-EI; ZB1 (30m × 0.32mm), DB-5MS (30m × LOD (GC-MS): 78,
chloroform extract); GC-MS-FAB; 0.25mm); DB-1 (15m × 0.25mm, 0.25µm); SE- 0.137 μg/mL 84, 85,
animal material GC-FID; 54 (20 m); HP5-ms (30m × 0.25mm, 0.25µm); [23] 88-91, 116,
(microsomal liver, eggs, HRGC-MS- ZB1 or ZB5 (30m × 0.32mm); HP-5 (30m × 131, 155,
larvae); food (honey, EI; HRGC- 0.32mm, 0.25µm); HP-5 (50m × 0.32mm, 172, 173,
pollen products, silage) FID/NPD; 0.17µm); Optima-5 (60m × 0.25μm); CP-Sil 175, 177]
GC-NPD m8 (50m × 0.25mm, 0.25μm), DB5 (15m ×
0.25mm); OV1 (30m × 0.25mm, 0.25µm); HP-
1 (30 m × 0.25 μm)

Alkaloid Sample analyzed Method and Stationary phase used Limit of detection Ref.
ionization mode (LOD)/Limit of
quantification (LOQ)
Seneciphylline Plant (methanol extract, GC-MS-EI; GC- CC*: DB-1 (15m × 0.25mm); ZB1 (30m × LOQ (GC-NPD): [8, 9, 45, 59,
(pyrrolizidine) acidic methanol extract, MS-PCI; GC-FID; 0.32mm, 0.25μm); DB-5 (15m or 30m × 30µg/g [45] 60, 61, 78,
chloroform extract, GC-NPD; HRGC- 0.25mm); HP-1 (30m, 0.25μm); glass 85, 88-91,
acidic aqueous extract); MS-EI; HRGC- column PS 264 (30 m, 0.3μm); Optima-5 94, 155,
food (honey, pollen FID/NPD (60m, 0.25μm); CP-Sil 8CB (50m × 173, 177]
products, silage), 0.25mm, 0.25μm); SE-54 (20m); DB-1ms
animal material (30m × 0.32mm, 0.25µm); HP-5ms (30m ×
(insects) 0.25mm, 0.25µm); SA-5 (30m × 0.25mm,
0.25µm); SE-54; OV1 (30m × 0.25mm,
0.25µm)
Senkirkine Plant (ethanol extract, GC-MS-EI; GC- CC*: HP-5ms (30m × 0.25mm, 0.25µm); [8, 9, 59, 60,
(pyrrolizidine) methanol extract, acidic MS-PCI; GC-FID; SA-5 (30m × 0.25mm, 0.25µm); ZB-1 61, 84, 88-
methanol extract, acidic HRGC-FID/NPD; (30m × 0.32mm); glass column PS 264 90, 116,
aqueous extract); food HRGC-MS-EI (30m, 0.3μm); ZB-1 (30m × 0.23mm, 131, 155]
(honey, pollen 0.25µm); DB-5ms (30m × 0.25mm); DB-
products); animal 1ms (30m × 0.32mm, 0.25µm); ZB-5 (30m
material (insects) × 0.32mm); DB-1 (15m × 0.25mm).
Strychnine Standard solution; GC-MS-EI; GC- Glass column: 1.0-l.15% SE-30 on Gas- LOD (GC-NP/FID): [31, 35, 57,
(indole) human material (fluids MS-CI; fast GC- Chrom P, 100-140 mesh (4-8ft. × 3mm); 0.3µg/mL [180]; LOD 64, 70, 71,
and tissues); animal MS-EI; GC-argon 1% SE-30 on Anakrom ABS 80-100mesh (GC-MS/MS): 375µg/kg 77, 93, 101,
material (fluids); plant β-ionization (2m × 3mm); 3.0% OV-1 (0.91m × 0.64cm [134]; LOD (GC-MS): 104, 106,
(tincture, herbal detector; GC-FID; od); 3% OV-17 on Chromosorb W, 100- 30ng/mL ou 30ng/g 113, 114,
medicine, food) GC-NPD; GC- 120 mesh (4ft × 1/8 inch id); 3% OV-1 on [71]; 100ng/mL [31]; 117, 125-
NP/FID; GC- Chromosorb W, 100-120mesh (4ft × 1/8 LOD (SPME-GC-MS): 130, 133-
MS/MS-EI; GC × inch id). CC*: HP 8 (10m × 0.1mm, 6.83ng/mL [136]; LOD 136,
GC–TOFMS; GC 0.34µm); CP-Sil 8 CB (30m × 250μm, (Oasis HLB-GC-MS) 138,
× GC–qMS 0.25μm); CP-Sil 5 CB (10m × 0.53m, 0.03µg/mL [133]; LOD 178-183]
5.2µm); CP-Sil 5 CB (25m × 0.32mm); (fast GC/MS): 10ng/mL

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Alkaloid Sample analyzed Method and Stationary phase used Limit of detection Ref.
ionization mode (LOD)/Limit of
quantification (LOQ)
DB-l (15m × 0.32mm, 0.25µm); DB-5 [183]; LOQ (GC-MS):
(15m × 0.53mm); Ultra-2 (12m × 0.25mm, 0.01mg/L [35];
0.25m); DB-5ms (30m or 15m × 0.25mm, 0.1µg/mL or 0.1µg/g
0.25µm); SE-54 (25m × 0.4-0.45µm); HP [64]; LOQ (GC-
SE-54 (17m × 0.2mm, 0.33µm); SE-54 MS/MS): 1,250µg/kg
(25m × 0.3mm, 0.17µm); BP-5 (12m × [134]; LOQ (fast GC-
0.53mm, 1.0µm); VF-5ms (30m × 0.25mm, MS): 25ng/mL [183];
0.25µm); VF-Xms (30m × 0.25mm, LOQ (SPME-GC-MS):
0.25µm); HP-5 (25m or 17m × 0.2mm, 8.91ng/mL [136]; LOQ
0.33µm); HP-1 (12.5m × 0.2mm, 0.33µm); (Oasis HLB-GC-MS)
Rtx-5MS (15m × 0.25mm, 0.25µm); HP- 0.10µg/mL [133]
5ms coupled with BPX50 (1.0m × 0.1mm,
0.1µm); HP cross-linked 5% phenylmethyl
silicone (12m × 0.2mm, 0.3µm). Ultra-1 or
Ultra-2 (12.5m × 0.32mm, 0.5µm); HP-17
(12.5m × 0.32mm, 0.5µm); BPX5 (30m ×
0.25mm, 0.25 µm); BPX50 (0.8m ×
0.1mm, 0.2µm).
Symphytine Plant (methanol extract, GC-MS-EI; GC- CC*: SE54 (20m or 50m × 0.32mm); DB-1 LOD (GC-NPD): 0.1 [5, 87, 184]
(pyrrolizidine) aqueous extract) MS-PCI; GC-FID; (30m, 0.25µm) ng/µL [87]
GC-NPD
Yohimbine Plant (methanol extract, GC-MS-EI CC*: Rtx-5ms (15m × 0.25mm, 0.25μm); [26, 82,
(indole) ethanol extract, acidic CP-PoraBOND Q (25m); HP-5MS (30m × 185, 186]
methanol extract) 0.25mm,0.25µm); DB-5ms (30m ×
0.32mm, 0.25µm).
CC*: Capillary column.

MASS FRAGMENTOGRAMS
The mass spectra (GC/MS) used as information for mounting the
possible fragmentation pathways (Figures 1 to 3) of the most frequently cited
alkaloids are shown in Table 1. They were obtained from the Scifinder
and Google Scholar databases, and the NIST and Wiley libraries. The base
peak is shown in most of the fragmentograms and when the base peak is the
molecular ion, the principal fragments are presented. The fragmentations are
based on characteristic alkaloid breaks and/or proposals based on mass
spectrometry theory. For some alkaloids, such as aconitine and echimidine, the
molecular ions do not appear in the mass spectra when these alkaloids are
injected without derivatization into the GC/MS. In the aconitine case, the
fragmentogram shows the fragmentation pathway of the characteristic peaks
(m/z 105) of the Aconitum alkaloid.

ADVANTAGES AND DISADVANTAGES OF THE GAS

CHROMATOGRAPHY AS ANALYTICAL TECHNIQUE

Analyses by gas chromatography/mass spectrometry in full scan or

SIM modes are the methods of choice for unequivocally confirming the
presence of certain alkaloids in biological fluids. The constituents in the
sample are identified based on comparison of the full scan spectra with a
library (NIST or Wiley) that exists on the GC apparatus and/or comparison
with the standards for the studied alkaloids.

Figure 1. Fragmentogram of diterpenoid alkaloid.

Figure 2. (Continued)

Figure 2. Fragmentograms of indole alkaloids.

Figure 3. Fragmentograms of pyrrolizidine alkaloids.

This is the most popular technique for the analysis of illicit drugs and their
analogs in various forensic cases. Other methods, such as LC/MS and capillary
electrophoresis (CE), are often chosen for alkaloid analysis. Each method has
unique advantages and disadvantages in relation to sensitivity, precision, and
simplicity of use [35]. Some examples of alkaloids analyzed by different
methods are presented below.
A comparison of these methods is made by Wang and coworkers [148] for
the analyses of tryptamines. Those authors describe and evaluate, for GC/MS
analysis the electron impact (EI) mode used, which shows good ionization
efficiency for tertiary amines such as DMT. They also describe the lowest
limit of detection (LOD) among the techniques, and the complications of
preparing the samples prior to their injection. The use of GC/MS in the area of
drug screening over many years has resulted in valuable libraries for users.
This is a highly positive point in favor of the method that is not mentioned in
other reports. However, one of the limitations is that it can only be used to
analyze volatile substances. The authors' choices for comparison of the
disadvantages of GC/MS are coupling methods with UV, HPLC and CE,
which improve the LOD of amines. In this case, HPLC/UV required a high
volume of organic solvents, and CE/UV, while providing the simplicity, speed,
sensitivity and economy necessary for the analysis of amines, requires alkaloid
standards for analysis.
The most important use of colchicine is for the treatment of acute gout.
This alkaloid has many side effects, and is responsible for many cases of
poisoning. GC/MS techniques can be applied to unequivocally detect
colchicines in urine. Nevertheless, LC/MS is the technique of choice, as it
provides more sensitive and specific detection of this alkaloid in blood and
urine, at therapeutic or subtherapeutic levels [35].
With respect to ibogaine, many analytical methods in biological
samples have been described in the literature, including GC, LC using MS or
fluorimetric detectors. GC/MS presents lower sensitivity then LC/MS [187].
Recently, Mazoyer and collaborators [74] show that the analysis of ibogaine
by GC-MS/MS using selected reaction monitoring mode (SRM) demonstrates
increased sensitivity, which led to the detection of the alkaloid in significant
toxicological quantities.
The analysis of the pyrrolizidine alkaloids by GC-EI-MS and LC-MS-MS
has well-established advantages and disadvantages that have been described
by Kempf and coworkers [61]. The main disadvantage of GC-MS is the need
to reduce PAS-N-oxides for further analysis, which increases the preparation
time of the samples. Other disadvantage are cited above for analysis by GC.

Aconitine must be extracted and derivatized before analysis by GC-MS.

However, despite these steps, the use of GC-MS with SIM mode is an accurate
and sensitive method to detect this alkaloid. Nevertheless, the preparation of
samples for analysis by LC-MS-MS is simpler and faster, which is important
when time is crucial to save lives [188, 189].

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[183] Rossi, S.S., de la Torre, X., Botrè, F., (2010). A fast gas
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[184] Röder, E., Wiedenfeld, H., KerstenJ, R., Kroger R., (1990).
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[185] Pawar, R.S., Grundel, E., Fardin-Kia, A.R., Rader, J.I., (2014).
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materials and dietary supplements using LC-MS/MS methods. J.
Pharm. Biomed. Anal. 88, 457-466.
[186] Kurzawa, M., Filipiak-Szok, A., Kłodzi´nskab, E., Szłyk, E., (2015).
Determination of phytochemicals, antioxidant activity and total phenolic
content in Andrographis paniculata using chromatographic methods. J.
Chromatogr. B 995–996, 101–106.
[187] Mačiulaitis, R., Kontrimavičiūtė, V., Bressolle, F.M.M., Briedis, V.,
(2008). Ibogaine, an anti-addictive drug: pharmacology and time to go
further in development. A narrative review. Hum. Exp. Toxicol. 27, 181-
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[188] Yoshioka, N., Gonmori, K., Tagashira, A., Boonhooi, O., Hayashi, M.,
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Reviewed by Fiona Pellew, Portuguese - English translator.

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Chapter 2

THE INFLUENCE OF SURFACTANT

MONOLAYER(S) ON THE EVAPORATION OF
LIQUID POLLUTANTS, STUDIED BY
REVERSE-FLOW GAS CHROMATOGRAPHY

H. H. Mohammad1,*, Rashid Atta Khan1 and

Khalisanni Khalid1,2
1
Chemistry Department, University of Malaya,
50603 Kuala Lumpur, Malaysia
2
Food and Agricultural Analysis Laboratory Program,
Technical Service Centre, Malaysian Agricultural Research and
Development Institute (MARDI), 43400 Serdang, Selangor, Malaysia

ABSTRACT
Reverse-flow gas chromatography (RF-GC) was been utilized to
compare the effect of Triton-X monolayer(s) on the evaporation of
methanol and ethanol. Evaporation rates and diffusion coefficients for the
respective liquid pollutants have been determined at 333.15 K in nitrogen.
The precision and accuracy of the method has confirmed the presented
methodology as suitable to be used in studying the retardation effect of
surfactants on the evaporation rates of volatile organic liquids. The
evaporation rates has been compared successfully with the available

* Corresponding
Author E-mail: [email protected]

published literature values, while the diffusion coefficients with compare

well with Fuller-Schettler-Giddings, affirming the validity of the
presented methodhology. The suppressing of the evaporation rates of
methanol and ethanol become significant (>40%) at amounts of surfactant
corresponding to more than two monolayers. The reduction of the
evaporation rate of the studied liquids is due to the formation of densely
packed surface monolayers or to the formation of an insoluble monolayer.

Keywords: evaporation, diffusion coefficients, rate coefficients, surfactants,

liquid pollutants, gas chromatography

1. INTRODUCTION
Chromatography is essentially separation process that is acheived through
differential migration of molecules under study (Giddings, 1965). The process
involves distribution of solute components between two phases, a mobile
phase and a stationary phase. The Russian botanist Tswett (Tswett, 1906)
became the first person to discover the chromatography technique, he used the
techique for isolation of plant pigments (Katsanos, 1988). Twenty five years
later, the method of chromatography was “reinvented” by Kuhn and Lederer in
1931 (R. Kuhn & Lederer, 1931; R. Kuhn, Winterstein, & Lederer, 1931).
They introduced liquid chromatography and the technique consists of thin-
layer and paper chromatography.
Wilson became the first person to describe the process mathematically, by
assuming solute adsorption-desorption equilibria (Wilson, 1940). The
transition of chromatographic techniques, first used for separation and later
applied to physiochemical measurements, became possible when Martin and
Synge developed the widely popular plate theory of chromatography, which
won the Nobel Prize in 1941. Even though the theory is inadequate to describe
recent developments in the chromatography field, the theory was first to
describe the development of a zone profile under the influence of a non-
equilibrium state and linear isotherm (Giddings, 1965).
The first study of physiochemical measurements by gas chromatography
(GC) was done by Glueckauf (Coates & Glueckauf, 1947) in 1947. He pointed
out the possibility of interpreting the data of adsorption isotherms that were
determined by gas-solid chromatography (GSC). In 1980, Prof. N.A. Katsanos
and his co-workers at the Physical Chemistry Laboratory, University of Patras,
developed the technique of reverse-flow gas chromatography (RF-GC)
(Agathonos & Karaiskakis, 1989; Khan Rashid Atta, Gavril, & Karaiskakis,

2002; Dalas, Katsanos, & Karaiskakis, 1986; Gavril, Katsanos, & Karaiskakis,
1999; Gavril, Koliadima, & Karaiskakis, 1999; Karaiskakis, 1985;
Karaiskakis, Katsanos, & Niotis, 1982, 1983; Karaiskakis, Lycourghiotis, &
Katsanos, 1982; Karaiskakis, Niotis, & Katsanos, 1984; Katsanos &
Karaiskakis, 1983; Katsanos & Karaiskakis, 1984; Katsanos, Karaiskakis, &
Niotis, 1984; Katsanos, Karaiskakis, & Niotis, 1985). The technique was
initially proposed to study kinetics in heterogeneous catalysis (Katsanos, 1980,
1982). The technique was then applied to the dehydration of the alcohols and
the deamination of primary amines (Karaiskakis, Katsanos, Georgiadou, &
Lycourghiotis, 1982).
The aim of this paper is to study the effect of surfactants on gas-liquid
interfaces by using RF-GC methodhology, since there are limited studies in
this area. The methodology of introducing surfactants on the gas-liquid
interface has been established by previous research (K.R. Atta, Gavril,
Loukopoulos, & Karaiskakis, 2004; H.H. Mohammad, Khalid, & Zain, 2014;
H.H. Mohammad, Mohd. Zain, Atta Rashid, & Khalid, 2013). However, there
is limited data that can contribute towards understanding how the molecules of
liquid pollutants migrate across a surfactant monolayer.
The research presented here studies the effects of Triton-X monolayer(s)
on the evaporation rates of methanol and ethanol. Low molecular weight
alcohol such as ethanol has been used as an additive in fuel in various
concentrations. Understanding the suppressive effect of surfactant monolayers
on the evaporation rates of those liquids will open a new horizon on how to
transport fuel-ethanol mixtures without losing the liquid during transport from
one city to another (Eric C. D. Tan & Dutta, 2013; Group, 2011). Futhermore,
the results from the research presented here can be used to mitigate the effect
of spillage of methanol into the sea; and give an alternative to the authorities
on how to handle any future industrial accident involving methanol or ethanol
(H.H. Mohammad et al., 2013; Riaz, Zahedi, & Klemeš, 2013).

2. METHODOLOGY
2.1. Materials

The solutes used as evaporating liquids (stationary phase) were methanol,

ethanol and Triton X-100 (iso-Octylphenoxypolyethoxyethanol, d = 1.06 g.
ml-1 and M = 646.37 g.mol-1) which were supplied by Merck. Purified
nitrogen (99.9% purity) which was used as the carrier gas (mobile phase)

supplied by Malaysian Oxygen Berhad (MOX). Hydrogen and compressed air

used to fuel the FID were supplied by MOX as well.

2.2. Techniques

Figure 1 shows the experimental setup of the reverse-flow gas

chromatography (RF-GC). Basically, the RF-GC system consists of the
conventional gas chromatograph oven, flame ionization detector (FID) and
six-port valve. RF-GC is a sampling technique and the sampling process is
carried out through a six or four port valve. The flow of the carrier gas is
reversed through the valve for short time intervals and then restored to the
original direction. RF-GC is different from conventional gas chromatography,
essentially it consists of a sampling cell which consist of sampling and
diffusion columns. Figure 2 shows the sampling cell located inside the
chromatography oven. The sampling cell is made from stainless steel with a
4mm i.d.. The length of the sampling column is l = l’ = 57 cm while the length
of the diffusion column is L = 28.5cm. A ¼-in Swagelok tee union is used to
connect them at the junction x = l’. The carrier gas flows continuously through
the sampling column and remains stagnant in the diffusion column. A glass
bottle (2 cm) filled with 0.5 cm3 of the solution containing surfactant is placed
at the bottom of the diffusion column by using a 1/4-in. Swagelok union. The
steps of preparing the Triton X-100 monolayer(s) on the surface of the low
molecular weight alcohols have been described in previous literature. A
restrictor is placed before the FID detector, to prevent the flame from being
extinguished when the valve position is switched.

2.3. Procedure

Before the RF-GC system is operated, every joint and connection in the
system is checked for leakage with Swagelok Snoop leak detection liquid.
Leakage of the system is indicated by bubble formation at the joints or the
connections of the system. When the RF-GC system is on, we have to wait for
a certain time, or until the baseline of the chromatogram becomes stable. After
monotonously rising until the concentration-time curve for the vapour phase of
the liquid is high enough, the chromatographic sampling procedure is started
by reversing the direction of the carrier gas via the six-port valve (the reversal
process is indicated in Figure 1 from one position (solid line) to the other

position (dotted line) and vice versa). The reversal period (6s) must be shorter
than the gas hold-up time in l + l’ columns. The temperature inside the oven
varies ± 0.1K while the pressure drops along the l + l’ columns are negligible.
The carrier gas flow is set at 1 cm3 s-1 while the pressure inside the sampling
cell is set at 1 atm.

Figure1. The apparatus of the Reverse-Flow Gas Chromatography system.

Figure 2. The sampling column located inside the gas chromatograph oven.

Figure 3. A sample chromatogram showing three sample peaks that “seat” on the
continuous concentration-time curve.

The reversal of the flow creates extra chromatography peaks on the

continuous concentration-time curve as shown in Figure 3. The area or height
of these peaks is proportional to the concentration of solute gas at the junction
of the diffusion and sampling columns.

3. MATHEMATICAL THEORY
The height, h of the sample peaks from the continuous signal, taken from
baseline to the maximum, was plotted as ln h versus time, giving diffusion
bands as shown in figure 4.
Mathematically the concentration of solute at the junction is given by h =
2c (l’, t) (3) where,

 h = height of the peak = concentration of vapors at x = l’ junction

 t = time
 l’ = length of sampling column

Figure 4. Diffusion band (plot of sample peaks height, h, against time, t0, from the
beginning of the experiment) for the evaporation of liquid, at 313.15 K and 101325 Pa
where t0 for each cycle (after 6s of flow reversal) is the time measured from the
beginning to the last reversal of gas flow.

Mathematical treatment of the RF-GC system for study of liquid-gas

interphases has been describe intensively in (Karaiskakis & Katsanos, 1984;
Khalid, 2011; Khalid, Khan, & Mohd. Zain, 2009, 2010, 2011a, 2011b, 2012;
Mohammad Hafiz Bin Hamzah, 2015; H.H. Mohammad et al., 2013; H.H.
Mohammad, Zain, Khan, & Khalid, 2014). Anyone interested in the
mathematical aspects of the experiment can easily refer to the publications for
reference.
The heights of the sample peaks obtained as shown in Figure 3 are
proportional to the concentration of the vapors of an evaporating liquid, c(l’, t)
at x = l’ and at time t0. The relationship can be further connected with the rate
coefficient for the evaporation process, KG, the diffusion coefficient of the
vapor into the carrier gas, D, and the geometrical details of the diffusion
column through the relation (Karaiskakis & Katsanos, 1984):

c(l ', t0 ) 
KG Dc0
V ( K G L  D)

1  exp  2(K G L  D)t0 / L2   (4)

where L is the length of the diffusion column and v the volumetric flow rate of
the carrier-gas. The sampling of the above-mentioned processes against time is

shown in figure 4. A steady-state situation is achieved after a period of time

where the graph shown in the figure becomes plateaued. After long times of
acquiring data, an infinite value for the peak height h∞ can be obtained from
this plot. This infinity h∞ value will be used for the linearization of the
resulting relation (Karaiskakis & Katsanos, 1984):

2 K G Dc0
h 
 v( K G L  D) (5)

By using the above approximation, one obtains (Karaiskakis & Katsanos,

1984):

 2( K G L  D ) 
ln(h  h)  ln h    t0 (6)
 L2 

A plot of ln (h∞- h) vs t0 is expected to be linear, at long enough times, for

which Eq. 4 was derived. A first value of KG can be calculated from the known
value of L, from literature or from the theoretically calculated value of D and
from the slope of the plotted graph, -2 (KG L+D)/L2 (Bird, Stewart, &
Lightfoot, 2002; Fuller, Schettler, & Glddlngs, 1966; Karaiskakis & Gavril,
2004; Karaiskakis & Katsanos, 1984)

Figure 5. Example of plotting for the diffusion of liquid vapor into carrier gas.

Figure 6. Data from evaporation of liquid vapor into carrier gas plotting according to
Eqn. 5

According to Eq. 14 of Ref. 35, the value of KG can now be used for the
plot of short-time data which is substituted now for c (l’, t0) in Eq. 2. The
results below are obtained after rearrangement logarithms are taken:

 1 
  1

  L    4 K c  DL  2
 L2 1
ln  1  KG t0   ln G 0

 v     4 D t0
2
  (7)
 2t02 
  

D value is obtained from the slope –L2/4D of the plot of the left hand side
of the above relationship, versus 1/t0 which yields a first approximation
experimental value.

4. RESULT AND DISCUSSION

The evaporation rates of methanol and ethanol under the influence of
Triton X-100 are shown in Tables 3 and 4. The diffusion coefficients of this

recent research, Dfound, are compared with the predicted ones from the Fuller-
Schettler-Giddings equation (Fuller et al., 1966) and with experimentally
obtained values from work done by Anikar H.J. (Anikar & Ghule, 1969). The
deviation (%) of the recent experimental values from the predicted and
published experimental literature values, Dlit is given in the last column of
each table.
The diffusion coefficients, Dfound, values from both tables show that the
addition of surfactant produced no effect on the diffusion coefficient of each
liquid, which is as expected (Gavril, Atta, & Karaiskakis, 2006). This is
because the diffusion coefficients measured by means of RF-GC is calculated
based on the diffusivity of the solute into the nitrogen gas. Thus the movement
of the molecules across the surfactant monolayer(s) will be not considered in
the Dfound calculation. The “diffusion” in this case is calculated after the
molecule successfully transits across the surfactant “barrier”. In the case of
methanol, the mean deviation values Dfound, differ from the respective
predicted (FSG) and published literature ones, 1.6% and 6.8% respectively. On
the other hand, the mean deviation of ethanol deviates 0.8% and 1.9% from
predicted and published literature, respectively. Dfound for both cases values
falls between predicted and experimental published literature values, which in
agreement with previous research (Gavril et al., 2006; H.H. Mohammad et al.,
2013). The total reproducibility of the method is determined to be 99.9%
respectively for both cases and with agreement with the previous work (H.H.
Mohammad et al., 2013).
Figure 7 shows the variation of the evaporation rates of methanol and
ethanol in the presence of surfactant versus the monolayer(s) coverage of
Triton X-100. The retardation of the evaporation rates of both liquid pollutants
is presented in Figure 8.
The uncertainty in determination of the evaporation rate values, kc varies
from 0.009% to 0.01% in the case of methanol and from 0.0002% to 0.02% in
the case of ethanol. Based on the results, ones can draw a safe conclusion of
the affect of Triton X-100 on the evaporation rates of the liquid pollutants, by
using RF-GC. (Gavril et al., 2006)

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Table 1. Rate Coefficients for the Evaporation of Methanol, kc, and Diffusion Coefficients of Its Vapors Into
Nitrogen, Dfound, Under the Effect of Various Amounts of Surfactant Triton X-100

Monolayer
Retardation 103Dfound /cm2s-1
Thickness of 102kc /cm s-1 103Dlit/cm2s-1 103Dlit/cm2s-1 Deviation,% Deviation,%
of kc, %
Triton X-100
0 107.15 ± 0.44a - 205.05 ± 0.03a 205.41 223.53 0.2* 8.2#
1 59.69 ± 0.39a 44.3 208.98 ± 0.02a 205.41 223.53 1.7* 6.5#

2 51.15 ± 0.29a 52.3 204.68 ± 0.03a 205.41 223.53 0.4* 8.4#

3 7.38 ± 0.25a 93.1 212.57 ± 0.02a 205.41 223.53 3.4* 4.9#

4 7.10 ± 0.07a 93.4 209.75 ± 0.02a 205.41 223.53 2.1* 6.2#

Mean values 208.21 ± 0.02 (1.6*)c (6.8#)c
Precision, % 99.9b

Table 2. Rate Coefficients for the Evaporation of Ethanol, kc, and Diffusion Coefficients of Its Vapors Into Nitrogen,
Dfound, Under the Effect of Various Amounts of Surfactant Triton X-100

Monolayer
Retardation 103Dfound/cm2s-1
Thickness of 102kc /cm s-1 103Dlit/cm2s-1 103Dlit/cm2s-1 Deviation,% Deviation,%
of kc, %
Triton X-100
0 195.11 ± 0.05a - 156.30 ± 0.03a 156.30 158.26 0.0* 1.2#
1 171.32 ± 0.22a 12.19 153.79 ± 0.03a 156.30 158.26 1.7* 2.8#

2 106.33 ± 0.25a 45.50 155.22 ± 0.03a 156.30 158.26 0.8* 1.9#

Monolayer
Retardation 103Dfound/cm2s-1
Thickness of 102kc /cm s-1 103Dlit/cm2s-1 103Dlit/cm2s-1 Deviation,% Deviation,%
of kc, %
Triton X-100
3 101.76 ± 0.30a 47.84 156.76 ± 0.03a 156.30 158.26 0.2* 0.9#
4 85.96 ± 0.29a 55.94 154.20 ± 0.02a 156.30 158.26 1.4* 2.6#
Mean values 155.25 ± 0.03 (0.8*)c (1.9#)c
Precision, % 99.9b
a
Uncertainty obtained from the standard error of the kc and D values, estimated from the slopes of the linear plots of Eqs. 20 and 21 of
Ref. 35, respectively.
b
Precision determined from the mean value and the standard error of the experimentally obtained diffusion coefficients.
c
Mean deviation of the experimental diffusion coefficients from the respective predicted*,36 and literature#,37 values, Dlit.

Figure 7. Variation of the rate, kc, for the evaporation of methanol (rectangle) and
ethanol (triangle) under various monolayer(s) coverage of Triton X-100.

Figure 8. Plots of the % reduction of evaporation of methanol (rectangle) and ethanol

(triangle) under various monolayer(s) coverage of Triton X-100.

There are two main factors that contribute in the evaporation rate – the
presence of stagnant gaseous (nitrogen in this case) and liquid layers located at
the interphase through which the solute must diffuse (the liquid being Triton
X-100 monolayer(s) in this study) (Gavril et al., 2006; H.H. Mohammad et al.,

2013). Drastic retardation of the evaporation is due to the presence of adsorbed

monolayers as discussed in previous literature (Gavril et al., 2006; H.H.
Mohammad et al., 2013). However, the retardation of evaporation of both
liquids becomes significant (>40%) at a coverage of 2 to 4 Triton X-100
monolayers, higher than those predicted from the Gibbs surface excess (Gavril
et al., 2006; H.H. Mohammad et al., 2013) suggesting the formation of an
insoluble monolayer of surfactant. The insoluble monolayer of surfactant will
further suppress the evaporation rate of both liquids as shown by the
decreasing of the evaporation rates of both liquids due to an additional more
than 2 monolayers of the surfactant as shown in Table 1 and 2.
The movement of the vapor (methanol or ethanol) in the Triton X-100, is
shown in the Figure 9. The molecules try to diffuse to the “free” surface across
the surfactant monolayer(s) before it reach the surface of the liquid before
being further evaporated. The molecules move randomly as depicted by the
random walk model (Giddings, 1965). However, the random movement
indirectly created a “concentration” gradient since the molecules move from
higher to lower concentration. Katsanos et al. Has used this understanding
with the assistance of first Fick’s law of diffusion to formulate equations to
study transport phenomena across the liquid-gas interphase by RF-GC.
The addition of Triton X-100 affects less the evaporation of ethanol
compared to that of methanol. Both liquids are polar protic compounds, which
can stabilize both the surfactant cationic group through uncoupled electron
pairs, as well as the anionic group through hydrogen bonding, which results in
a more favorable orientation of a densely packed adsorption surfactant layer
(Gavril et al., 2006). Since Triton X-100 is a non-ionic surfactant, the surface-
active portion bears no apparent ionic charge, and thus will adsorb onto
surfaces with either the hydrophilic or the hydrophobic group oriented toward
the surface (Gavril et al., 2006). Since methanol has higher dielectric and
dipole moment bond values compared to ethanol (Chemistry, 2006), methanol
has a higher ability to donate its uncoupled electron pairs to form a hydrogen
bond with the hydrophilic group of the surfactant. This will result in the
adsorption of the surfactant with its hydrophilic group oriented toward the
surface (Gavril et al., 2006; Rosen, 1989). However, at lower coverage (in the
absence of polar protic solvent), hemimicele formation may occur as the
hydrophobic group may be displaced by a hydrophilic group and thus causing
lateral interactions between adjacent hydrophobic groups. As a result, the
nonionic surfactant may lie prone on the surface of the liquid (Gavril et al.,
2006; Partyka, Zaini, Lindheimer, & Brun, 1984)

Figure 9. Movement of the liquid molecules through the surfactant monolayer(s).

5. CONCLUSION
The retardation of evaporation rates, kc of both liquid pollutants -
methanol and ethanol is due to the formation of the “theoretical” adsorbed
monolayer(s) of Triton X-100 at the liquid surface. The retardation values
become significant (>40% in both liquids) with an addition of more than 2
monolayers of surfactant, due to formation of an insoluble monolayer and
further addition of surfactant will result multilayer formation. The variation of
the retardation values between the two alcohols – methanol and ethanol are
due to ability of the liquids to form a hydrogen bond with the hydrophilic
group of the surfactant as discussed earlier. For future work, the author will try
to investigate the orientation of the surfactant at the liquid-gas interphase,
which can be done by using BAM imaging (Moroi, Rusdi, & Kubo, 2004); and
the formation of the insoluble monolayer as well as the formation of the
multilayer can be explained once the images are obtained.

ACKNOWLEDGMENTS
The work was funded by the University of Malaya under Grant
RG045/09SUS. The authors want to dedicate special thanks to Dr. Tay Kheng
Soo for his thoughts and criticisms on the findings of the experiments; as well
as to Miss Kumuthini A/P Chandrasekaram for her assistance on tensiometer
usage.

NOMENCLATURE
Roman Letter

aL free surface area of the liquid

c concentration of a solute vapor concentration in the sampling column
c0 equilibrium vapor concentration, initial concentration
cL concentration of the adsorbed solute in the bulk liquid phase
D mutual diffusion coefficient of two gases
h height of a sample peak measured from the ending baseline
h∞ infinity peak height defined by equation (5)
kc evaporation rate of liquid
KG overall mass transfer coefficient in the gas phase
l, l’ lengths of two sections of the sampling column
s-1 per second(s)
t0 time from the beginning to the last backward reversal of gas flow
v linear velocity of carrier gas in interparticle space of the sampling
column

Superscript

2 power of two (squared)

Subscript

0 initial
-1 reciprocal
∞ infinity
c concentration of liquid vapor in the sampling column
G gas phase

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by gas chromatography. Journal of Chromatography A, 1037, 147-189.
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of Pure Liqulds and Diffusion Coefficients of Vapors. Journal of Physical
Chemistry, 88, 3674-3678.
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chromatography. Journal of Chemical Society, Faraday Transaction 1, 78,
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adsorption equilibrium constant by reversed-flow gas chromatography.
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diffusion coefficients in multicomponent gas mixtures by the reversed-
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Gases by the Reversed-Flow GC Technique. Journal of Chromatographic
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heterogeneous catalysis. Journal of Chemical Society, Faraday
Transaction I, 78, 1051.
Katsanos, N. A. (1988). Flow Perturbation Gas Chromatography. New York:
Marcel Dekker Inc.
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diffusion coefficients measured by the reversed-flow sampling technique.
Journal of Chromatography A, 254(0), 15-25. doi:http:// dx.doi.org/ 10.
1016/S0021-9673(01)88314-X.
Katsanos, N. A. & Karaiskakis, G. (1984). In J. C. Giddings (Ed.), Advances
in Chromatography, (pp. 138). New York: Marcel Dekker Inc.
Katsanos, N. A., Karaiskakis, G. & Niotis, A. (1984). The Reversed-Flow
Technique applied in Heterogeneous Catalysis with complicated Kinetics.
Paper presented at the Proceedings of the 8th International Congress on
Catalysis, West Berlin.
Katsanos, N. A., Karaiskakis, G. & Niotis, A. (1985). Catalytic
hydrodesulfurization of thiophene studied by the reversed-flow gas
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of Evaporated n-Heptane using RF-GC Methodologies. Oriental Journal
of Chemistry, 27(2), 559-562.
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of the Liquid Pollutants Using Reversed Flow-Gas Chromatographic
Methodologies. Paper presented at the The 5th Mathematics and Physical
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Pollutant Using RF-GC Methodologies. Paper presented at the
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154.
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Chemical Society, 62, 1583.

BIOGRAPHICAL SKETCH
1. H.H. Mohammad

Mohammad Hafiz Bin Hamzah (H.H. Mohammad) was born on 15

December 1987 in Lumut, Perak, Malaysia. He obtained the Bachelor of
Degree in Education (majoring in chemistry) and Master of Science
(Analytical Chemistry) from University of Malaya in the year of 2011 and
2015 respectively. Being offered to do a PhD at Universiti Malaya in
Environmental Chemistry. Currently, he is waiting for the scholarship from
any organization to support his doctorate studies. He has experienced on
teaching secondary school for a year before deciding to continue his studies in
area of chemistry. Mr. H.H. Mohammad has served as research assistant for
two years under the grant rg045/09sus “studies of the flux of gaseous pollutant
across air-water interface using reversed-flow gas chromatography (RF-GC)
TECHNIQUES” which comes under the niche of sustainable science. Mr.
H.H. Mohammad is also one of the recipient of fellowship from University
Malaya under the “Skim Biasiswazah”, the prestigious fellowship given by the
university to undergraduate student to pursue higher degree. Current working
in the project entitled “Physiochemical Measurements and Enviromental
Applications Of Reversed-Flow Gas Chromatography (RF-GC)” (Project
Number: PG067-2013A and SAGA Project Number: 6000267) under
supervision of Project Leader, Prof. Dr. Sharifuddin Bin Md Zain and Pakar
Umum Mardi, Khalisanni Khalid. The grant was granted by The Institute of
Research Management & Monitoring (Institut Pengurusan & Pemantauan

Penyelidikan), IPPP, Universiti Malaya (UM), Kuala Lumpur Malaysia. He

has published one publication entitled, “Study the Effect of Imposing
Surfactants toward the Evaporation of Low Molecular Weight Alcohol”.

2. Rashid Atta Khan

Rashid Atta Khan received his PhD from University of Patras, Athens,
Greece back to 2006. His PhD thesis entitled “Development of new
chromatographic methods for the study of exchange of pollutants between the
atmosphere and the water environment” has made an impact in the field of
Reversed-Flow Gas Chromatography since he got the directly supervised by
the inventor of the methodologies which is G. Karaiskakis. He major interest is
in analytical chemistry. Associate Professor Khan is currently a member of
American Chemical Society, since 2009, and The chemical society of
Pakistan, Member, since 2004. He is also a course coordinator SCES 3311,
Advance Analytical Chemistry, University Malaya, from 01-Jan-07 to 01-Jul-
12.

3. Khalisanni Khalid

Khalisanni Khalid was born in Ipoh in 1985. He pursued his studies in

Universiti Teknologi MARA (UiTM) and graduated with a BSc. (Hons.) in
Applied Chemistry at the end of 2007. After a year as a research assistant in
University of Malaya, he was offered the University Malaya Fellowship (UM),
Postgraduate Study Scheme (KPT), Postgraduate Dana (MOSTI) and National
Science Fellowship (NSF). He chose National Science Fellowship to read the
master’s degree in Universiti Malaya.
Upon study, he was appointed as residential assistance for PERMATA
Pintar Program in Universiti Kebangsaan Malaysia. He flew away to Thailand
and Singapore to give the speech on his research. His diligence was rewarded
with a degree in Master of Science in Physical/ Environmental Sciences in
2011. Before graduation, he was offered to join Malaysian Agricultural
Research and Development Institute (MARDI). There onwards, his interest of
research in science and business grew. This was further encouraged by the
recognition and support from MARDI, where he was appointed as Technical
Officer for MARDI Kuala Linggi Incubator Program. This project leads him to
train SMEs for essential oil production. In MARDI Headquarters Serdang, he
is responsible to lead Essential Oil Analysis Unit under Food and Agricultural
Analysis Laboratory Program, Technical Service Centre. He is also the
gatekeeper for Malaysian Herbal Authentication Centre (MHAC).

Mr. Khalid has exposed over 5 years in diverse research areas especially
research ethics, essential oil, polymer, biofuel, fermentation, analytical and
environmental chemistry. He has been honoured and recognised both
nationally and internationally for his research creativity and innovativeness. At
his age of 28, he has published more than 60 articles in books, book chapters,
and proceedings of which more than 30 articles in refereed journals.

EBSCO Publishing : eBook Collection (EBSCOhost) - printed on 10/3/2018 2:19 PM via UNIVERSIDAD DE
ANTIOQUIA
AN: 1540094 ; Warren, Valerie.; Gas Chromatography : Analysis, Methods and Practices
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In: Gas Chromatography ISBN: 978-1-53611-990-9
Editor: Valerie Warren © 2017 Nova Science Publishers, Inc.

Chapter 3

THE APPLICATION OF HEADSPACE:

SOLID-PHASE MICROEXTRACTION
(HS-SPME) COUPLED WITH GAS
CHROMATOGRAPHY/MASS SPECTROMETRY
(GC/MS) FOR THE CHARACTERIZATION
OF POLYMERS

Peter Kusch*
Hochschule Bonn-Rhein-Sieg, University of Applied Sciences,
Department of Applied Natural Sciences, Rheinbach, Germany

ABSTRACT
Solid-Phase Microextraction (SPME) is a very simple and efficient,
solventless sample preparation method, invented by Pawliszyn and co-
workers at the University of Waterloo (Canada) in 1989. This method
has been widely used in different fields of analytical chemistry since
its first applications to environmental and food analysis. SPME integrates
sampling, extraction, concentration and sample introduction into a single
solvent-free step. The method saves preparation time, disposal costs and
can improve detection limits. It has been routinely used in combination
with gas chromatography (GC) and gas chromatography/mass

*
Corresponding Author address Email: [email protected].

spectrometry (GC/MS) and successfully applied to a wide variety of

compounds, especially for the extraction of volatile and semi-volatile
organic compounds from environmental, biological and food samples.
Since the last twenty years, SPME in headspace (HS) mode is used
as a valuable sample preparation technique for identifying degradation
products in polymers and for determination of rest monomers and other
light-boiling substances in polymeric materials. For more than ten years,
our laboratory has been involved in projects focused on the application
of HS-SPME-GC/MS for the characterization of polymeric materials
from many branches of manufacturing and building industries. This
book chapter describes the application examples of this technique for
identifying volatile organic compounds (VOCs), additives and
degradation products in industrial plastics, rubber, and packaging
materials.

Keywords: HS-SPME, GC/MS, polymers, volatile organic compounds

(VOCs), identification

INTRODUCTION
Sample preparation is an essential step in analysis, greatly influencing the
reliability and accuracy of resulted time and cost of analysis. Most of modern
sampling methodologies for chromatographic analysis involve one of the basic
mass transfer processes, alone or in combination: partition (where analytes are
removed from samples by dissolution in a proper solvent), adsorption (the
analyte are bonded or retained over the solid surface) and volatilization
(volatile target species are selectively vaporized and separated from the matrix
and interfering compounds) [1]. Solid-Phase Microextraction (SPME) is a very
simple and efficient, solventless sample preparation method, invented by
Pawliszyn and co-workers at the University of Waterloo (Canada) in 1989 [2-
4]. This method has been widely used in different fields of analytical
chemistry since its first applications to environmental and food analysis.
SPME integrates sampling, extraction, concentration and sample introduction
into a single solvent-free step. Solutes from a sample are directly extracted
into an absorptive polymeric layer coated onto a solid fused silica fiber. After
some time of exposure of fiber to the sample, equilibrium is reached and the
extracted mass is, from this moment on, maximized and constant. The amount
of extracted analytes is proportional to their concentration in the sample. Then
the SPME fiber and captured solutes are transferred into an injection-system
that desorbs the solutes into a gas mobile phase (helium) of the gas

chromatograph (GC). At the same time the analysis run is started. The method
saves preparation time, disposal costs and can improve detection limits. It has
been routinely used in combination with gas chromatography (GC) and gas
chromatography/mass spectrometry (GC/MS) and successfully applied to a
wide variety of compounds, especially for the extraction of volatile and semi-
volatile organic compounds from industrial, environmental, biological and
food samples [5].
Since the last twenty years, SPME in headspace (HS) mode is used as a
valuable sample preparation technique for identifying degradation products in
polymers and for determination of rest monomers and other light-boiling
substances in polymeric materials [6-12]. For more than ten years, our
laboratory has been involved in projects focused on the application of HS-
SPME-GC/MS for the characterization of polymeric materials from many
branches of manufacturing and building industries. This book chapter
describes the application examples of this technique for identifying volatile
organic compounds (VOCs), additives and degradation products in industrial
plastics, rubber, and packaging materials.

Prinziples of SPME

In SPME, a small amount of the extracting phase associated with a solid

support is placed in contact with the sample matrix for a predetermined
amount of time. If the time is long enough, concentration equilibrium is
established between the sample matrix and the extraction phase. When
equilibrium conditions are reached, exposing the fiber for a longer amount of
time does not accumulate more analytes [13]. The amount of solute in the
SPME layer at equilibrium (Mi,SPME) can be approximated by the following
equation 1:

Mi,SPME~Ki,SPME VSPMECi (1)

where Ki,SPME is an aggregate solute distribution constant between the SPME

absorptive layer and the sample, VSPME is the volume of the SPME layer, and
Ci is the solute concentration in the sample before performing SPME sampling
[14]. Equation 1 assumes that the sample volume is much greater than the
volume of the SPME layer. SPME coatings typically have thicknesses of about
10-100 µm typically around 10 times the film thickness range normally
encountered in capillary GC columns. Standard SPME layers, with smaller

volumes, would imply correspondingly smaller minimum sample volumes

[14]. SPME coatings can be classified primarily into four categories: by the
type of coating, by the coating thickness, by polarity and by whether the
coating is an absorbent or an adsorbent [15]. A listing of commercial fibres
available from Supelco is shown in Table 1 [15, 19]. The type of phase applied
determines the polarity of the coating. Polarity can provide selectivity by
enhancing the affinity of the coating for polar analytes compared to a non-
polar fibre coating. Essentially, all SPME fibres are bipolar to some degree
because they will extract both polar and non-polar analytes [15].

Table 1. Summary of commercially available SPME fibres [15, 19]

Fibre coating Film Polarity Coating Maximum Technique Compounds

thickness method operating to be
(µm) temperature analysed
(°C)
Polydimethylsiloxane 100 Non - Non-bonded 280 GC/HPLC Volatiles
(PDMS) polar
Polydimethylsiloxane 30 Non- Non-bonded 280 GC/HPLC Non-polar
(PDMS) polar semivolatiles
Polydimethylsiloxane 7 Non- Bonded 340 GC/HPLC Medium- to
(PDMS) polar non-polar
semivolatiles
PDMS–Divinylbenzene 65 Bipolar Partially 270 GC Polar
(DVB) cross-linked volatiles
PDMS–Divinylbenzene 60 Bipolar Partially 270 HPLC General
(DVB) cross-linked purpose
Polyacrylate (PA) 85 Polar Partially 320 GC/HPLC Polar
cross-linked semivolatiles
DVB–Carboxen-PDMS 50/30 Bipolar Highly 270 GC Odours and
cross-linked flavours
Carboxen–PDMS 75 Bipolar Partially 320 GC Gases and
cross-linked volatiles
Carboxen–PDMS 85 Bipolar Highly 320 GC Gases and
cross-linked volatiles
Polyethylene glycol 60 Polar Partially 250 HPLC Surfactants
(PEG) (Carbowax) cross-linked
Carbowax–DVB 65 Polar Partially 265 GC Polar analytes
cross-linked
Carbowax–DVB 70 Polar Highly 265 GC Polar analytes
cross-linked

Figure 1. Schematic view of a SPME manual fibre assembly holder. Reprinted from
[15] with permission from Elsevier.

Figure 2. Schematic illustration of a SPME device. A) SPME device with sampling

vial. B) Fiber assembly. C) Extraction mechanism in the three-phase system. Reprinted
from [17] with permission from ACS.

Figure 3. Steps of typical SPME extraction and thermal desorption in GC injector.

Reprinted from [15] with permission from Elsevier.

Figures 1-2 show the schematic view of the first commercial version of
the SPME manual fibre assembly holder (SPME device) introduced by
Supelco in 1993 [15-19]. The manual holder has a z-slot to lock the fibre in the
exposed position. When the plunger is unlocked, the fibre will retract into the
needle if it is a manual assembly. The holder designed for autosamplers does
not contain the needle guide depth gauge or the z-slot. It is simply a straight
slot. The process of sampling is illustrated in Figure 3 [15]. The sample is
placed in a glass vial, which is sealed with a septum-type cap. The new SPME
fibre should be conditioned before using, and cleaned after analyzing.
Cleaning can be done by inserting the fibre in an auxiliary hot injection port or
by inserting into a syringe cleaner. When the SPME needle pierces the septum
and the fibre is extended through the needle into the sample (Figure 3),
partitioning between the sample matrix and the stationary phase takes place.
This may occur in two different ways: headspace (HS-SPME) or direct
immersion (DI-SPME). In HS-SPME, the fibre is exposed in the vapour phase
above a gaseous, liquid or solid sample. In DI-SPME, the fibre is directly
immersed in liquid samples. Agitation of the sample is often carried out with a
small stirring bar for liquid samples or by sonication of solid samples for HS-
SPME to decrease the time necessary for equilibration. For liquid polymeric
SPME coatings, the amount of analyte absorbed by the coating at equilibrium

is directly related to the concentration of the analyte in the sample according to

the equation 2 [16-18]:

n = KfsVfC0Vs/KfsVf + Vs (2)

where:

n = mass of analyte absorbed by coating

C0 = initial concentration of analyte in sample
Kfs = partition coefficient for analyte between coating and sample matrix
Vf = volume of coating
Vs = volume of sample

This equation shows that the relationship between the initial concentration
of analyte in the sample and the amount of analyte absorbed by the coating is
linear [16-18].
The mass of the analyte absorbed by the coating at equilibrium for HS
SPME can be expresses as in the equation 3 [18]:

n = KfsVfC0Vs/KfsVf + KhsVh + Vs (3)

where:

n = mass of analyte absorbed by coating

C0 = the initial concentration of the analyte in the matrix
Kfs = the fibre/headspace distribution constant
Khs = the headspace/sample distribution constant
Vf, Vh and Vs are the volumes of the coating, the headspace and the
matrix, respectively.

After a suitable extraction time the fibre is withdrawn into the needle, the
needle is removed from the septum and is then inserted directly into the hot
injection port of the GC or GC/MS system (Figure 3). The analytes are
thermally desorbed and transferred by a carrier gas to the capillary column.
Desorption temperature must be high enough, so that the solutes rapidly leave
the SPME fiber. A desorption that is too slow may lead to peak broadening
and tailing unless additional arrangements are made for trapping solutes at the
beginning of the GC column before temperature-programmed elution.
Conversely, too high of an inlet temperature may induce thermal

decomposition and introduce some contaminants into the column from septum
bleed, as well as from the SPME layer itself [14]. The HS- and DI-SPME
techniques can be used in combination with any GC or GC/MS equipment
[19].

EXPERIMENTAL
Samples

Samples (A and B) of commercially available expanded polystyrene

(EPS, Styropor) and polyurethane packaging foam (PUR) from Germany,
poly(acrylonitrile-co-1,3-butadiene-co-styrene)/polycarbonate (ABS/PC) and
poly(acrylonitrile-co-1,3-butadiene-co-styrene)/polyamide-6 (ABS/PA 6)
blends, car wrapping foils and rubber membranes from the hydraulic cylinders
(all samples from the German automotive industry), as well as samples of
poly(vinyl chloride) (PVC) floor covering from a day nursery were used for
investigation.

Solid-Phase Microextraction (SPME)

The SPME fiber holder for manual use and the 75-µm Carboxen-
Polydimethylsiloxane (CAR/PDMS) fibers obtained from Supelco (Bellefonte,
PA, USA) were used for extraction.
The fiber was conditioned at 300°C for one hour prior to first use.
Twenty-milliliter headspace glass vials with an aluminum-coated silicone
rubber septum and pressure released aluminium seal, obtained from LABC
Labortechnik (Hennef, Germany) were used. A Sonorex Super RK 31H
compact ultrasonic bath from Bandelin electronic (Berlin, Germany) was
employed at 60°C for sample agitation.

SPME Procedure

Ca. 50 mg of the solid sample was sealed in a twenty-milliliter headspace

glass vial with aluminum-coated silicone rubber septum. The septum of the
vial was pierced with the needle of the SPME device and the fiber was
exposed approximately 10 mm above the solid sample. Afterwards the glass

vial with the SPME injector was placed in an ultrasonic bath and agitated by
sonication for 15 min at 60°C. After a sorption time of 15 min in the
headspace above the sample, the fiber was retracted into the protective sheath
and removed from the headspace glass vial. It was transferred without delay
into the injection port of the gas chromatograph/mass spectrometer. The fiber
was thermally desorbed in the injection port at 250°C for one minute and the
GC/MS run was started.

Instrumentation and Analytical Conditions

A 7890A gas chromatograph (GC) with a series 5975C quadrupole mass

spectrometer (MS) (Agilent Technologies Inc., Santa Clara, CA, USA)
operated in electron impact ionization (EI) mode was used for measurments.
The fused silica GC capillary column (30 m long, 0.25 mm I.D.) with DB-
5MS UI stationary phase, film thickness 0.25 μm (J&W Scientific, Folsom,
CA, USA) was used for chromatographic separations. Helium, grade 5.0
(Westfalen AG, Münster, Germany) was used as a carrier gas at constant flow
of 1.1 cm³/min. The gas chromatographic conditions were as follows:
programmed temperature of the capillary column from 60°C (1 min hold) at
7°C/min to 280°C (hold to the end of analysis); the temperature of the
split/splitless injector was 250°C and the split ratio was 5:1.
The transfer line temperature was 280°C. The MS EI ion source
temperature was kept at 230°C.
The ionization occurred with a kinetic energy of the impacting electrons of
70 eV. The quadrupole temperature was 150°C. Mass spectra and
reconstructed chromatograms (TIC) were obtained by automatic scanning in
the mass range m/z 35-750 u. GC/MS data were processed with the
ChemStation software (Agilent Technologies) and the NIST 05 mass spectral
library.

RESULTS AND DISCUSSION

Among volatile monomers, residual solvents and impurities, the
commercial plastics and rubbers always contain low-molecular-weight
additives. These compounds are essential in polymer or copolymer processing
and in ensuring the end-use properties of a polymer or copolymer. Additives
can improve or modify the mechanical properties (fillers and reinforcements),

modify the color and appearance (pigments and dyestuffs), give resistance
to heat degradation (antioxidants and stabilizers), provide resistance to
light degradation (UV stabilizers), improve the flame resistance (flame
retardants), improve the performance (antistatic or conductive additives,
plasticizers, blowing agents, lubricants, mould release agents, surfactants, and
preservatives) and improve the processing characteristics (recycling additives)
of polymers or copolymers [20]. Some of the additives accumulate in the
environment and affect our health and the environment. Knowledge of
additives is important for evaluating the environmental impact and interaction
of polymeric materials, investigating long-term properties and degradation
mechanisms, verifying ingredients, investigating manufacturing problems,
qualifying control polymeric materials, identifying odorants, avoiding
workplace exposure and insuring safety of food packaging and medical
products. Identification of polymer or copolymer additives is also desired if
competitor products are investigated [20].
For about 15 years, our laboratory has been involved in projects from the
area of failure analysis in the automotive, chemical or rubber industry by using
the pyrolysis-GC/MS and headspace-SPME-GC/MS. The practical application
of these analytical techniques ranges from case studies of automotive
components failure analysis of failed hydraulic cylinders, membranes, as well
as the packaging materials, sealing rings, tire materials and additives, to auto
paints or auto wrapping foils. The obtained analytical results are then used for
troubleshooting and remedial action of the technological process. Here, I
report on application examples of the headspace-SPME-GC/MS method for
identification of volatile organic compounds and additives in polymers and
rubbers from packaging, automotive and domestic materials.

Identification of Volatile and Semivolatile Organic Compounds

in Packaging Materials

Packaging is a major end-use for four primary plastics, as high-density

polyethylene (HDPE), low-density polyethylene (LDPE), polypropylene
(PP) and polystyrene (PS). Thermoplastic polyesters, such as bottle-grade
poly(ethylene terephthalate) (PET), find extensive use in the soft-drink bottle
market. Knowledge about the content of volatile residual solvents, monomers,
and impurities or additives, for example, plasticizers and UV stabilizers, in
such plastics is important if the material is used in the packaging of food,
beverages, cosmetics or medicines. The substances may affect the quality of

products stored inside, if they migrate through the plastic. Because of

problems with the direct gas chromatographic (GC) analysis of a polymer
solution, the organic emissions from plastics are usually controlled by various
hyphenated gas chromatographic techniques, for example, coupling of GC
with headspace (HS) [21], with thermal desorption (TD) [22], with pyrolysis
(Py) [20], and more recently, with solid-phase microextraction (SPME) [6-12,
23-26].

Expanded Polystyrene (EPS)

EPS is produced by polymerizing styrene monomer and adding iso-
pentane as a blowing agent. It is used for food packaging and for protection of
products against damage during transport and storage. EPS is also used in the
building industry for insulation of exterior walls and foundations.

Figure 4. Total ion current GC/MS chromatograms (TIC) obtained from the headspace
of two extracted EPS (expandable polystyrene) samples A and B.

Table 2. Volatile organic compounds released from expanded polystyrene

(EPS) by headspace-SPME-GC/MS at 60°C

Peak Retention Identified compound CAS

No. time tR [min] EPS sample A EPS sample B Number
1 2.02 Carbon dioxide Carbon dioxide 124-38-9
2 2.17 2-Methylbutane 2-Methylbutane 78-78-4
3 3.71 Toluene 108-88-3
4 4.97 Ethylbenzene Ethylbenzene 100-41-4
5 5.11 p-Xylene 106-42-3
6 5.48 Styrene Styrene 79637-11-9
7 6.04 Cumene Cumene 98-82-8
8 6.45 2- 2-Propenylbenzene 300-57-2
Propenylbenzene
9 6.60 Propylbenzene Propylbenzene 103-65-1
10 6.77 Benzaldehyde Benzaldehyde 100-52-7
11 7.15 α-Methylstyrene 98-83-9
12 7.35 1-Ethenyl-2- 1-Ethenyl-2-methylbenzene 611-15-4
methylbenzene
13 7.99 2-Ethyl-1- 104-76-7
hexanol
14 8.90 Acetophenone Acetophenone 98-86-2
15 9.28 Benzenemethanol 100-51-6
16 9.63 α-Methylbenzeneacetaldehyde 93-53-8
17 12.26 β-Methylenebenzeneethanol 6006-81-1

It has been known for a long time that EPS emits residual styrene
monomer and other volatile organic compounds (VOCs) at ambient
temperature. Styrene is harmful when inhaled, it is irritating to eyes, nose,
throat, skin, and acts as a depressant on the central nervous system, causing
neurological impairment [10, 11]. In my investigation, headspace-SPME
followed by gas chromatography/mass spectrometry (GC/MS) has been
applied to the identification of volatile organic compounds (VOCs) released
from expanded polystyrene (EPS) at 60°C. Figure 4 shows typical total ion
current GC/MS chromatograms (TIC) obtained from the headspace of two
extracted EPS samples (A and B). Identification of compounds was carried out
by comparison of retention times and mass spectra of standards, study of the
mass spectra and comparison with data in the NIST 05 mass spectral library.
The retention data and the summarizing of the identification results are given
in Table 2. As can be seen from Table 2, the headspace above the EPS
samples contains residual styrene monomer, impurities of styrene such as alkyl

benzenes, and oxidation products, as well as residual 2-methylbutane

(iso-pentane) used as a blowing agent by polymerizing of EPS. A part of the
identified VOCs also can be formed by thermooxidative degradation of EPS
when exposed to high temperatures and solar irradiation [11].

Polyurethane (PUR) Foam

Polyurethanes (PUR) are a large family of polymers whose composition
has evolved over time. Polyurethane foams are largely used in automobiles,
home furniture and thermal insulation. Approximately 13 kg of polyurethane
foams are used in a car [27]. The applications range from seat cushions to
headrests, instrument panel foams and headliners. Polyurethanes are also
widely present in museum collections such as natural history museums, fine
art museums, modern art museums, either as a part of the artefacts, or as a
material for their conservation (stuffing, protection, packaging and storage)
[25, 26]. Among museum collections they feature predominantly as sculptures,
design objects, cushioning materials, textiles and toys [25, 26]. Polyurethane
foams are regarded as potential causes of VOCs emissions.
Figure 5 shows the total ion current GC/MS chromatogram (TIC) obtained
from the headspace of the investigated packaging polyurethane foam (PUR).
The results of GC/MS identification are summarized in Table 3. As can be
seen from Table 3, the low molecular weight compounds contain alkyl
aldehydes and residual solvents, like tripropylene glycol monomethyl ether
and tri(1,2-propylene glycol) monomethyl ether. Of the semivolatile organic
compounds (SVOCs) phenolic antioxidants (2,6-di-tert-butyl-4-methylphenol
and 3,5-di-tert-butyl-4-hydroxybenzaldehyde) were detected as well as
plasticizers, like diisobutyl adipate and diethyl-, dibutyl- and diisobutyl
phthalates. Phthalate esters are produced all over the world in large quantities
for different uses. One important application is the use as a polymer
plasticizer. The release of phthalates into the environment may occur during
production and distribution and due to migration from polymeric materials
[24]. Due to the widespread use, they have become common organic
pollutants. In recent years, considerable attention has been paid to human
exposure to phthalates because they are suspected to cause various health
effects and possess carcinogenic and estrogenic properties [24, 28].

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Figure 5. Total ion current GC/MS chromatogram (TIC) obtained from the headspace of the packaging polyurethane foam (PUR).

Table 3. Volatile and semi-volatile organic compounds released from

polyurethane (PUR) foam by headspace-SPME-GC/MS at 60°C

Peak Retention Identified compound Chemical structure

No. time tR [min]
1 7.53 1-Octanal
2 7.99 2-Ethyl-1-hexanol

3 9.62 1-Nonanal
4 11.72 1-Decanal
5 13.65 Tripropylene glycol monomethyl
ether (Dowanol 62 b)
6 13.74 Tri(1,2-propylene glycol)
monomethyl ether

7 15.50 n-Tetradecane
8 16.62 Not identified
9 16.70 2,6-Di-tert-butyl-p-benzoquinone

10 17.41 2,6-Di-tert-butyl-4-methylphenol
(BHT)

11 18.83 Diethyl phthalate

12 19.03 n-Hexadecane
13 19.45 2,6-Di-tert-butyl-4-sec-butylphenol

14 20.36 Diisobutyl adipate

15 20.68 Not identified

16 21.63 3,5-Di-tert-butyl-4-
hydroxybenzaldehyde

17 23.09 Diisobutyl phthalate

18 24.45 Dibutyl phthalate

Emission of Volatile and Semivolatile Organic Compounds from

Polymers/Copolymers from the Automotive Industry

Plastic materials are viewed as the culprits for the VOCs emission in
vehicle cabins. Material testing for outgassing volatile organic chemicals is
required in many industries to ensure consumers are not being exposed to
harmful contaminants. This is especially important when a material such as a
plastic is exposed to excess heat with little or no ventilation. A good example
would be plastic materials in a car such as dashboards, which are exposed to
very high temperatures in direct sunlight.
For determination of volatile organic compounds in a variety of solid
waste matrices the US EPA 8260B GC/MS method is used [29]. This method
is applicable to nearly all types of samples, regardless of water content,
including various air sampling trapping media, ground and surface water,
aqueous sludges, caustic liquors, acid liquors, waste solvents, oily wastes,
mousses, tars, fibrous wastes, polymeric emulsions, filter cakes, spent carbons,
spent catalysts, soils, and sediments. The US EPA 8260B GC/MS method can
be used to quantitate most volatile organic compounds that have boiling points
below 200°C [29].
In this investigation, headspace-SPME-GC/MS method was used for the
identification of volatile and semivolatile organic compounds in polymers/
copolymers from the automotive industry. Some application examples are
described below.

ABS/PC Blend
Poly(acrylonitrile-co-butadiene-co-styrene) (ABS) is a common
thermoplastic used in light, rigid, and molded products such as automotive
body parts, musical instruments, household appliances, toys, and food
containers [30]. 1,3-Butadiene, acrylonitrile, and styrene are starting materials
in the production of ABS. In general, synthetic polymers contain residual
monomers, which remain in the polymers after the synthetic process. 1,3-
Butadiene is classified as a carcinogen by the International Agency for
Research on Cancer (IARC) and is a hazardous air pollutant. It is a potent
classical alkylating agent and its metabolites are reactive compounds that form
adducts with DNA or proteins [30]. Acrylonitrile is also believed to be
carcinogenic. The acute toxicity of styrene has been well studied, being a skin
and mucous membranes irritant and having narcotic properties [30]. Therefore,
analysis of the trace residual monomers remained in this copolymer is needed.

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Figure 6. Total ion current GC/MS chromatograms (TIC) obtained from the headspace of the extracted A) ABS/PC blend, B) ABS/PA 6
blend from the automotive industry.

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Figure 7. Total ion current GC/MS chromatograms (TIC) obtained from the headspace of the extracted car wrapping foils A (orange)
and B (black).

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Figure 8. Total ion current GC/MS chromatogram (TIC) obtained from the headspace of the extracted rubber membrane from the
hydraulic cylinder 1 from the automotive industry.

Table 4. Volatile and semi-volatile organic compounds released from

ABS/PC und ABS/PA 6 blends from the automotive industry by
headspace-SPME-GC/MS at 60°C

Peak Retention Identified compound Chemical structure

N. time tR [min] ABS/PC ABS/PA 6
1 4.97 Ethylbenzene Ethylbenzene

2 5.48 Styrene Styrene

3 6.98 Phenol

4 7.14 α-Methylstyrene

5 9.62 1-Nonanal
6 11.59 n-Tetradecane
7 11.72 1-Decanal
8 12.77 ɛ-Caprolactam

9 13.10 n-Hexadecene
10 18.83 Diethyl
phthalate

11 20.67 Not identified

Polycarbonate (PC) is a clear and transparent, hard and ductile

material. The great commercial success of bisphenol A polycarbonate (BPA-
PC) is due to its unique combination of properties: extreme toughness,
outstanding electrical insulation, transparency, good flame retardance,
excellent compatibility with several polymers, and high heat distortion
resistance. The electrical sector is the classical and major user of bisphenol A
polycarbonate. Typical applications include housings for car telephones and
distributor equipment, lamp sockets, relay parts, and components for electronic
calculators. The building and construction industry has become the second
most important user of polycarbonate [31]. Wall sheets from polycarbonates
are used as roofs for green houses, halls, and bus- or railway stations.
Polycarbonate is used in automobiles in light covers, reflectors, and fan or
radiator grills. In optical information storage systems, special grade BPA-PC is
used for production of audio/video compact discs (CD) [31]. This polymer is

widely used in reusable food packaging and in water and baby bottles. The
migration studies concerned the migration of bisphenol A (BPA) from
polycarbonate materials and information on other potential migrants. In the
study by Nerín et al. [32] the extract from a commercial polycarbonate
container consisted of a complex mixture containing monomers, oligomers,
UV stabilizers, antioxidants and degradation products. In the method
developed by Alin and Hakkarainen [33] headspace-SPME enabled extraction
and identification of low molecular weight compounds migrating from PC
containers during microwave heating in different food simulants. The migrants
could be detected at low detection limits and all the compounds could be
simultaneously quantified by using MHS-SPME (multiple headspace-SPME)
or direct injection depending on the food simulant used. As an example 4-
ethoxy-benzoic acid ethyl ester, 2,4-bis(1,1-dimethylethyl)-phenol and
benzophenone had detection limits of 1, 0.1 and 3 ng/L respectively in water
when extracted by the PDMS/DVB fibre.
In this work HS SPME-GC/MS was used for the identification of VOCs
and SVOCs that were emitted from ABS/PC blend used in the automotive
industry. Figure 6A shows the total ion current GC/MS chromatogram (TIC)
obtained from the headspace of the extracted ABS/PC blend at 60°C. The
identification results are summarized in Table 4. As can be seen from Table 4,
the headspace above the ABS/PC blend contain residual styrene monomer and
ethylbenzene (impurity of styrene) from ABS and phenol from thermal
degradation of polycarbonate. Other of the emitted VOCs like 1-nonanal and
1-decanal may be formed by thermooxidative degradation of the blend when
exposed to high temperatures and solar irradiation. The identified diethyl
phthalate was used as plasticizer.

ABS/PA 6 Blend
Polyamides (PA) known as nylons are polymers that contain an amide
group, -CONH-, as a recurring part of the chain. Polycaprolactam (PA 6) was
the first polyamide made in an I. G. Farben (Germany) laboratory in 1938 by
the hydrolytic polymerization of ε-caprolactam [31]. Today nylons are found
in appliances, business equipment, electrical/electronic devices, furniture,
hardware, machinery, packaging, and transportation. Transportation is the
largest market for nylons. The softer nylons are used in fuel lines, air brake
hoses, and coatings. Industrial applications are attracted to the excellent
fatigue resistance and repeated impact strength of nylons. Examples are
hammers and moving machine parts. Consumer products exploit the toughness

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90 Peter Kusch

of nylons in ski boots, ice and roller skate supports, bicycle wheels, kitchen
utensils, garden equipment, toys, and fishing lines [31].
Watanabe et al. [34] studied the thermal degradation of various
plastics at various temperatures from 70 to 300°C under oxygen-present
conditions to identify the semivolatile organic compounds (SVOCs) emitted
and to understand their thermal behaviors. The plastics examined were
nitrogen-containing polymers/copolymers, such as polyamide 6 (PA 6),
polyurethane (PUR), melamine-formaldehyde resin, urea-formaldehyde
resin and poly(acrylonitrile-co-1,3-butadiene-co-styrene) copolymer (ABS). ɛ-
Caprolactam was the predominant compound in SVOCs emitted from PA 6
[34]. This chemical is known as a raw material of PA 6 and also as the major
thermal-degradation product at high temperature.
Figure 6B shows the total ion current GC/MS chromatogram (TIC)
obtained from the headspace of the extracted ABS/PA 6 blend from the
automotive industry at 60°C. The identification results are summarized in
Table 4. As can be seen from Table 4, the headspace above the ABS/PA 6
blend contain residual styrene monomer and ethylbenzene (impurity of
styrene) from ABS and residual ɛ-caprolactam from PA 6. Also small amounts
of n-alkanes, like n-tetradecane and n-hexadecane were detected in the
headspace of ABS/PA 6 blend.

Car Wrapping Foils

The next objects of identification were car wrapping foils A and B. The
plastic material of the investigated foil A was identified by pyrolysis-GC/MS
in previous work of the author (P. K.) [35] as a mixture of flexible poly(vinyl
chloride) (PVC) with bis(2-ethylhexyl) phthalate (BEHP) plasticizer and
poly(hexamethylene adipamide) (Nylon 66). Figure 7A shows the obtained
SPME-GC/MS total ion chromatogram (TIC) of the headspace (HS) of
the extracted car wrapping foil A at 60°C. The identification results are
summarized in Table 5. As can be seen from Table 5, the headspace above
the car wrapping foil A (orange) contain alkyl alcohols (2-ethyl-1-hexanol,
methyloctanol and 1-nonanol), 1-decanal, p-tert-butylbenzoic acid and
dodecanoic acid. The identified 2-ethyl-1-hexanol is probably formed by
thermal decomposition of bis(2-ethylhexyl) phthalate plasticizer. Furthermore,
the antioxidant 2,6-di-tert-butyl-4-methylphenol (BHT) and its oxidized form
2,6-di-tert-butyl-p-benzoquinone were detected. The examined headspace
above the car wrapping foil A contains some plasticizers, like diisobutyl
adipate (fatty acid ester) and diethyl-, diisobutyl- and dibutyl phthalate
(phthalate plasticizers).

Table 5. Volatile and semivolatile organic compounds released from car

wrapping foil A (orange) by headspace-SPME-GC/MS at 60°C

Retention time tR [min] Identified compound Chemical structure

7.99 2-Ethyl-1-hexanol

10.37 Methyloctanol

10.97 1-Nonanol
11.72 1-Decanal
16.70 2,6-Di-tert-butyl-p-
benzoquinone

17.24 p-tert-Butylbenzoic acid

17.41 2,6-Di-tert-butyl-4-
methylphenol (BHT)

18.43 Dodecanoic acid

18.83 Diethyl phthalate

20.34 Bis(2-methylpropyl)
hexanedioate (Diisobutyl
adipate)
23.09 Diisobutyl phthalate

24.45 Dibutyl phthalate

Figure 7B shows the obtained SPME-GC/MS total ion chromatogram

(TIC) of the headspace (HS) of the extracted car wrapping foil B (black) at
60°C. The identification results are summarized in Table 6. At 60°C the car
wrapping foil B released various rest solvents like alkyl benzenes, 2-
butoxyethanol, diethylene glycol dimethylether or 3-methylheptyl acetate. The

main component of the headspace above the foil B is the residual monomer 2-
ethylhexyl acrylate (EHA) (retention time 12.16 min). 2-Ethylhexyl acrylate is
a major base monomer for the production of acrylic adhesives. This adhesive
is the main component of the analyzed car wrapping foil B.

Table 6. Volatile organic compounds released from car wrapping foil

B (black) by headspace-SPME-GC/MS at 60°C

Retention time tR [min] Identified compound Chemical structure

3.74 Toluene

5.11 p-Xylene

5.49 o-Xylene

6.09 2-Butoxyethanol
6.72 1-Ethyl-3-methylbenzene

6.95 Phenol

7.38 1,2,3-Trimethylbenzene

8.53 1-Methyl-3-propylbenzene

8.65 2-Ethyl-1,4-dimethylbenzene

8.84 1-Methyl-4-propylbenzene

8.97 Diethylene glycol dimethylether

9.04 1-Ethyl-2,3-dimethylbenzene

9.23 4-Ethyl-1,2-dimethylbenzene

10.43 3-Methylheptyl acetate

12.16 2-Ethylhexyl acrylate (EHA)

15.50 n-Tetradecane

Application of HS SPME-GC/MS in Failure Analysis in

the Automotive Industry

Failure of the structure of materials or components often results in

accidents and plant shutdowns, resulting in hefty compensations. Failure
analysis is the process of collecting and analyzing data to determine the cause
of a failure and to take action to prevent it from reoccurring [36]. It is an
important discipline in many branches of manufacturing industry, such as the
automotive industry and chemical or rubber industry. For the failure analysis
in motor vehicles, there is often a lack of information about the component
itself, such as chemical composition, temperature resistance, possible
contaminants, or mechanical properties. The damage range is usually limited
and not always homogeneous. There are often only small amounts of samples
available to clarify the damage, which may be important for recognizing the
cause of damage [36].
Commonly used rubbers in the automotive industry are natural rubber
(NR, polyisoprene), synthetic polyisoprene (IR), polybutadiene (BR), styrene-
butadiene copolymers (SBR) and nitrile rubber (NBR). Nitrile rubber
[poly(acrylonitrile-co-butadiene)] is a copolymer containing 15 – 50%
acrylonitrile, manufactured by emulsion polymerisation of acrylonitrile and
1,3-butadiene. It was invented at roughly the same time as SBR (near the end
of the 1920s), as a substitute for natural rubber [37]. The major applications
for this material are in areas requiring oil and solvent resistance. The largest
market for nitrile rubber is in the automotive industry because of its solvent
and oil resistance. Major end uses are for membranes, hoses, fuel lines, O-
rings, gaskets and seals [37].
The goal of the study was to find the difference between the chemical
composition of two different functioning rubber membranes from hydraulic
cylinders from the automotive industry. Both investigated membranes
were assigned by pyrolysis-GC/MS to nitrile rubber [poly(acrylonitrile-co-
butadiene)] (NBR) based on the identified pyrolysis products [38]. Figures 8
and 9 show the obtained SPME-GC/MS total ion chromatograms (TIC)
of the headspace (HS) of the extracted rubber membranes from the
hydraulic cylinders 1 and 2 at 60°C, respectively. The identification
results are summarized in Tables 7 and 8. As can be seen from Figure 8
and Table 7, triallyl isocyanurate (TAIC) was the main component of
the headspace above the rubber membrane 1. TAIC is a crosslinking agent
for improvement crosslinking efficiency by manufacturing of polymers
and rubbers. The rubber obtained by using of TAIC has better mechanical

characteristics and larger heat-, hydrolytic- and weather resistance.

Other compounds released from the rubber membrane 1 were 2-ethyl-1-
hexanol (rest solvent or thermal degradation/hydrolysis product of bis(2-
ethylhexyl) adipate plasticizer), α,α-dimethylbenzenemethanol, 1,2-dihydro-
2,2,4-trimethylquinoline, phenanthrene and bis(2-ethylhexyl) adipate. 1,2-
Dihydro-2,2,4-trimethylquinoline is used as an antioxidant in styrene-
butadiene and nitrile-butadiene rubbers and latexes but the content of this
substance in the headspace of the rubber membrane 1 was small (see Figure 8,
peak 3). Bis(2-ethylhexyl) adipate (DEHA) is used as a plasticizer and as a
functional hydraulic fluid. The main component in the headspace above
the rubber membrane 2, however, was the antioxidant 3-tert-butyl-4-
hydroxyanisole (BHA) (Figure 9, Table 8). Other rubber additives identified in
the headspace of the rubber membrane 2 were benzothiazole, 1,2-dihydro-
2,2,4-trimethylquinoline, antioxidant BHT and diethyl phthalate plasticizer
(Figure 9, Table 8). The identified benzothiazole has been formed by the
thermal degradation of 2-mercaptobenzothiazole. 2-Mercaptobenzothiazole is
used as an accelerator for the vulcanisation of rubber and as an antioxidant.

Table 7. Volatile and semivolatile organic compounds released from

rubber membrane from the hydraulic cylinder 1 from the automotive
industry by headspace-SPME-GC/MS at 60°C

Peak Retention time tR Identified compound Chemical structure

No. [min]
1 7.99 2-Ethyl-1-hexanol

2 9.24 α,α-
Dimethylbenzenemethanol
3 16.34 1,2-Dihydro-2,2,4-
trimethylquinoline
(Vulkanox hs)
4 20.01 Triallyl isocyanurate (TAIC)

5 22.20 Phenanthrene

6 29.93 Bis(2-ethylhexyl) adipate

(Plasticizer DOA)

Table 8. Volatile and semivolatile organic compounds released from

rubber membrane from the hydraulic cylinder 2 from the automotive
industry by headspace-SPME-GC/MS at 60°C

Peak No. Retention time tR [min] Identified compound Chemical structure

1 3.36 Methylisobutylketone

2 4.04 1-Hexanal
3 4.72 tert-Butylisothiocyanate

4 4.97 Ethylbenzene

5 5.48 Styrene

6 6.77 Benzaldehyde

7 7.99 2-Ethyl-1-hexanol

8 9.24 α,α-Dimethylbenzenemethanol

9 9.62 1-Nonanal
10 11.72 1-Decanal
11 12.30 Benzothiazole

12 13.74 2-(Methylmercapto)-benzimidazol

13 16.34 1,2-Dihydro-2,2,4-trimethylquinoline
(Vulkanox hs)

14 16.69 3-tert-Butyl-4-hydroxyanisole (BHA)

15 17.41 Di-(tert-butyl)-4-methylphenol (BHT)

16 18.83 Diethyl phthalate

17 19.74 Not identified

18 22.26 9-Methylene-9H-fluorene

19 23.55 N-Morpholinomethyl-isopropyl-sulfide

Figure 9. Total ion current GC/MS chromatogram (TIC) obtained from the headspace
of the extracted rubber membrane from the hydraulic cylinder 2 from the automotive
industry.

The observed differences in the functioning of the two rubber membranes

1 and 2 from hydraulic cylinders could be due different content of
the identified rubber additives, like crosslinking agent, antioxidants and
plasticizers.

Application of HS SPME-GC/MS for Identification of Vinyl

Flooring Emission

The high sensitivity of SPME-GC-MS as a polymer analysis tool can be

also demonstrated by identification of VOCs released from vinyl flooring
(PVC). Vinyl flooring (VF) is manufactured in a variety of styles and
compositions and is widely installed in residential and commercial buildings in
either sheet or tile form [39]. VF is primarily composed of a mixture of
poly(vinyl chloride) (PVC), inert filler (usually calcium carbonate, CaCO3),
and organic plasticizers such as dioctyl phthalate (DOP). Other additives such
as stabilizers, lubricants, antioxidants, and colorants are used to aid in
processing and improve product functionality and appearance [39]. VF may
also be manufactured as a multi-layer system with a bottom backing (usually
glass fiber) and a top coating of transparent PVC or polyurethane. In the
United States during 1998, 214 million kilograms of PVC were used in the
production of VF [39]. VF has been shown to emit a number of volatile

organic compounds (VOCs). VOCs can migrate from the interior to exposed
surfaces by diffusion and then partition into the surrounding air. Most of the
VOCs that are emitted by VF are probably present as contaminants in the
various raw materials or as residues from the manufacturing process.

Figure 10. Total ion current GC/MS chromatograms (TIC) of substances emitted from
A) PVC floor covering (vinyl flooring) and B) from the screed under the vinyl flooring
from a day nursery.

Table 9. Volatile and semivolatile organic compounds released from PVC

floor covering and from screed under the PVC floor covering from
a day nursery by headspace-SPME-GC/MS at 60°C

Peak tR Identified compound Chemical structure

No. [min] PVC floor Screed under
covering the PVC floor
covering
1 2.81 1-Butanol

2 5.28 3-Heptanon

3 5.54 n-Nonane
4 5.60 2-
Butoxyethanol
5 6.54 2-Ethylhexanal

6 7.43 n-Decane
7 7.99 2-Ethyl-1- 2-Ethyl-1-
hexanol hexanol

8 8.10 Limonene

9 9.50 n-Undecane n-Undecane

10 10.43 2-Ethylhexyl 2-Ethylhexyl
acetate acetate

11 11.58 n-Dodecane n-Dodecane

12 13.58 n-Tridecane n-Tridecane
13 15.50 n-Tetradecane n-Tetradecane
14 17.31 n-Pentadecane n-Pentadecane
15 19.03 n-Hexadecane n-Hexadecane
16 20.66 n-Heptadecane n-Heptadecane

Peak tR Identified compound Chemical structure

No. [min] PVC floor Screed under
covering the PVC floor
covering
17 23.09 Diisobutyl
phthalate

18 24.45 Dibutyl
phthalate

19 31.55 Bis(2-
ethylhexyl)
phthalate

The aim of the investigation was the identification of VOCs and SVOCs
emitted from PVC floor covering (vinyl flooring) and from the screed under
the VF covering from a day nursery by HS SPME-GC/MS at 60°C. The results
of the identification are shown in Figure 10 and Table 9. As can be seen from
Figure 10 and Table 9, 2-ethyl-1-hexanol was the main component emitted
from PVC floor covering and from the screed under the VF covering. 2-Ethyl-
1-hexanol is the rest solvent and/or thermal degradation product of the
identified bis(2-ethylhexyl) phthalate plasticizer (Figure 10A, peak 19). Other
identified rest solvents were 1-butanol, 3-heptanon, 2-butoxyethanol and 2-
ethylhexyl acetate (Figure 10, Table 9). Other emitted substances from VF
were diisobutyl- and dibutyl phthalate plasticizers. The presence of limonene
and n-alkanes C9H20 to C17H36 in the investigated headspace were associated
with the cleaning and floor care products.

CONCLUSION
The headspace-SPME-GC/MS analytical method has been proven to be a
valuable tool for the identification of volatile and semivolatile organic

compounds emitted from polymeric materials from many branches of

manufacturing, building and automotive industries as well as in failure analysis in
the automotive industry. The headspace-SPME technique can be introduced
easily and quickly in every GC and GC/MS chemical laboratory.

ACKNOWLEDGMENTS
The author (P. K.) is grateful to his son Dipl.-Päd. Matthäus Kusch for his
critical reading of the manuscript.

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Assoc. 2001, 51(8), 1195-1201.

Chapter 4

SAMPLING OF THE POSTMORTEM SPECIMEN

FOR THE ANALYSIS OF VOLATILE OR
GASEOUS SUBSTANCES IN FORENSIC
PRACTICE

Hiroshi Kinoshita1,, Naoko Tanaka1, Ayaka Takakura1,

Mostofa Jamal1, Asuka Ito1, Mitsuru Kumihashi1,
Shoji Kimura1, Kunihiko Tsutsui2, Shuji Matsubara3
and Kiyoshi Ameno1
1
Department of Forensic Medicine;
2
Health Sciences, Faculty of Medicine, Kagawa University, 1750-1, Miki,
Kita, Kagawa 761-0793, Japan
3
Community Health Care Education Support Center, and Postgraduate
Clinical Education Center, Kagawa University Hospital, 1750-1, Miki,
Kita, Kagawa 761-0793, Japan


All correspondence concerning to this paper should be addressed to: Dr. H. Kinoshita,
Department of Forensic Medicine, Faculty of Medicine, Kagawa University, 1750-1,
Ikenobe, Miki, Kita, Kagawa, 761-0793, Japan. E-mail: [email protected].

ABSTRACT
Postmortem samples for toxicological examination are routinely
collected at forensic autopsy. Usually we collected various biological
specimens such as blood, urine, stomach contents, cerebrospinal fluid or
tissues (brain, liver, lung, kidney, muscle). The analysis of volatile and
gaseous chemical compounds in those biological samples is commonly
performed by the gas chromatography (GC) and gas chromatography-
mass spectrometry (GC/MS) in combination with head-space (HS)
method. The HS method has some advantages such as simple procedure,
less time consuming and without contamination of non-volatile
component in the sample matrix. The HS-GC or HS-GC/MS is useful not
only for the quantification of volatile and gaseous chemicals, but also for
the screening of industrial products containing volatiles used as solvents.
In the present paper, we discuss about the routine and additional
sampling procedure for analysis of volatile and gaseous substances used
in daily life in forensic medicine.

Keywords: sampling, toxicological analysis, volatile substances, gaseous

substances

INTRODUCTION
Volatile or gaseous substances such as carbon monoxide (CO), hydrogen
sulfide, (aliphatic, aromatic and halogenated-) hydrocarbons, alcohols, esters,
ethers and ketones are popular in our daily life. The annual number of victims
by CO poisoning are about 2000-4000 in Japan, and most of them are
accidental or suicidal [1-4]. Inhalation of CO is the leading cause of poisoning
death in Japan [1-4], and also common cause of poisoning in United States [5,
6]. Ethanol is widely used in our daily life, as alcoholic beverages, and it is
commonly encountered in the toxicological examination [7]. Although,
accidental inhalation of volatile substances in occupational exposure are
reported in some conditions [8], a lot of epidemiological study shows the
volatile substance abuse in youth [9, 10].
Poisoning death cases by homicide, suicide or accidents including
fatalities related to substance misuse are received the medico-legal
investigation by forensic pathologist and toxicologist. The detailed forensic
analysis and evaluation in each case is indispensable for planning to the
preventive measures [11]. In this paper, we have focused the volatile or

gaseous compounds used in daily life, and describe the sample collection at
the postmortem examination. As those substances are easily diffuse to
surrounding atmosphere and tissues [12], we have to consider proper sample
collection and handling for suitable interpretation of results and diagnosis.

CLASSIFICATION OF VOLATILE
OR GASEOUS SUBSTANCES

The volatile or gaseous substances are classified according to their

chemical structure, as follows; gases, (aliphatic, aromatic and halogenated)
hydrocarbons, alcohols, esters, ethers, ketones and nitrites [12, 13].
Representative and typical substances in each category are shown in Table1.

AUTOPSY FINDINGS OF POISONING DUE TO INHALATION

OF VOLATILE OR GASEOUS SUBSTANCES

There may be unique findings at autopsy in some cases of poisoning such

as carbon monoxide (cherry red appearance of post-mortem lividity) and
hydrogen sulfide (dark green coloration of post-mortem lividity). The unique
odor was reported in some kinds of volatile gas poisoning case (bitter almond
odor: cyanide, fruity odor: ethanol or most of solvents, sweet odor: chloroform
or other halogenated hydrocarbons, rotten eggs: hydrogen sulfide) [14].
However, the most of volatile or gaseous substances cause no tissue damages,
even in immediately after inhalation, no evidence can be obtained by
macroscopic or microscopic examination was observed in some cases [14, 15].
Various information such as the circumstances of incidents, estimated time of
exposure, should be also considered for the collection of the post-mortem
sample or subsequent laboratory tests [13].

SAMPLING FOR TOXICOLOGICAL EXAMINATION

IN FORENSIC PRACTICE

Toxicological examination is performed routinely in daily forensic

practice [13-16]. Forensic pathologist requests the toxicological analysis for
identification and quantification of chemicals in collected specimens in case of

poisoning or poisoning suspected cases [15]. It is an important to collect the

proper specimen for toxicological examination and subsequent interpretation
of those results. Most of laboratory provides a guideline for routine
collection/storage of samples. A generally required postmortem specimen for
routine examination is shown in Table 2 [13, 14, 16].
In case of death due to poisoning and poisoning suspected cases by the
volatile or gaseous substances, we have to take some points into consideration
and additional procedure for sample collection would be required. Since the
effects of postmortem diffusion and postmortem redistribution have been
reported [8, 14, 16-19], the preferable postmortem blood sample should be
collected from peripheral vein. Whole blood should be used for the evaluation
of volatile substances [13]. Brain, lung and subcutaneous tissue are
recommended as a tissue specimen, when the poisoning by organic solvents or
other volatile substance is suspected [13, 20].
It is necessary for considering not only proper sample collection, but also
the storage and handling of the collected samples [20, 21]. As most of gaseous
or volatile substances are well and rapidly diffusion, loss of the substances by
evaporation is the large problem for quatntitative analysis [12]. The blood
should be collected directly into the vial in which the analysis will be carried
out in case of very volatile substances such as propane or butane [20, 21].
Some other precautions are required in cases especially in volatile
substances. The sample should be collected and stored in gas-tight glass
container with minimal headspace [12, 20]. A cap lined with Teflon® or
aluminium foil should be used. Rubber stoppers or plastic tube should be
avoided, especially in case of organic solvents poisoning. And the sample
storage and handling is recommended at around 4℃ (between 2 and 8℃) [12,
20, 21].

Gases Hydrocarbons alcohol esters ethers ketones nitrites

aliphatic aromatic halogenated
carbon monoxide propane toluene tetrachloroethylene methanol ethyacetate dimethyl ether acetone amyl nitrite
carbon dioxide butane ethyl benzene methylene chloride ethanol butylacetate diethyl ether butanone isoamyl nitrite
nitrogen oxide heptane xylene halothane propanol butyl nitrite
phosgene hexane benzene isoflurane butanol isobutyl nitrite
chlorine sevoflurane
cyanides chloroform
hydrogen sulfide
inert gases

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Table 2. Recommended specimens for routine toxicological examination

specimen volume and comments

blood (cardiac and peripheral) 10 ml each (whole blood for volatile substances)
urine 20-50ml
stomach contents 20-50ml
vitreous humour if available
bile if available
cerebrospinal fluid if available
tisssues
(brain, liver, lung, kidney, muscle) 5 g each

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Sampling of the Postmortem Specimen … 111

DETECTION OF VOLATILE OR GASEOUS SUBSTANCES

The analysis of volatile and gaseous chemical compounds is commonly
performed by the gas chromatography (GC) and gas chromatography-mass
spectrometry (GC/MS) in combination with static head-space (HS), head-
space solid phase microextraction (HS-SPME), cryogenic oven trapping,
pulse-heating and other procedures [12, 22-27]. In this short paper, we will not
discuss about the analytical method, but focused on the special procedure for
sample preparation. The details of analytical procedure should refer to the
other paper or book [12, 22].

SPECIAL PROCEDURE FOR SPECIFIC SUBSTANCES

We described here a special consideration for sample collection and
interpretation of results in addition to the routine procedure (Table 3).

Table 3. Additional specimens for toxicological examination of volatile or

gaseous substances

specimen volume and comments

squeezed splenic if available For CO-Hb measurement.
blood
intratracheal if available Using a syringe with needle. Sample is put into already
gas/contents sealed glass vial
stomach gas tisssues if available Using a syringe with needle. Sample is put into already
sealed glass vial
(subcutaneous fat 5g solvent, hydrocarbon
tissue)

1. Ethanol

Ethanol is a most frequently encountered in forensic practice, since

alcoholic beverages are popular in our life [7]. Its interpreting of postmortem
data are sometimes difficult, because we have to consider various factors, such
as condition of the body and environment, time between death and autopsy
and nature of the specimen for its analysis [7]. Postmortem ethanol production
by the microbial action is one of the large problem for the evaluation of the
influence of alcohol drinking. Vitreous humour has been used as the specimen

for various substance measurement including ethanol [7, 16]. The postmortem
formation of ethanol does not occur in it to any significant extent, as the
interior of the eye is partitioned and a sterile, even in the case of advanced
putrefaction [7, 16].

2. Carbon Monoxide (CO)

CO is an odorless and colorless gas, which is produced by incomplete

combustion of organic compounds [28, 29]. It binds to hemoglobin in
erythrocyte, and forms carboxyhemoglobin (CO-Hb). Its values are important
for the diagnosis of CO-poisoning or fire related death [28]. Post-mortem
blood sample was usually used for CO-Hb measurement. However, it may be
sometimes difficult to obtain in case of advanced putrefaction.
In the case of severe putrefied and no collected blood, we sometimes
collect pleural effusion for toxicological analysis. However, as the postmortem
production of CO has been reported in some conditions, we should not use
body cavity fluid for the measurement of CO [30-34]. In recent study, it has
been reported that squeezed splenic blood is applied for alternative specimen
for CO-Hb measurement in combination with oximeter system [35]. This
oximeter system require 50µl of blood as sample, and this method may be
valid option in case of difficult blood sampling due to severely blood loss.

3. Helium

Helium, a colorless, odorless and nonflammable inert gas, used as a career

gas for party balloons or cryogenic liquids [36-38]. It acts as a simple asphyxic
agent, and causes oxygen depletion [36, 37]. It has been reported that lung
tissue is suitable matrix for analysis of the inert gases including helium [39-
44]. The detection of helium from blood sample may be difficult, since it has a
low solubility in water, and highly diffusive properties. In addition,
intratracheal and stomach gas are useful for identification of helium [39, 40,
43, 45]. The stomach gas reflects the ante-mortem gas exposure since it
undergoes no postmortem exchange with surrounding air [39, 40, 45]. As the
sampling of intratracheal/stomach gas is easy at the time of autopsy, they
provide useful information for forensic diagnosis [44, 45].

4. Hydrocarbons (Kerosene and Butane)

Kerosene is a mixture of hydrocarbons [29], and it sometimes used as an

accelerants in fire-related case. Detection of volatile hydrocarbons in post
mortem blood of the fire related cases are useful for forensic diagnosis [46-
49]. Intratracheal gas or contents are also useful as a forensic examination [50-
54]. It indicates that the body had been exposed to kerosene just before death.
The sampling of intratracheal gas or contents are relatively easy at autopsy,
and its examination by HS-GC or HS-GC/MS may be useful as a primary
screening for accelerant use [53]. Kerosene is sometimes detected from
stomach contents [51, 54-56]. Detection of small amounts of kerosene from
stomach contents in fire related case may be a finding of vital reaction [54].
Butane is a colorless aliphatic hydrocarbon, which is used as a fuel source
or a propellant [29]. It is sometimes abused and observed its related death in
youth, and forensic toxicological evaluation is required [57-59]. As butane has
highly diffusive and lipophilic properties, its blood concentration would be
decreased gradually during postmortem interval [12]. The brain concentration
of butane is relatively stable [59], same as toluene [60]. And the concentration
in lung tissue is sometimes higher than that in blood, in case of inhalation of
high concentration of butane gas [59]. These indicate that tissue sample
collection such as lung and brain are useful for forensic diagnosis in case of
inhalation of hydrocarbons.

5. Solvents in Pesticide (Methanol and Xylene)

Methanol or xylene is used as a solvent in the commercial products of

pesticides [29, 61-67]. They are volatile and easily detectable by routine
toxicological examination using conventional GC or GC/MS analysis.
Identification of these solvents in the stomach contents or in blood may be a
good indicator of pesticide ingestion [65-67]. Examination of the stomach
contents or blood by HS-GC or HS-GC/MS is useful for the primary screening
[65-67]. We should pay more attention to solvents used in commercial
products.

CONCLUSION
Post-mortem samples for toxicological examination, collected at forensic
autopsy, are useful for the diagnosis of poisoning. Proper sampling, storage
and sample handling are important in an accurate diagnosis, especially in
poisoning cases due to volatile or gaseous substances.

ACKNOWLEDGMENT
This work was supported by JSPS KAKENHI Grant-in-Aid for Scientific
Research (C) Number 15K08873.

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[32] Kojima T, Yashiki M, Une I. (1983) Experimental study on postmortem
formation of carbon monoxide. Forensic Sci. Int., 22, 131-135.
[33] Kojima T, Yashiki M, Okamoto I, Noda J, Une I, Miyazaki T, Chikasue
F. (1984) Postmortem formation of carbon monoxide in blood and body

cavity fluids of rats drowned and kept immersed in fresh water.

Hiroshima J. Med. Sci., 33, 591-594.
[34] Kojima T, Okamoto I, Yashiki M, Miyazaki T, Chikasue F, Degawa K,
Oshida S, Sagisaka K. (1986) Production of carbon monoxide in
cadavers. Forensic Sci. Int., 32, 67-77.
[35] Tanaka N, Kinoshita H, Jamal M, Takakura A, Kumihashi M, Miyatake
N, Ameno K. (2015) Squeezed splenic blood sampling as an alternative
method for carboxyhemoglobin measurement. Rom. J. Leg. Med., 23,
106-108.
[36] Ogden RD, Wooten RH. (2002) Asphyxial suicide with helium and a
plastic bag. Am. J. Forensic Med. Pathol., 23, 234-237.
[37] Gallagher KE, Smith DM, Mellen PF. (2003) Suicidal asphyxiation by
using pure helium gas. Case report, review, and discussion of the
influence of the internet. Am. J. Forensic Med. Pathol., 24, 361-363.
[38] Berganza CJ, Zhang JH. (2013) The role of helium gas in medicine.
Medical Gas Research, 3, 18.
[39] Yoshitome K, Ishikawa T, Inagaki S, Yamamoto Y, Miyaishi S, Ishizu
H. (2002) A case of suffocation by an advertising balloon filled with
pure helium gas. Acta Med. Okayama, 56, 53-55.
[40] Auwärter V, Pragst F, Strauch H. (2004) Analytical investigations in a
death case by suffocation in an argon atmosphere. Forensic Sci. Int.,
143, 169-175.
[41] Auwaerter V, Grosse Perdekamp M, Kempf J, Schmidt U, Weinmann
W, Pollak S. (2007) Toxicological analysis after asphyxia suicide with
helium and a plastic bag. Forensic Sci. Int., 170, 139-141.
[42] Musshoff F, Hagemeier L, Kirschbaum K, Madea B. (2012) Two cases
of suicide by asphyxiation due to helium and argon. Forensic Sci. Int.,
223, e27-e30.
[43] Tanaka N, Kinoshita H, Jamal M, Kumihashi M, Tobiume T, Tsutsui K,
Ameno K. (2013) Usefulness of intratracheal gas analysis in an autopsy
case of helium inhalation. Rom. J. Leg. Med., 21, 237-238.
[44] Wigergowski M, Kaliszan M, Sumińska-Ziemann B, Gos T, Jankowski
Z. (2014) Helium detection in the lungs in case of suicide by helium
inhalation – case report and literature review. Rom. J. Leg. Med., 22,
153-156.
[45] Tanaka N, Takakura A, Jamal M, Kumihashi M, Ito A, Ishimoto S,
Tsutsui K, Kimura S, Ameno K, Kinoshita H. (2016) Stomach gas as a
useful matrix for detecting ante-mortem gas exposure. A case ofasphyxia
by helium inhalation. Rom. J. Leg. Med., 24, 21-22.

[46] Matsubara K, Akane A, Takahashi S, Shiono H, Fukui Y. (1988) Gas

chromatographic determination for forenisic purposes of petroleum fuel
inhaled just before fatal burning. J. Chromatogr., 424, 49-59.
[47] Morinaga M, Kashimura S, Hara K, Hieda Y, Kageura M. (1996) The
utility of volatile hydrocarbon analysis in cases of carbon monoxide
poisoning. Int. J. Legal Med., 109, 75-79.
[48] Morinaga M. (2003) Application for forensic science of combustion gas
analysis using GC/MS. J. Mass. Spectrom. Soc. Jpn., 51, 201-204.
[49] Yonemitsu K, Sasao A, Oshima T, Mimasaka S, Ohtsu Y, Nishitani Y.
(2012) Quantitative evaluation of volatile hydrocarbons in post-mortem
blood in forensic autopsy cases of fire-related deaths. Forensic Sci. Int.,
217, 71-75.
[50] Takatori T. (1980) Gas chromatographic determination of kerosene
components from cadaveric hypopharyngeal contents. Hokkaido Igaku
Zasshi, 55, 471-473.
[51] Yoshida M, Watabiki T, Tokiyasu T, Akane A, Ishida N. (1994) Case of
death by fire with kerosene –Analysis of contents of trachea and
stomach-. Nihon Hoigaku Zasshi, 48, 96-104.
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analysis for volatile substances by gas chromatography/ mass
spectrometry - application to forensic autopsies. J. Forensic Sci., 46, 98-
104.
[53] Adachi N, Kinoshita H, Nishiguchi M, Takahashi M, Ouchi H, Minami
T, Matsui K, Yamamura T, Motomura H, Ohtsu N, Yoshida S, Ameno
K, Hishida S. (2009) Analysis of tracheal contents using headspace gas
chromatography-mass spectrometry to screen for accelerant use. Soud
Lek., 54, 2-3.
[54] Tanaka N, Takakura A, Jamal M, Kumihashi M, Ito A, Tsutsui K,
Kimura S, Ameno K, Kinoshita H. (2016) Detection of kerosene in
stomach contents – useful indicator of vital reaction. Rom. J. Leg. Med.,
24, 128-130.
[55] Yoshida M, Akane A, Okii Y, Yoshimura S, Kobayashi T, Tokiyasu T,
Watabiki T. (1997) A case report of detection of ethylene, propylene and
kerosene from the burned body. Res. Pract. Forens. Med., 40, 177-182.
[56] Yoshida M, Akane A, Tokiyasu T, Yoshimura S, Okii Y, Mitani T,
Watabiki T. (2002) The origin of the volatile components detected from
a corpse burnt after the ingestion of fenitrothion. Res. Pract. Forens.
Med., 45, 45-50.
[57] Tanaka N, Kinoshita H, Haba R, Jamal M, Ohkubo E, Ameno K. (2010)

An autopsy case of butane gas abuse. Soud Lek., 55, 44-45.

[58] Tanaka N, Kinoshita H, Takatsu M, Kuse A, Jamal M, Ohkubo E,
Nagasaki Y, Yoshioka N, Asano M, Ueno Y, Ameno K. (2010) A fatal
case of butane gas inhalation. Current study of environmental and
medical sciences, 3, 15-16.
[59] Tanaka N, Kinoshita H, Jamal M, Kumihashi M, Tsutsui K, Ameno K.
(2012) An autopsy case of fuel gas abuse. Rom J Leg Med, 20, 195-196.
[60] Kiriu T, Ameno K, Fuke C, Ameno S, Shinohara T, Sogo K, Ijiri I.
(1993) Experimental studies of postmortem diffusion of toluene in
blood, brain, muscle and fat of rats exposed to toluene vapor. Nihon
Hoigaku Zasshi, 47, 29-32.
[61] Yamaguchi Y, Shirakawa Y, Ogura S, Ameno K, Fuke C, Ogli K.
(1989) A case of amitraz poisoning. Jpn. J. Clin. Toxicol., 2, 289-292.
[62] Yamazaki M, Terada M, Kuroki H, Honda K, Matoba R, Mitsukuni Y.
(2001) Pesticide poisoning initially suspected as a natural death. J.
Forensic Sci., 46, 165-170.
[63] kinoshita H, Ameno K, Ameno S, Kubota T, Zhang X, Ijiri I, Taniguchi
T, Nishiguchi M, Ouchi H, Minami T, Hishida S. (2001) A case of
burning with fenitrothion ingestion. Res. Pract. Forens. Med., 44, 155-
159.
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Marukawa S, Ameno K, Hishida S. (2005) Methanol: toxicity of the
solvent in a commercial product should also be considered. Hum.
Toxicol., 24, 1-2.
[65] Kinoshita H, Tanaka N, Jamal M, Kumihashi M, Tsutsui K, Ameno K.
(2013) Xylene; a useful marker for agricultural products ingestion. Soud.
Lek., 58, 59-60.
[66] Tanaka N, Kinoshita H, Takakura A, Jamal M, Kumihashi M, Uchiyama
Y, Tsutsui K, Ameno K. (2015) Combination of energy-dispersive X-ray
fluorescence spectrometry (EDX) and head-space gas chromatography
mass spectrometry (HS-GC/MS) is a useful screening tool for stomach
contents. Rom. J. Leg. Med., 23, 43-44.
[67] Kinoshita H, Tanaka N, Takakura A, Kumihashi M, Jamal M, Ito A,
Tsutsui K, Kimura S, Nagano T, Matsubara S, Ameno K. (2015)
Analysis of stomach contents by head-space gas chromatography/mass
spectrometry to screen for ingestion of insecticide. Revista e Mjekësisë
Ligjore Shqiptare, 11, 85-89.

"As for me, I will dwell at Mizpah": the Tell en-Naṣbeh excavations after
85 years
LCCN 2014039951
Type of material Book
Main title "As for me, I will dwell at Mizpah": the Tell en-
Naṣbeh excavations after 85 years / edited by Jeffrey
R. Zorn, Aaron J. Brody.
Published/Produced Piscataway, NJ: Gorgias Press, 2014.
Description xviii, 308 pages: illustrations; 24 cm
ISBN 9781463204167
LC classification DS110.T5 A8 2014
Related names Zorn, Jeffrey R., 1958-
Brody, Aaron Jed.
Badè, W. G. (William G.), 1924-2012.
Scope and content "Tell en-Naṣbeh (biblical Mizpah of Benjamin) was
excavated on a grand scale by William F. Badè of
Pacific School of Religion between 1926 and 1935.
His team uncovered approximately two-thirds of this
eight-acre site, providing an unmatched view of a
typical rural Israelite town in the hill country in the
Iron Age. The studies included in this volume provide
insights into the life ways of the inhabitants of this
important border town. Until relatively recently
excavations in the ancient Near East have focused on
macro level questions involving political history and
chronology. Often these efforts in Israel focused on

elucidating biblical history itself and tying that world

into the larger ancient world. Very often the daily lives
of average Israelites were ignored, and materials
associated with them left largely unstudied and
relegated to lists at the ends of site reports. Since 1990,
efforts have been underway to restudy Tell en-Naṣbeh
to better understand aspects of daily life centered at
this town. The present volume includes studies
originally presented in a special session devoted to Tell
en-Naṣbeh at the annual meeting of the American
Schools of Oriental Research in 2011. The studies
incorporate aspects of trade and economy, death and
burial, metals, cooking, and water management. Also
included are a study of the curation of the Tell en-
Naṣbeh materials and records in Berkeley, California;
an interview with William Badè Jr., who was at the
excavations in 1935; and an up-to-date bibliography of
publications related to the site"--Provided by publisher.
Contents Tell en-Naṣbeh in the 20th and 21st centuries /
JEFFREY R. ZORN -- Memories from Tell en-Naṣbeh
/ AARON J. BRODY -- Life and death at Tell en-
Naṣbeh: a bioarchaeological analysis / ALEXIS T.
BOUTIN, WHITNEY R. MCCLELLAN and DANIEL
A. CUSIMANO -- Transjordanian commerce with
Northern Judah in the Iron II-Persian period: ceramic
indicators, interregional interaction, and modes of
exchange at Tell en-Naṣbeh / AARON J. BRODY --
Iron in the Iron Age: the life-cycle of agricultural
implements from Tell en-Naṣbeh / STEPHANIE H.
BROWN -- Curating Badè's legacy: management of
the Tell en-Nasbeh collection / CATHERINE P.
FOSTER -- "Let me eat some of that red stuff, for I am
famished!" (Gen 25:30): preliminary insights into Iron
Age cooking practices at Tell en-Naṣbeh resulting
from gas chromatography/mass spectrometry analyses
/ MARY LARKUM -- Observations regarding an oil
lamp of the late Roman-Byzantine period from Tell en-
Naṣbeh / VARDA SUSSMAN -- On the use and reuse
of rock-cut tombs and a ritual bath at Tell en-Naṣbeh:

new perspectives on the Roman and Byzantine

Necropoleis / BOAZ ZISSU AND EITAN KLEIN --
Tell en-Naṣbeh's contributions to understanding Iron
Age Israelite water systems / JEFFREY R. ZORN.
Subjects Bible. Old Testament--Antiquities.
Excavations (Archaeology)--West Bank.
Iron age--West Bank.
Iron age--Israel.
Material culture--West Bank--History.
Material culture--Israel--History.
Jews--Antiquities.
Social archaeology--West Bank.
Social archaeology--Israel.
Tell en-Naṣbeh (Extinct city)
Notes Includes bibliographical references and index.

Advanced gas chromatography

LCCN 2016934744
Type of material Book
Main title Advanced gas chromatography / [edited by] Adrianna
Coty.
Edition 1st edition.
Published/Produced Valley Cottage, NY: Scitus Academics, 2016.
ISBN 9781681171975 (hardcover: alk. paper)

Advanced techniques in gas chromatography-mass spectrometry (GC-

MS-MS and GC-TOF-MS) for environmental chemistry
LCCN 2014381896
Type of material Book
Main title Advanced techniques in gas chromatography-mass
spectrometry (GC-MS-MS and GC-TOF-MS) for
environmental chemistry / edited by Imma Ferrer and
E. Michael Thurman, Center for Environmental Mass
Spectrometry, Department of Environmental
Engineering, University of Colorado.
Published/Produced Amsterdam: Elsevier, [2013]
Description xxii, 502 pages: illustrations; 24 cm.
ISBN 9780444626233 (hbk.)
0444626239 (hbk.)

LC classification QD79.C45 A39 2013

Related names Ferrer, Imma, 1970- editor of compilation.
Thurman, E. M. (Earl Michael), 1946- editor of
compilation.
Subjects Gas chromatography.
Mass spectrometry.
Environmental chemistry--Technique.
Notes Includes bibliographical references and index.
Series Comprehensive Analytical Chemistry; Volume 61
Comprehensive analytical chemistry; v. 61.

Applications of gas chromatography

LCCN 2016937430
Type of material Book
Main title Applications of gas chromatography / [edited by]
Adrianna Coty.
Edition 1st edition.
Published/Produced Valley Cottage, NY: Scitus Academics, 2016.
ISBN 9781681172620 (hardcover: alk. paper)

Bioanalysis of pharmaceuticals: sample preparation, separation

techniques, and mass spectrometry
LCCN 2015035265
Type of material Book
Main title Bioanalysis of pharmaceuticals: sample preparation,
separation techniques, and mass spectrometry / editors,
Steen Honore Hansen, Stig Pedersen-Bjergaard.
Published/Produced Chichester, West Sussex: John Wiley & Sons, Inc.,
2015.
ISBN 9781118716816 (cloth: alk. paper)
9781118716823 (pbk.: alk. paper)
LC classification RM301.55 .B56 2015
Related names Hansen, Steen, 1947- editor.
Pedersen-Bjergaard, Stig, editor.
Contents Introduction -- Physicochemical properties of drug
substances -- Biological samples: their composition
and properties and their collection and storage --
General chromatographic theory and principles --
Quantitative and qualitative chromatographic analysis

-- Sample preparation -- Liquid chromatography

(HPLC) and liquid chromatography-mass spectrometry
(LC-MS) -- Gas chromatography (GC) and gas
chromatography-mass spectrometry (GC-MS) --
Analysis of small molecule drugs in biological fluids --
Analysis of biopharmaceuticals in biological fluids --
Regulated bioanalysis and guidelines.
Subjects Drugs--Metabolism--Research--Methodology.
Mass spectrometry.
Pharmacokinetics--Research--Methodology.
Notes Includes bibliographical references and index.
Additional formats Online version: Bioanalysis of pharmaceuticals
Chichester, West Sussex: John Wiley & Sons, Inc.,
2015 9781118716847 (DLC) 2015041722

Brain energy metabolism

LCCN 2014946822
Type of material Book
Main title Brain energy metabolism / edited by Johannes
Hirrlinger, Carl-Ludwig-Institute for Physiology,
University of Leipzig, Leipzig, Germany, Helle S.
Waagepetersen, Faculty of health and Medical
Sciences, University of Copenhagen, Copenhagen,
Denmark.
Published/Produced New York; Heidelberg: Humana Press, [2014]
©2014
Description xiv, 368 pages: illustrations (some color); 26 cm
ISBN 9781493910588 (alk. paper)
1493910582 (alk. paper)
(eBook)
LC classification QP376 .B6995 2014
Related names Hirrlinger, Johannes, editor.
Waagepetersen, Helle S., editor.
Summary Brain Energy Metabolism addresses its challenging
subject by presenting diverse technologies allowing for
the investigation of brain energy metabolism on
different levels of complexity. Model systems are
discussed, starting from the reductionist approach like
primary cell cultures which allow assessing of the

properties and functions of a single brain cell type with

many different types of analysis, however, at the
expense of neglecting the interaction between cell
types in the brain. On the other end, analysis in
animals and humans in vivo is discussed, maintaining
the full complexity of the tissue and the organism but
making high demands on the methods of analysis.
Written for the popular Neuromethods series, chapters
include the kind of detailed description and key
implementation advice that aims to support
reproducible results in the lab. Meticulous and
authoritative, Brain Energy Metabolism provides an
ideal guide for researchers interested in brain energy
metabolism with the hope of stimulating more research
in this exciting and very important field. -- Source
other than Library of Congress.
Contents Determination of CO2 Production in Subcellular
Preparations like Synaptosomes and Isolated
Mitochondria Using 14C-Labeled Substrates and
Radioactive CO2 Measurements -- Transport of
Lactate: Characterization of the Transporters Involved
in Transport at the Plasma Membrane by Heterologous
Protein Expression in Xenopus Oocytes -- Primary
Cultures of Astrocytes and Neurons as Model Systems
to Study the Metabolism and Metabolite Export from
Brain Cells -- Metabolic Mapping of Astrocytes and
Neurons in Culture Using Stable Isotopes and Gas
Chromatography-Mass Spectrometry (GC-MS) --
Metabolic Flux Analysis Tools to Investigate Brain
Metabolism In Vitro -- Fluorescent Nanosensor Based
Flux Analysis: Overview and the Example of Glucose
-- Mitochondrial Bioenergetics Assessed by Functional
Fluorescence Dyes -- RNA Interference as a Tool to
Selectively Down-Modulate Protein Function --
Localizing and Quantifying Metabolites In Situ with
Luminometry: Induced Metabolic Bioluminescence
Imaging (imBI) -- A Chip Off the Old Block: The
Brain Slice as a Model for Metabolic Studies of Brain
Compartmentation and Neuropharmacology --

Integrated Measurements of Electrical Activity,

Oxygen Tension, Blood Flow, and Ca2+-Signaling in
Rodents In Vivo -- Measuring Cerebral
Hemodynamics and Energy Metabolism by Near-
Infrared Spectroscopy -- Compartmental Analysis of
Metabolism by 13C Magnetic Resonance
Spectroscopy -- Positron Emission Tomography of
Brain Glucose Metabolism with
[18F]Fluorodeoxyglucose in Humans.
Subjects Brain--Metabolism.
Energy metabolism.
Brain chemistry--Physiology.
Brain--Metabolism--Laboratory manuals.
Brain chemistry--Physiology--Laboratory manuals.
Energy metabolism--Laboratory manuals.
Brain--metabolism--Laboratory Manuals.
Brain Chemistry--physiology--Laboratory Manuals.
Energy Metabolism--Laboratory Manuals.
Notes Includes bibliographical references and index.
Series Neuromethods, 0893-2336; v. 90
Springer Protocols, 1949-2448
Neuromethods; v. 90. 0893-2336
Springer protocols (Series) 1949-2448

Chemiluminescence and bioluminescence: past, present and future

LCCN 2012397475
Type of material Book
Main title Chemiluminescence and bioluminescence: past,
present and future / edited by Aldo Roda.
Published/Created Cambridg, UK: Royal Society of Chemistry, c2011.
Description xvii, 590 p.: ill.; 24 cm.
Links Contributor biographical information http://www.loc.
gov/catdir/enhancements/fy1304/2012397475-b.html
Publisher description http://www.loc.gov/catdir/
enhancements/fy1304/2012397475-d.html
Table of contents only http://www.loc.gov/catdir/
enhancements/fy1304/2012397475-t.html
ISBN 9781847558121
1847558127

LC classification QP517.C54 C546 2011

Related names Roda, A. (Aldo)
Contents 14.1.Introduction -- 14.2.Chemiluminescence --
14.2.1.Reaction Triggering -- 14.3.Bioluminescence --
14.3.1.Firefly Bioluminescence -- 14.3.2.Bacterial
Bioluminescence -- 14.4.Biosensors Generalities --
14.5.Immunosensor Generalities -- 14.6.Analytical
Applications -- 14.6.1.Chemiluminescent Biosensors --
14.6.2.Electrochemiluminescent Biosensors --
14.6.3.Chemiluminescent Immunosensors --
14.6.4.Electrochemiluminescent Immunosensors --
14.6.5.Electrochemiluminescent DNA Sensors --
14.6.6.Bioluminescent Biosensors -- 14.7.Conclusion -
- References -- ch. 15 Cell-based Bioluminescent
Biosensors / Aldo Roda -- 15.1.Introduction --
15.2.Design and Construction of Bacterial Cell-based
Bioluminescent Biosensors -- 15.2.1.Regulation of
Reporter Gene Expression -- 15.2.2.Reporter Genes
and Their Attributes -- 15.2.3.Advantages and
Limitations of Bacterial Cell-based Bioluminescent
Biosensors -- 15.3.Applications of Bacterial Cell-based
Bioluminescent Biosensing Systems --
15.4.Bioluminescent Biosensors: the Eukaryotic
Alternative -- 15.4.1.Yeast-based Biosensors --
15.4.2.Bioluminescent Cell-based Assays for
Endocrine Disruptors Monitoring --
15.4.3.Bioluminescent Yeast and Mammalian Cell-
based Assays for Genotoxic Compounds and ADMET
Studies -- 15.4.4.Bioluminescent Mammalian Cell-
based Biosensors as Functional Detection Systems --
15.5.Multiplexed and Multicolor Assays --
15.6.Miniaturization of Cell-based Biosensing Systems
-- 15.7.Conclusions and Future Potential --
Acknowledgements -- References -- ch. 16
Miniaturized Analytical Devices Based on
Chemiluminescence, Bioluminescence and
Electrochemiluminescence / Jason Y. Park --
16.1.Introduction -- 16.2.Fabrication Methods for
Microchips -- 16.3.Microchip Components --

16.4.Advantages of Microchips for Analysis --

16.5.Applications of Microchip Analytical Devices --
16.5.1.Chemiluminescence -- 16.5.2.Bioluminescence
-- 16.5.3.Electrochemiluminescence -- 16.6.μTAS
Chips -- 16.7.Microarray Chips -- 16.8.Flow Injection
Analysis (FIA) on Microchips -- 16.9.Capillary
Electrophoretic Analysis (CE) on Microchips --
16.10.Point-of-care Applications for Microchips --
16.11.Conclusions -- References -- ch. 17 Recent
Analytical Application Areas of Chemiluminescence
and Bioluminescence / Aldo Roda -- 17.1.Introduction
-- 17.2.Forensic Sciences -- 17.2.1.Luminol Test for
Bloodstain Detection -- 17.2.2.Factors Affecting the
Luminol Test -- 17.2.3.Improvement of the Luminol
Test -- 17.2.4.Other Applications of the Luminol Test -
- 17.3.Detection of Explosives -- 17.3.1.Analysers
Based on the NO-Ozone CL Reaction --
17.3.2.Analysers Based on the Luminol CL Reaction --
17.3.3.Direct Detection of Degradation Products of
Nitrated Explosives -- 17.3.4.Detection of Explosives
by Gas Chromatography -- 17.3.5.Detection of
Explosives by Liquid Chromatography --
17.3.6.Detection of Explosives by Immunoassays --
17.4.Study and Conservation of Cultural Heritage --
17.4.1.Detection of Microbial Contamination by BL
Imaging -- 17.4.2.Detection and Localization of
Proteins in Artworks by CL Imaging Microscopy --
17.4.3.Dating of Ancient Bones -- References.
Subjects Chemiluminescence.
Bioluminescence.
Notes Includes bibliographical references and index.

Clinical applications of mass spectrometry: methods and protocols

LCCN 2009939452
Type of material Book
Main title Clinical applications of mass spectrometry: methods
and protocols / edited by Uttam Garg, Catherine A.
Hammett-Stabler.
Published/Created New York, NY: Humana Press, c2010.

Description xvi, 538 p.: ill.; 27 cm.

Links http://dx.doi.org/10.1007/978-1-60761-459-3
ISBN 9781607614586 (hbk.: alk. paper)
1607614588 (hbk.: alk. paper)
9781607614593 (e-book)
1607614596 (e-book)
LC classification QD95 .C58 2010
Related names Garg, Uttam.
Hammett-Stabler, Catherine A., 1952-
Contents The evolution of mass spectrometry in the clinical
laboratory / Catherine A. Hammett-Stabler and Uttam
Garg -- Measurement of plasma/serum acylcarnitines
using tandem mass spectrometry / Nathalie Lepage and
Susan Aucoin -- Comprehensive determination of
amino acids for diagnosis of inborn errors of
metabolism / Dennis J. Dietzen and Annette L.
Weindel -- Identification and quantitation of
amphetamine, methamphetamine, MDMA,
pseudoephedrine, and ephedrine in blood, plasma, and
serum using gas chromatography-mass spectrometry
(GC/MS) / Josh Gunn, Scott Kriger, and Andrea R.
Terrell -- Quantification of antidepressants using gas
chromatography-mass spectrometry / Ruth E.
Winecker -- Quantitation of argatroban in plasma
using liquid chromatography electrospray tandem mass
spectrometry (UPLC-ESI-MS/MS) / Ross J. Molinaro
-- Quantitation of amobarbital, butalbital,
pentobarbital, phenobarbital, and secobarbital in urine,
serum, and plasma using gas chromatography-mass
spectrometry (GC-MS) / Leonard L. Johnson and
Uttam Garg -- Quantitation of benzodiazepines in
blood and urine using gas chromatography-mass
spectrometry (GC-MS) / Bruce A. Goldberger, Chris
W. Chronister, and Michele L. Merves -- LC-MS/MS
analysis of 13 benzodiazepines and metabolites in
urine, serum, plasma, and meconium / Stephanie J.
Marin and Gwendolyn A. McMillin -- Simultaneous
determination and quantification of 12
benzodiazepines in serum or whole blood using

UPLC/MS/MS / Josh Gunn, Scott Kriger, and Andrea

R. Terrell -- Determination of benzoic acid in serum or
plasma by gas chromatography-mass spectrometry
(GC/MS) / Jeff M. Knoblauch ... [et al.] --
Quantification of busulfan in plasma using liquid
chromatography electrospray tandem mass
spectrometry (HPLC-ESI-MS/MS) / Marion L. Snyder
and James C. Ritchie -- Quantitation of total 11-nor-9-
carboxy-delta 9-tetrahydrocannabinol in urine and
blood using gas chromatography-mass spectrometry
(GC-MS) / C. Clinton Frazee III, Michael Kiscoan,
and Uttam Garg -- Quantitation of cocaine,
benzoylecgonine, ecgonine methyl ester, and
cocaethylene in urine and blood using gas
chromatography-mass spectrometry (GC-MS) / Steven
W. Fleming, Amitava Dasgupta, and Uttam Garg --
Identification and quantitation of cocaine,
benzoylecgonine, and cocaethylene in blood, serum,
and plasma using ultra-performance liquid
chromatography coupled to tandem mass spectrometry
(UPLC-MS/MS) / Scott Kriger, Josh Gunn, and
Andrea R. Terrell -- Detection and quantification of
cocaine and benzoylecgonine in meconium using solid
phase extraction and UPLC/MS/MS / Josh Gunn, Scott
Kriger, and Andrea R. Terrell -- Diagnosis of creatine
metabolism disorders by determining creatine and
guanidinoacetate in plasma and urine / Qin Sun and
William E. O'Brien -- Broad spectrum drug screening
using electron-ionization gas chromatography-mass
spectrometry (EI-GCMS) / Judy Stone -- Broad
spectrum drug screening using liquid chromatography-
hybrid triple quadrupole linear ion trap mass
spectrometry / Judy Stone -- High sensitivity
measurement of estrone and estradiol in serum and
plasma using LC-MS/MS / Mark M. Kushnir ... [et al.]
-- 3-hydroxy-fatty acid analysis by gas
chromatography-mass spectrometry / Patricia M. Jones
and Michael J. Bennett -- Quantitation of fentanyl in
blood and urine using gas chromatography-mass

spectrometry (GC-MS) / Bruce A. Goldberger, Chris

W. Chronister, and Michele L. Merves --
Determination of total homocysteine in plasma using
liquid chromatography coupled to tandem mass
spectrometry (LC/MS/MS) / Bruno Casetta --
Quantitation of homovanillic acid (HVA) and
vanillylmandelic acid (VMA) in urine using gas
chromatography-mass spectrometry (GC/MS) / Ryan
Allenbrand and Uttam Garg -- Quantitation of 17-OH-
progesterone (OHPG) for diagnosis of congenital
adrenal hyperplasia (CAH) / Ravinder J. Singh --
Determination of hydroxyurea in serum or plasma
using gas chromatography-mass spectrometry (GC-
MS) / David K. Scott, Kathleen Neville, and Uttam
Garg -- Quantitation of ibuprofen in blood using gas
chromatography-mass spectrometry (GC-MS) / Gerry
Huber and Uttam Garg -- Quantitation of indomethacin
in serum and plasma using gas chromatography-mass
spectrometry (GC-MS) / Sarah Thomas, Amanda
Sutton, and Uttam Garg -- Quantitation of iothalamte
in urine and plasma using liquid chromatography
electrospray tandem mass spectrometry (HPLC-ESI-
MS/MS) / Ross J. Molinaro and James C. Ritchie --
Identification and quantitation of ketamine in
biological matrices using gas chromatography-mass
spectrometry (GC-MS) / Timothy P. Rohrig, Megan
Gamble, and Kim Cox -- Measurement of filter paper
bloodspot lead byi nductively coupled plasma-mass
spectrometry (ICP-MS) / Denise M. Timko and
Douglas F. Stickle -- Multiplex lysosomal enzyme
activity assay on dried blood spots using tandem mass
spectrometry / X. Kate Zhang ... [et al.] -- Gas
chromatography-mass spectrometry method for the
determination of methadone and 2-ethylidene-1,5-
dimethyl-3, 3-diphenylpyrrolidine (EDDP) / Christine
L.H. Snozek, Matthew W. Bjergum, and Loralie J.
Langman -- Liquid chromatography-tandem mass
spectrometry (LC-MS-MS) method for monitoring
methotrexate in the setting of carboxypeptidase-G2

therapy / Vikram S. Kumar, Terence Law, and Mark

Kellogg -- Quantitation of methylmalonic acid in
serum or plasma using isotope dilution-selected ion
gas chromatograpy-mass spectrometry / Jie Chen and
Michael J. Bennet -- Quantitation of methylmalonic
asid in plasma using liquid chromatography-tandem
mass spectrometry / Claudine Fasching and Jasbir
Singh -- Monitoring of mycophenolate acid in serum
or plasma using LC tandem mass spectrometry /
Catherine A. Hammett-Stabler ... [et al.] --
Quantitation of nicotine, its metabolites, and other
related alkaloids in urine, serum, and plasma using LC-
MS-MS / Bingfang Yue ... [et al.] -- Quantitation of
opioids in blood and urine using gas chromatography-
mass spectrometry (GC-MS) / Bruce A. Goldberger,
Chris W. Chronister, and Michele L. Merves --
Quantitation of morphine, codeine, hydrocodone,
hydromorphone, oxycodone, oxymorphone, and 6-
monoacetylmorphine (6-MAM) in urine, blood, serum,
or plasma using liquid chromatography with tandem
mass spectrometry detection / Tim Dahn ... [et al.] --
Urine organic acid analysis for inherited metabolic
disease using gas chromatography-mass spectrometry /
Patricia M. Jones and Michael J. Bennett --
Identification of urine organic acids for the detection
of inborn errors of metabolism using urease and gas
chromatography-mass spectrometry (GC-MS) /
Stanley F. Lo, Velta Young, and William J. Rhead --
Quantitation of orotic acid in urine using isotope
dilution-selected ion gas chromatography-mass
spectrometry / Jie Chen and Michael J. Bennett --
Quantitation of oxycodone in blood and urine using
gas chromatography-mass spectrometry (GC-MS) /
Bruce A. Goldberger, Chris W. Chronister, and
Michele L. Merves -- Quantitation of phencyclidine
(PCP) in urine and blood using gas chromatography-
mass spectrometry (GC-MS) / Angela M. Ferguson
and Uttam Garg -- Quantitation of sirolimus using
liquid chromatography-tandem mass spectrometry

(LC-MS-MS) / Magdalena Korecka and Leslie M.

Shaw -- Quantitation of tacrolimus in whole blood
using high performance liquid chromatography-tandem
mass spectrometry (HPLC-MS-MS) / Keri J.
Donaldson and Leslie M. Shaw -- Analysis of
testosterone in serum using mass spectrometry / Robert
L. Fitzgerald, Terrance L. Griffin, and David A.
Herold -- Determination of tetrahydrozoline in urine
and blood using gas chromatography-mass
spectrometry (GC-MS) / Judy Peat and Uttam Garg --
Quantitation of 25-OH-vitamin D (25OHD) using
liquid tandem mass spectrometry (LC-MS-MS) /
Ravinder J. Singh -- Identification and quantitation of
zolpidem in biological matrices using gas
chromatograrphy-mass spectrometry (GC-MS) /
Timothy P. Rohrig, Lydia A. Harryman, and Melissa
C.Norton -- Identification and quantitation of
zopiclone in biological matrices using gas
chromatography-mass spectrometry (GC-MS) /
Timothy P. Rohrig, Melissa C.Norton, and Lydia A.
Harryman.
Subjects Mass spectrometry.
Clinical chemistry.
Mass Spectrometry--methods--Laboratory Manuals.
Chemistry, Clinical--methods--Laboratory Manuals.
Notes Includes bibliographical references and index.
Additional formats Also available in an electronic version.
Series Methods in molecular biology, 1064-3745; 603
Springer protocols
Methods in molecular biology (Clifton, N.J.); v. 603.
1064-3745
Springer protocols.

Comprehensive chromatography in combination with mass spectrometry

LCCN 2010036838
Type of material Book
Main title Comprehensive chromatography in combination with
mass spectrometry / edited by Luigi Mondello.
Published/Created Hoboken, N.J.: Wiley, c2011.

Description xii, 481 p.: ill. (chiefly col.); 25 cm.

ISBN 9780470434079 (cloth)
0470434074 (cloth)
LC classification QD79.C4 C66 2011
Related names Mondello, Luigi.
Contents Multidimensional gas chromatography: theoretical
considerations / Leonid M. Blumberg --
Multidimensional liquid chromatography: theoretical
considerations / Pavel Jandera -- History, evolutaion
and optimization aspects of comprehensive two-
dimensional gas chromatography / Ahmed Mostafa, ...
[et al.] -- Flow-modulated comprehensive two-
dimensional gas chromatorgraphy / John V. Seeley --
Comprehensive two-dimensional gas chromatography
combined with mas spectrometry / Peter Q. Tranchida,
... [et al.] -- Detector technologies and applications in
comprehensive two-dimensional gas chromatography /
Philip J. Marriott -- History, evolution, and
optimization aspects of comprehensive two-
dimensional liquid chromatography / Isabelle Francois,
Koen Sandra, and Pat Sandra -- Comprehensive two-
dimensional liquid chromatography combined with
mass spectrometry / Paolo Dugo, ... [et al] --
Comprehensive two-dimensional liquid
chromatography applications / Paola Dugo, ... [et al.] --
Other comprensive chromatography methods / Isabelle
Francois, ... [et al.] -- Comprehensive chromatography
data interpretation technologies / Elisabeth M.
Humston and Robert E. Synovec.
Subjects Chromatographic analysis.
Multidimensional chromatography.
Notes Includes bibliographical references and index.
Series Wiley-Interscience series on mass spectrometry
Wiley-Interscience series on mass spectrometry.

Differentiation of enantiomers I
LCCN 2013956811
Type of material Book
Main title Differentiation of enantiomers I / Volker Schurig,

editor; with contributions by A. Ciogli [and 12 others].

Published/Produced Heidelberg; New York: Springer, [2013]
©2013
Description ix, 280 pages: illustrations (some color); 24 cm.
ISBN 9783319032382 (cloth: alk. paper)
3319032380 (cloth: alk. paper)
LC classification QD79.C4 D54 2013
Related names Schurig, Volker, 1940-, editor of compilation.
Ciogli, A. (Alessia), contributor.
Contents Molecular chirality: language, history, and significance
/ Joseph Gal -- Terms for the quantification of a
mixture of stereoisomers / Volker Schurig --
Enantiomeric differentiation by synthetic helical
polymers / Eiji Yashima, Hiroki Iida, and Yoshio
Okamoto -- Chiral supramolecular selectors for
enantiomer differentiation in liquid chromatography /
Alessia Ciogli, Dorina Kotoni, Francesco Gasparrini,
Marco Pierini, and Claudio Villani -- Chiroptical
detectors for the study of unusual phenomena in chiral
chromatography / Nicolas Vanthuyne and Christian
Roussel -- Salient features of enantioselective gas
chromatography: the enantiomeric differentiation of
chiral inhalation anesthetics as a representative
methodological case in point / Volker Schurig --
Differentiation of enantiomers by capillary
electrophoresis / Gerhard K.E. Scriba.
Subjects Chromatographic analysis.
Enantiomers--Analysis.
Enantiomers--Differentiation.
Stereoisomerism.
Notes Includes bibliographical references and index.
Series Topics in current chemistry, 0340-1022; 340
Topics in current chemistry; 340. 0340-1022

Earth, life, and isotopes

LCCN 2012538661
Type of material Book
Main title Earth, life, and isotopes / edited by N. Ohkouchi, I.
Tayasu, and K. Koba.

Published/Created Kyoto: Kyoto University Press, 2010.

Description xii, 415 p.: ill. (some col.); 22 cm.
ISBN 9784876989607 (pbk.)
4876989605 (pbk.)
Related names Ohkouchi, Naohiko.
Tayasu, Ichirou.
Koba, Keisuke.
Summary Section 3. Method development: 21. Ultra-sensitive
elemental analyzer/isotope ratio mass spectrometer for
stable nitrogen and carbon isotope analyses / Ogawa,
N.O. ... [et al.] -- 22. An improved method for precise
determination of carbon isotopic composition of amino
acids / Chikaraishi, Y. and Ohkouchi, N. -- 23.
Instrumental optimization of compound-specific
nitrogen isotope analysis of amino acids by gas
chromatography/combustion/isotope ratio mass
spectrometry / Chikaraishi, Y. ... [et al.] -- 24.
Enantiomer-specific isotope analysis of D-and L-
alanine / Takano, Y., Chikaraishi, Y. and Ohkouchi, N.
-- Appendix. Summary of methods for measuring
isotopic compositions presented in this book /
Ohkouchi, N., Tayasu, I., and Koba, K.
Subjects Wada, Eitaro, 1939-
Stable isotopes in ecological research.
Global environmental change--Measurement.
Notes Includes bibliographical references and index.

Evaluating naturally durable wood species for repair and rehabilitation of

above-ground components of covered bridges
LCCN 2013379089
Type of material Book
Personal name Kirker, Grant Terral, 1977- author.
Main title Evaluating naturally durable wood species for repair
and rehabilitation of above-ground components of
covered bridges / Grant T. Kirker, Carol A. Clausen,
A.B. Blodgett, Stan T. Lebow.
Published/Produced Madison, Wisconsin: United States Department of
Agriculture, Forest Service, Forest Products
Laboratory, July 2013.

Description 40 pages: illustrations (some color), color maps; 28

cm.
Rights advisory British Library not licensed to copy 0.
LC classification TA420 .K47 2013
Related names Clausen, Carol A., author.
Blodgett, A. B., author.
Lebow, Stan T., author.
Forest Products Laboratory (U.S.), publisher.
United States. Federal Highway Administration.
National Historic Covered Bridge Preservation
Program.
Abstract More than 1,500 covered bridges remain in the United
States. They are a unique part of our history; thus,
replacement of bridge components is an equally
important part of preserving this uncommon style of
craftsmanship. The goal of this project was to evaluate
seven wood species for their durability in above-
ground field exposure. Chemical analysis was also
conducted using gas chromatography-mass
spectrometry (GC-MS) for fatty acids and terpenoids
in an attempt to correlate extractive content with
durability. Extracts removed from the durable wood
species were also tested in laboratory bioassays to
determine their biological activity against wood decay
fungi and termites. This report serves as a guide for the
use of these naturally durable wood species for
rehabilitation of above-ground components of covered
bridges and incorporates the results of filed and
laboratory tests into the final recommendations.
Subjects Wood--Testing.
Gas chromatography.
Mass spectrometry.
Covered bridges--United States--Maintenance and
repair.
Notes Title from cover.
In cooperation with the United States Department of
Transportation Federal Highway Administration as
part of the Research, Technology and Education
portion of the National Historic Covered Bridge

Preservation Program.
Includes bibliographical references.
Series General technical report; FPL-GTR-224
General technical report FPL; 224.

False carbamazepine positives due to 10,11-dihydro-10-

hydroxycarbamazepine breakdown in the GC/MS injector port
LCCN 2010443989
Type of material Book
Personal name Johnson, Robert D. (Robert David), 1974-
Main title False carbamazepine positives due to 10,11-dihydro-
10-hydroxycarbamazepine breakdown in the GC/MS
injector port / Robert D. Johnson, Russell J. Lewis, and
Mike K. Angier.
Published/Created Washington, D.C.: Federal Aviation Administration,
Office of Aerospace Medicine, 2010.
Description iii, 5 p.: ill.; 28 cm.
Links http://www.faa.gov/library/reports/medical/oamtechrep
orts/2010s/media/201004.pdf Online PDF version
FAA - OAM Technical Reports. http://www.faa.gov/
library/reports/medical/oamtechreports/index.cfm
http://worldcat.org/oclc/607280243/viewonline View
Online
LC classification RC1075 .J64 2010
Related names Lewis, Russell J.
Angier, Mike K.
Civil Aerospace Medical Institute.
United States. Office of Aerospace Medicine.
United States. Federal Aviation Administration.
United States. Department of Transportation.
Abstract "During the investigation of aviation accidents,
postmortem specimens from accident victims are
submitted to the Federal Aviation Administration's
Civil Aerospace Medical Institute (CAMI) for
toxicological analysis. A case recently received by
CAMI screened positive for the anticonvulsant
medication carbamazepine (Tegretol) by gas
chromatography/mass spectrometry (GC/MS). The
carbamazepine found during the routine screening

procedure was subsequently confirmed using a

carbamazepine-specific GC/MS procedure.
Concurrently, it was discovered that the accident
victim had been prescribed oxcarbazepine (Trileptal).
Oxcarbazepine is nearly structurally identical to
carbamazepine and is metabolized by cytosolic
enzymes in the liver to the active compound 10,11-
dihydro-10-hydroxycarbamazepine. The
carbamazepine initially found in this case was present
due to the breakdown of the active oxcarbazepine
metabolite in the GC/MS injector port. In the current
study this conversion is investigated, the percentage of
carbamazepine formed at various injector port
temperatures is determined, and these three
compounds are quantified in nine fluid and tissue
specimens from the case in question. Lastly, liquid
chromatography/mass spectrometry (LC/MS) was used
to demonstrate the absence of carbamazepine, and its
formation, in the same specimens."--Report
documentation page.
Subjects Aviation toxicology--Research.
Forensic toxicology.
Aircraft accidents--Investigation.
Aircraft accidents--Human factors.
Carbamazepine--Research.
Aviation medicine--United States.
Notes "This work was accomplished under the approved task
AM-B-05-TOX-204."--P. i.
"February 2010."
"DOT/FAA/AM-10/4."
Includes bibliographical references.
Final report.
Sponsored by the Office of Aerospace Medicine,
Federal Aviation Administration; performed by the
FAA Civil Aerospace Medical Institute.
Additional formats Also available online in PDF from the Aerospace
Medicine Technical Reports Web site.

Flavor, fragrance, and odor analysis

LCCN 2011031500
Type of material Book
Main title Flavor, fragrance, and odor analysis / edited by Ray
Marsili.
Edition 2nd ed.
Published/Created Boca Raton, FL: CRC Press, c2012.
Description xi, 268 p.: ill.; 24 cm.
ISBN 9781439846735 (hardback)
1439846731 (hardback)
LC classification TX546 .F52 2012
Related names Marsili, Ray, 1946-
Summary "Emphasizing SBSE techniques alongside advances in
mass spectrometry, sample preparation, gas
chromatography (GC)-olfactometry, and electronic-
nose technology, this new edition discusses the
significant advantage of these methods for flavor and
odor studies in the food, cosmetic, and pharmaceutical
industries. Written from a practical, problem-solving
perspective, it discusses the chemical structures of key
flavor and fragrance compounds, contains numerous
examples and chromatograms, and emphasizes novel
solid-phase micro extraction procedures. It also
presents important updates on GC-olfactometry as a
tool for studying flavor synergy effects"-- Provided by
publisher.
"Sample preparation techniques for isolating and
concentrating flavor and odor-active chemicals from
foods prior to GC-MS analysis continue to evolve,
providing lower detection limits while being more
amenable to instrumental automation. Solventless
extraction techniques like solid-phase microextraction
(SPME) and stir bar sorptive extraction (SBSE) have
wide application appeal and are now significant
problem-solving tools for flavor and odor chemists.
While the first edition of Flavor, Fragrance and Odor
Analysis emphasized SPME, a newer technique at the
time, this edition focuses on the advantages of SBSE,
including sequential SBSE and other sample

manipulation techniques that increase the sensitivity

and application potential of this surprisingly simple but
amazingly powerful technique"-- Provided by
publisher.
Subjects Food--Sensory evaluation.
Notes Includes bibliographical references and index.

Forensic applications of gas chromatography

LCCN 2013000523
Type of material Book
Personal name Carlin, Michelle Groves.
Main title Forensic applications of gas chromatography /
Michelle Groves Carlin, John R. Dean.
Published/Produced Boca Raton: CRC Press, [2013].
©2013
Description xx, 166 pages: illustrations; 23 cm.
ISBN 9781466507548 (alk. paper)
LC classification HV8073.5 .C27 2013
Related names Dean, John R.
Subjects Gas chromatography--Forensic applications.
Chemistry, Forensic.
Notes Includes bibliographical references and index.
Series Analytical concepts in forensic chemistry; 2

G protein-coupled receptor signaling in plants: methods and protocols

LCCN 2013942971
Type of material Book
Main title G protein-coupled receptor signaling in plants:
methods and protocols / edited by Mark P. Running,
Department of Biology, University of Louisville,
Louisville, KY, USA.
Published/Produced New York: Humana Press, [2013]
©2013
Description x, 162 pages: illustrations (some color); 26 cm.
Links Table of contents http://catdir.loc.gov/catdir/
enhancements/fy1314/2013942971-t.html
ISBN 9781627035316 (alk. paper)
1627035311 (alk. paper)
LC classification QK725 .G15 2012

Related names Running, Mark P., editor of compilation.

Contents Topology Assessment, G Protein-Coupled Receptor
(GPCR) Prediction, and In Vivo Interaction Assays to
Identify Plant Candidate GPCRs -- Measurement of
GTP-Binding and GTPase Activity of Heterotrimeric
G[alpha] Proteins -- Biochemical Analysis of the
Interaction Between Phospholipase D[alpha]1 and
GTP-Binding Protein [alpha]-Subunit from
Arabidopsis thaliana -- Analysis of Cell Division and
Cell Elongation in the Hypocotyls of Arabidopsis
Heterotrimeric G Protein Mutants -- Aequorin
Luminescence-Based Functional Calcium Assay for
Heterotrimeric G Proteins in Arabidopsis -- Methods
for Analysis of Disease Resistance and the Defense
Response in Arabidopsis -- Fusarium oxysporum
Infection Assays in Arabidopsis -- Analysis of
Unfolded Protein Response in Arabidopsis --
Functional Analysis of Heterotrimeric G Proteins in
Chloroplast Development in Arabidopsis -- G Protein
Signaling in UV Protection: Methods for
Understanding the Signals in Young Etiolated
Seedlings -- Functional Analysis of Small Rab
GTPases in Cytokinesis in Arabidopsis thaliana -- In
Vivo Localization in Arabidopsis Protoplasts and Root
Tissue -- Analysis of Protein Prenylation and S-
Acylation Using Gas Chromatography-Coupled Mass
Spectrometry -- In Vitro Myristoylation Assay of
Arabidopsis Proteins -- Assaying Protein S-Acylation
in Plants -- In Vitro Prenylation Assay of Arabidopsis
Proteins.
Subjects Plant cellular signal transduction--Laboratory manuals.
G proteins--Laboratory manuals.
Plant Cells--physiology.
Receptors, G-Protein-Coupled--physiology.
Signal Transduction.
Form/Genre Laboratory Manuals.
Notes Includes bibliographical references and index.
Series Methods in molecular biology, 1064-3745; 1043
Springer protocols

Methods in molecular biology (Clifton, N.J.); v. 1043.

1064-3745
Springer protocols (Series). 1949-2448

Gas chromatography in plant science, wine technology, toxicology and

some specific applications
LCCN 2016946445
Type of material Book
Main title Gas chromatography in plant science, wine
technology, toxicology and some specific applications
/ [edited by] Federico Noguerra.
Edition 1st edition.
Published/Produced Valley Cottage, NY: Scitus Academics, 2016.

Gas chromatography
LCCN 2012012782
Type of material Book
Personal name Poole, C. F.
Main title Gas chromatography / Colin F. Poole.
Edition 1st ed.
Published/Created Amsterdam; Boston: Elsevier, 2012.
Description viii, 743 p.: ill.; 25 cm.
ISBN 9780123855404
LC classification QD79.C45 P64 2012
Subjects Gas chromatography.
Chromatographic analysis.
Notes Includes bibliographical references and index.

Gas chromatography and mass spectrometry: a practical guide

LCCN 2010027725
Type of material Book
Personal name Sparkman, O. David (Orrin David), 1942-
Main title Gas chromatography and mass spectrometry: a
practical guide / O David Sparkman, Zelda Penton,
Fulton G. Kitson.
Edition 2nd ed.
Published/Created Boston: Elsevier, 2011.
Description xix, 611 p.: ill.; 23 cm.
ISBN 9780123736284

LC classification QD79.C45 S66 2011

Related names Penton, Zelda.
Kitson, Fulton G.
Contents The fundamentals of GC/MS -- Introduction and
history -- Gas chromatography -- The gc/ms interface -
- Mass spectrometry instrumentation -- Mass spectral
data interpretation -- Quantitation with GC/MS -- GC
conditions, derivatization, and mass spectral
interpretation -- Of specific compound types -- Acids -
- Alcohols -- Aldehydes -- Amides -- Amines -- Amino
acid -- Common contaminants -- Drugs and their
metabolites -- Esters -- Ethers -- Fluorinated
compounds -- Gases -- Glycols -- Halogenated
compounds (other than fluorinated) -- Hydrocarbons --
Isocyanates -- Ketones -- Nitriles -- Nitroaromatics --
Nitrogen-containing heterocyclics -- Nucleosides
(TMS derivatives) -- Pesticides -- Phenols --
Phosphorus compounds -- Plasticizers and other
polymer additives (including phthalates) --
Prostaglandins (MO-TMS derivatives) -- Solvents and
their impurities -- Steroids -- Sugars
(monosaccharides) -- Sulfur compounds -- Appendices
-- A definitions of terms related to gas chromatography
-- B definitions of terms related to mass spectrometry -
- C atomic masses and isotope abundances -- X+1 and
x+2 values for ions containing atoms of C and H based
on -- Isotope contributions -- E isotope peak patterns
for ions containing atoms of Cl and/or Br -- F steps to
follow in the determination of an elemental
composition -- Based on isotope peak intensity ratios -
- G derivatization in GC/MS -- H points of comparison
of LC/MS vs GC/MS -- I list of available EI mass
spectral databases -- J information required for
reporting a GC/MS analysis -- K third-party software
for use with GC/MS -- GC installation and
maintenance -- Troubleshooting common GC
problems -- N maintenance, operating tips, and
troubleshooting for mass spectrometers -- O mixtures
for determining mass spectral resolution -- P cross-

index chart for GC stationary phases -- Q ions for

determining unknown structures.
Subjects Gas chromatography.
Mass spectrometry.
Notes Includes bibliographical references and index.

Handbook of analysis of oligonucleotides and related products

LCCN 2010033563
Type of material Book
Main title Handbook of analysis of oligonucleotides and related
products / edited by Jose V. Bonilla, Susan Srivatsa.
Published/Created Boca Raton, FL: CRC Press, 2011.
Description xiv, 497 p.; 27 cm.
ISBN 9781439819937 (hardcover: alk. paper)
LC classification QP625.O47 H36 2011
Related names Bonilla, Jose V.
Srivatsa, Susan.
Contents Purity analysis and impurities determination by
reversed-phase HPLC / Hagen Cramer, Eric Herzberg
& Kevin Finn -- Purity analysis and impurities
determination by AEX-HPLC / J.R. Thayer,
Veeravagu Murugaiah, Yansheng Wu -- Purity
analysis and molecular weight determination by size
exclusion HPLC analysis / Ming Fai Chan & Ipsita
Roymoulik -- Analysis of oligonucleotides by liquid
chromatography & mass spectrometry / Soheil
Pourshahian & Sean McCarthy -- Sequence
determination and confirmation by MS/MS and
MALDI-TOF / Zoltan Timar -- Determination of melt
temperature (TM) of oligonucleotides / Huihe Zhu &
G. Susan Srivatsa -- Purity and content analysis of
oligonucleotides by capillary gel electrophoresis / Judy
Carmody and Bernhard Noll -- Bioanalysis of
therapeutic oligonucleotides using hybridization-based
immunoassay techniques / Sandra Carriero & Helen
Legakis -- Oligonucleotide assay and potency / Dennis
Michaud -- Microbial analysis: endotoxin testing /
Barbara J. Markley -- Analysis of residual solvents by
headspace gas chromatography / Sky Countryman &

Jose V. Bonilla -- Determination of extinction

coefficient / Veeravagu Murugaiah -- Structural
determination by NMR / Michele L. Derider, Doug
Brooks & Gary Burt -- Infrared analysis of
oligonucleotides / Jose V. Bonilla -- Stability
indicating methods for oligonucleotide products /
Veeravagu Murugaiah -- Analysis by hydrophilic
interaction chromatography (HILIC) / Patrick Limbach
and Renee N. Easter -- Determination of base
composition / Hüseyin Aygün -- Analysis of metals in
oligonucleotides / Mike Murphy -- Regulatory
considerations for the development of oligonucleotide
therapeutics / G. Susan Srivatsa.
Subjects Oligonucleotides--Analysis.
Oligonucleotides--analysis.
Notes Includes bibliographical references and index.

Handbook of sample preparation

LCCN 2010010828
Type of material Book
Main title Handbook of sample preparation / edited by Janusz
Pawliszyn, Heather L. Lord.
Published/Created Hoboken, N.J.: Wiley, c2010.
Description x, 491 p.: ill.; 29 cm.
ISBN 9780470099346 (cloth)
0470099348 (cloth)
LC classification QD75.4.S24 H36 2010
Related names Pawliszyn, Janusz.
Lord, Heather L. (Heather Lynn)
Contents Theory of extraction / Janusz Pawliszyn -- Headspace
gas chromatography / Zelda E. Penton -- Liquid-liquid
extraction in environmental analysis / Toh Ming Hii
and Hian Kee Lee -- Solid-phase extraction / Ronald E.
Majors -- Solid-phase microextraction / Sanja
Risticevic, Dajana Vuckovic, and Janusz Pawliszyn --
Microdialysis sampling as a sample preparation
method / Pradyot Nandi and Susan M. Lunte -- Liquid-
phase microextraction (LPME) utilizing porous hollow
fibers / Stig Pedersen-Bjergaard, Knut Einar

Rasmussen, and Jan Åke Jönsson -- Sample

preparation in membrane introduction mass
spectrometry / Raimo A. Ketola, Tapio Kotiaho, and
Frants R. Lauritsen -- Pressurized fluid extraction /
John R. Dean and Renli Ma -- Superheated water
extraction / Roger M. Smith -- Supercritical fluid
extraction / Jeremy J. Kroon and Douglas E. Raynie --
Microwave-assisted extraction / J.R. Jocelyn Paré and
Jacqueline M.R. Bélanger -- Chemical derivatizations
in analytical extractions / Jack Rosenfeld -- Sample
preparation techniques for environmental organic
pollutant analysis / Ray E. Clement and Chunyan Hao
-- Sample preparation for the study of flavor
compounds in food / Henryk H. Jeleń -- Sampling and
sample preparation for clinical and pharmaceutical
analysis / Hiroyuki Kataoka, Keita Saito, and Atsushi
Yokoyama -- Statistics of sampling and sample
preparation / Byron Kratochvil -- SPME devices
integrating sampling with sample preparation for on-
site analysis / Gangfeng Ouyang -- Developments in
the use of passive sampling devices for monitoring
pollutants in water / Graham A. Mills ... [et al.] --
Solid-phase microextraction for drug analysis /
Heather L. Lord -- Sample handling protocols for
biosensor applications / Andrew Chan, Teresa Artuso,
and Ulrich J. Krull -- Sol-gel coatings and monoliths in
analytical sample preparation / Scott Segro and Abdul
Malik -- The use of molecularly imprinted polymers
for sampling and sample preparation / Börje Sellergren
and Antonio Martin Esteban.
Subjects Sample preparation (Chemistry)
Extraction (Chemistry)
Chemistry, Analytic.
Notes Includes bibliographical references and index.

Hans Hofmann: the artist's materials

LCCN 2016009233
Type of material Book
Personal name Rogala, Dawn V., author.

Main title Hans Hofmann: the artist's materials / Dawn V.

Rogala.
Published/Produced Los Angeles: Getty Conservation Institute, [2016]
©2016
ISBN 9781606064870 (pbk.)
LC classification ND237.H667 R64 2016
Related names Hofmann, Hans, 1880-1966, artist.
Getty Conservation Institute, issuing body.
Contents A life in art -- The young artist in Germany -- The
Paris years -- Return to Munich and a new role
teaching avant-garde art -- Journey to America --
Hofmann and the culture of modern painting --
Hofmann's role in abstract expressionism and his
influence on generations of artists -- The role of
materials in abstract expressionism -- Hofmann's late-
career paintings -- Origins and development of
Hofmann's late-career style -- Existing information
regarding Hofmann's materials -- Selection and
conservation history of the paintings in this study --
Selection of the study group paintings -- Physical
history of the study group paintings -- Identification of
Hofmann's late-career materials -- Analytical methods
and sample selection -- Optical microscopy --
Pyrolysis-gas chromatography-mass spectrometry --
Scanning electron microscopy-energy dispersive
spectroscopy -- Fourier transform infrared
spectroscopy -- X-ray diffraction -- Discussion of
analyses -- Hofmann's late-career materials --
Hofmann's palette and modern art history -- Hofmann's
manipulation of materials -- The correlation between
condition issues and Hofmann's use of new materials --
Conclusion: the lessons of Hofmann's late-career
materials.
Subjects Hofmann, Hans, 1880-1966.
Hofmann, Hans, 1880-1966--Criticism and
interpretation.
Painting, Modern--20th century--Technique.
Artists' materials--Analysis.
Paint materials--Analysis.

Notes Includes bibliographical references and index.

Historical overview of chromatography and related techniques in analysis

of antimalarial drug primaquine
LCCN 2010036139
Type of material Book
Personal name Brondz, Ilia.
Main title Historical overview of chromatography and related
techniques in analysis of antimalarial drug primaquine
/ Ilia Brondz.
Published/Created New York: Nova Science Publishers, c2011.
Description xii, 222 p.: ill.; 27 cm.
ISBN 9781617619441 (hardcover: alk. paper)
1617619442 (hardcover: alk. paper)
LC classification RM666.P828 B76 2011
Contents History of malaria -- Discovery and introduction of
natural and synthetic antimalarial drugs and agents
relevant to the suppression of the malaria mosquito --
Pharmacopeias: their history and place in drug quality
control -- Analytical quantitative measurements --
Discovery and development of chromatography --
Planar chromatography or open-bed chromatography
as a tool for the qualitative and quantitative analysis of
primaquine -- High-performance liquid
chromatography (HPLC) -- Supercritical fluid
chromatography (SFC) -- Gas chromatography (GC)
and gas chromatography-mass spectroscopy --
Spectroscopy and spectrometry -- In search of
antimalarial drugs in the 8-methoxyaminoquinoline --
Who's who in the world struggle to curb malaria -- The
Via Dolorosa (the Way of Grief or Suffering).
Subjects Primaquine--Analysis.
Primaquine--analysis.
Primaquine--history.
Antimalarials--analysis.
Antimalarials--history.
Chromatography--history.
Chromatography--methods.
Notes Includes bibliographical references and index.

Series Tropical diseases-- etiology, pathogenesis and

treatments
Pharmacology-- research, safety testing and regulation
Tropical diseases-- etiology, pathogenesis, and
treatments series.
Pharmacology-research, safety testing, and regulation
series.

Instrumental assessment of food sensory quality: a practical guide

LCCN 2013943671
Type of material Book
Main title Instrumental assessment of food sensory quality: a
practical guide / edited by David Kilcast.
Published/Created Oxford, UK; Philadelphia: Woodhead Pub., 2013.
Description xxx, 627 p., [4] p. of plates: ill. (some col.); 24 cm.
ISBN 9780857094391 (acid-free paper)
0857094394 (acid-free paper)
LC classification TX546 .I57 2013
Related names Kilcast, David.
Contents Measurement of the sensory quality of food: an
introduction / D. Kilcast -- Food appearance quality
assessment and specification / J.B. Hutchings, M.
Ronnier Luo and W. Ji -- Principles of food flavor
analysis / G. Reineccius and D. Peterson -- Principles
of solid food texture analysis / R. Lu -- Principles of
food viscosity analysis / B.M. McKenna and J.G. Lyng
-- Food colour measurement using computer vision /
D. Wu and D.-W. Sun -- Gas chromatography-
olfactometry (GC-O), electronic noses (e-noses) and
electronic tongues (e-tongues) for in vivo food flavour
measurement / W. Wardencki, T. Chmiel and T.
Dymerski -- Non-destructive methods for food texture
assessment / R. Lu and H. Cen -- In-mouth
measurement of food quality / I.A.M. Appelqvist --
Emerging flavour analysis methods for food
authentication / S.P. Heenan and S.M. van Ruth --
Advances in analysis of instrumental food sensory
quality data / M. Bevilacqua ... [et al.] -- Instrumental
assessment of the sensory quality of meat, poultry and

fish / M.G. O'Sullivan and J.P. Kerry -- Instrumental

assessment of the sensory quality of baked goods /
S.M. Fiszman, T. Sanz and A. Salvador --
Measurement of the texture of dry crisp products /
L.M. Duizer -- Instrumental assessment of the sensory
quality of dairy products / J.L. Le Quéré and N. Cayot
-- Instrumental assessment of the sensory quality of
fruits and vegetables / Z. Schmilovitch and A. Mizrach
-- Instrumental assessment of the sensory quality of
wine / A.J. Buglass and D.J. Caven-Quantrill --
Instrumental assessment of the sensory quality of beer
/ K.J. Siebert -- Instrumental assessment of the sensory
quality of juices / F.J. Heredia ... [et al.].
Subjects Food--Quality--Testing.
Flavor--Testing.
Notes Includes bibliographical references and index.
Series Woodhead Publishing series in food science,
technology and nutrition, 2042-8049; no. 253
Woodhead Publishing in food science, technology, and
nutrition; no. 253.

Introduction to GC-MS spectrometry

LCCN 2012037919
Type of material Book
Personal name Bouchonnet, Stéphane.
Main title Introduction to GC-MS spectrometry / Stéphane
Bouchonnet.
Published/Created Boca Raton, FL: Taylor & Francis, c2013.
Description xxi, 206 p.: ill.; 24 cm.
ISBN 9781466572515 (pbk.)
LC classification QD79.C45 B68 2013
Variant title Introduction to gas chromatography-mass spectrometry
Summary "Without neglecting the fundamental theory, this book
emphasizes the practical aspects of gas
chromatography-mass spectrometry (GC-MS). It
discusses important topics such as choosing the most
successful device for a given application and the
problems usually encountered by novice users and
ways to solve them. Additional topics include

acquisition modes in GC-MS, quadrupolar analyzer

performance, quantitation by GC-MS, spectra
databases for GC-MS, dissociation mechanisms, and
mass spectra interpretation. The book supports
theoretical demonstrations with numerous examples
and figures to assist with reader assimilation"--
Provided by publisher.
Subjects Gas chromatography.
Mass spectrometry.
Science / Chemistry / Analytic
Science / Research & Methodology
Science / Spectroscopy & Spectrum Analysis
Notes Includes bibliographical references and index.

Leucocytes: methods and protocols

LCCN 2011945167
Type of material Book
Main title Leucocytes: methods and protocols / edited by Robert
B. Ashman.
Published/Created New York: Humana Press, c2012.
Description xi, 296 p.: ill. (some col.); 27 cm.
ISBN 9781617795268 (hbk.: alk. paper)
1617795267 (hbk.: alk. paper)
LC classification QR185.8.L48 L485 2012
Related names Ashman, Robert B.
Contents ENU-based phenotype-driven screening / Vera M.
Ripoll, Philip L. Kong, and Paul K. Potter -- Detection
and quantification of cytokines and other biomarkers /
Evan L. Chiswick ... [et al.] -- Flow cytometry analysis
of cell cycling and proliferation in mouse
hematopoietic stem and progenitor cells / Valérie
Barbier ... [et al.] -- Flow cytometry measurement of
bone marrow perfusion in the mouse and sorting of
progenitors and stems cells according to position
relative to blood flow in vivo / Valérie Barbier ... [et
al.] -- Analyzing cell death events in cultured
leukocytes / Karin Christenson, Fredrik B. Thorén, and
Johan Bylund -- Towards a four-dimensional view of
neutrophils / Ben A. Croker, Andrew W. Roberts, and

Nicos A. Nicola -- Isolation of human and mouse

neutrophils ex vivo and in vitro / Yan Hu --
Measurement of oxidative burst in neutrophils / Yu
Chen and Wolfgang G. Junger -- Measurement of
neutrophil elastase, proteinase 3, and cathepsin G
activities using intramolecularly quenched fluorogenic
substrates / Brice Korkmaz ... [et al.] -- The
macrophage / Chris P. Verschoor, Alicja Puchta, and
Dawn M.E. Bowdish -- Generation and
characterization of MacGreen mice, the CFS1R-EGFP
transgenic mice / R. Tedjo Sasmono and Elizabeth
Williams -- Generation of mouse bone marrow-derived
macrophages / Silvia Manzanero -- Isolation and
differentiation of monocytes-macrophages from human
blood / Dipti Vijayan -- In vitro measurement of
phagocytosis and killing of Cryptococcus neoformans
by macrophages / André Moraes Nicola and Arturo
Casadevall -- Measuring the inflammasome / Olaf
Gross -- Arginine and macrophage activation / Mònica
Comalada -- Immunodetection of granzyme B tissue
distribution and cellular localisation / Catherina H.
Bird ... [et al.] -- Detection of human and mouse
granzyme B activity in cell extracts / Sarah Elizabeth
Stewart ... [et al.] -- T cell transfer model of colitis: a
great tool to assess the contribution of T cells in
chronic intestinal inflammation / Rajaraman Eri,
Michael A. McGuckin, and Robert Wadley --
Measurement of nitrite in urine by gas
chromatography-mass spectrometry / Dimitrios Tsikas
... [et al.].
Subjects Leucocytes.
Leukocytes--Laboratory Manuals.
Immunity, Cellular.
Immunity, Innate.
Leukocytes--immunology.
Notes Includes bibliographical references and index.
Additional formats Also available in electronic format via the World Wide
Web.
Series Methods in molecular biology, 1064-3745; 844

Springer protocols
Methods in molecular biology (Clifton, N.J.); v. 844.
1064-3745
Springer protocols.

Mass spectral and GC data of drugs, poisons, pesticides, pollutants, and

their metabolites
LCCN 2012360939
Type of material Book
Personal name Maurer, Hans, 1950-
Main title Mass spectral and GC data of drugs, poisons,
pesticides, pollutants, and their metabolites / Hans H.
Maurer, Karl Pfleger, Armin A. Weber.
Edition 4th, rev. and enlarged ed.
Published/Created Weinheim: Wiley-VCH, 2011-
Description <1-2>: ill.; 29-30 cm. + 1 CD-ROM (4 3/4 in.)
Links Contributor biographical information http://www.loc.
gov/catdir/enhancements/fy1210/2012360939-b.html
Publisher description http://www.loc.gov/catdir/
enhancements/fy1210/2012360939-d.html
Table of contents only http://www.loc.gov/catdir/
enhancements/fy1210/2012360939-t.html
ISBN 9783527329922
LC classification RS189 .P425 2011
Related names Pfleger, Karl, 1924-
Weber, Armin, 1954-
Pfleger, Karl, 1924- Mass spectral and GC data of
drugs, poisons, pesticides, pollutants, and their
metabolites.
Incomplete contents v. 1. Methods and tables -- v. 2. Mass spectra
Subjects Drugs--Analysis--Tables.
Poisons--Analysis--Tables.
Mass spectrometry--Tables.
Gas chromatography--Tables.
Notes Rev. ed. of: Mass spectral and GC data of drugs,
poisons, pesticides, pollutants, and their metabolites /
Karl Pfleger, Hans H. Maurer, Armin Weber. 1992.
Includes bibliographical references.

Mass spectrometry in food safety: methods and protocols

LCCN 2011929940
Type of material Book
Main title Mass spectrometry in food safety: methods and
protocols / edited by Jerry Zweigenbaum.
Published/Created New York: Humana; Springer, c2011.
Description xii, 416 p.: ill.; 26 cm.
Links Publisher description http://www.loc.gov/catdir/
enhancements/fy1206/2011929940-d.html
Table of contents only http://www.loc.gov/catdir/
enhancements/fy1206/2011929940-t.html
ISBN 1617791350
9781617791352
LC classification TX547 .M37 2011
Related names Zweigenbaum, Jerry Arthur, 1951-
Contents European union regulations / Peter Furst -- China's
food safety regulation and mass spectrometry /
Xiaogang Chu ... [et al.] -- United States and Japanese
food regulations / Jerry Zweigenbaum -- QuEChERS
sample preparation approach for mass spectrometric
analysis of pesticide residues in foods / Steven J.
Lehotay -- Automated solid phase extraction / Norbert
Helle, Meike Baden, and Kaj Petersen -- Multiresidue
pesticide analysis by capillary gas chromatography-
mass spectrometry / Jon W. Wong ... [et al.] --
Targeted pesticide residue analysis using triple quad
LC-MS/MS / Lutz Alder -- LC/TOF-MS analysis of
pesticides in fruits and vegetables: the emerging role of
accurate mass in the unambiguous identification of
pesticides in food / Imma Ferrer, E. Michael Thurman,
and Jerry Zweigenbaum -- Hormone analysis in food
products / Marco H. Blokland and Saskia S. Sterk --
Analysis of multiple mycotoxins in food / Jana
Hajslova, Milena Zachariasova, and Tomas Cajka --
Multi mycotoxin analysis in food products using
immunoaffinity extraction / Masahiko Takino, Hiroki
Tanaka, and Toshitsugu Tanaka -- Multiresidue
analysis of antibiotics in food of animal origin using
liquid chromatography-mass spectrometry / Katerina

Mastovska -- LC-MS/MS methods for the

determination of specific antibiotics residues in food
matrices / Gui-Liang Chen and Yan-Yan Fang --
Identification of unknown migrants from food contact
materials / Malcolm Driffield ... [et al.] -- Halogenated
persistent organic pollutants and polycyclic aromatic
hydrocarbons in food / Tomas Cajka and Jana
Hajslova.
Subjects Food--Safety measures.
Mass spectrometry.
Food Safety--methods.
Mass Spectrometry.
Notes Includes bibliographical references and index.
Series Methods in molecular biology, 1064-3745; 747
Springer protocols
Methods in molecular biology (Clifton, N.J.); v. 747.
Springer protocols.

Mass spectrometry in metabolomics: methods and protocols

LCCN 2014946353
Type of material Book
Main title Mass spectrometry in metabolomics: methods and
protocols / edited by Daniel Raftery, University of
Washington and Fred Hutchinson Cancer Research
Center, Seattle, WA, USA.
Published/Produced New York: Humana Press, [2014]
Description xvi, 360 pages: illustrations (some color); 26 cm.
Links Table of contents http://www.loc.gov/catdir/
enhancements/fy1501/2014946353-t.html
ISBN 9781493912575 (alk. paper)
1493912577 (alk. paper)
LC classification QP171 .M3627 2014
Related names Raftery, Daniel, editor.
Contents Overview of mass spectrometry-based metabolomics:
opportunities and challenges -- Global metabolic
profiling using ultra-performance liquid
chromatography/quadrupole time-of-flight mass
spectrometry -- LC-MS profiling to link metabolic and
phenotypic diversity in plant mapping populations --

Mitochondrial metabolomics using high-resolution

Fourier-transform mass spectrometry -- Sample
preparation methods for LC-MS-based global aqueous
metabolite profiling -- Methods of discovery-based and
targeted metabolite analysis by comprehensive two-
dimensional gas chromatography with time-of-flight
mass spectrometry detection -- Analysis of mouse liver
metabolites by GC x GC-TOF MS -- Metabolite
fingerprinting by capillary electrophoresis-mass
spectrometry -- Quantitative metabolomic profiling
using dansylation isotope labeling and liquid
chromatography mass spectrometry -- Quantitative
analysis of amino and organic acids by methyl
chloroformate derivatization and GC-MS/MS analysis
-- Stable isotope-labeled tracers for metabolic pathway
elucidation by GC-MS and FT-MS -- Multiplexed,
quantitative, and targeted metabolite profiling by LC-
MS/MRM -- Multidimensional mass spectrometry-
based shotgun lipidomics -- Comprehensive
quantitative determination of PUFA-related bioactive
lipids for functional lipidomics using high-resolution
mass spectrometry -- Ultra-performance liquid
chromatography-mass spectrometry targeted profiling
of bile acids: application to serum, liver tissue, and
cultured cells of different species -- Analysis of
volatile organic compounds in exhaled breath by gas
chromatography-mass spectrometry combined with
chemometric analysis -- Headspace SPME-GC-MS
metabolomics analysis of urinary volatile organic
compounds (VOCs) -- Metabolite profiling by direct
analysis in real-time mass spectrometry -- Analysis of
dried blood spots using DESI mass spectrometry --
DESI-MS imaging of lipids and metabolites from
biological samples -- Metabolic imaging using
nanostructure-initiator mass spectrometry (NIMS) --
Statistical analysis and modeling of mass
spectrometry-based metabolomics data.
Subjects Metabolites--Laboratory manuals.
Mass spectrometry--Laboratory manuals.

Metabolomics--Laboratory Manuals.
Mass Spectrometry--methods--Laboratory Manuals.
Mass spectrometry.
Metabolites.
Form/Genre Laboratory Manuals.
Handbooks, manuals, etc.
Notes Includes bibliographical references and index.
Series Methods in molecular biology, 1064-3745; 1198
Springer protocols
Methods in molecular biology (Clifton, N.J.); v. 1198.
1064-3745
Springer protocols (Series) 1949-2448

Metabolic profiling: methods and protocols

LCCN 2011414455
Type of material Book
Main title Metabolic profiling: methods and protocols / edited by
Thomas O. Metz.
Published/Created New York: Humana Press, c2011.
Description xi, 391 p.: ill; 27 cm.
Links Inhaltsverzeichnis. http://bvbr.bib-bvb.de:8991/F?func
=service&doc_library=BVB01&doc_number=022481
345&line_number=0001&func_code=DB_RECORDS
&service_type=MEDIA
ISBN 9781617379840 (hbk.: alk. paper)
1617379840 (hbk.: alk. paper)
9781617379857 (ebook)
LC classification QP171 .M37753 2011
Related names Metz, Thomas O.
Contents Origins of metabolic profiling / Arthur B. Robinson
and Noah E. Robinson -- Amino acid profiling for the
diagnosis of inborn errors of metabolism / Monique
Piraud ... [et al.] -- Acylcarnitines: analysis in plasma
and whole blood using tandem mass spectrometry /
David S. Millington and Robert D. Stevens -- Analysis
of organic acids and acylglycines for the diagnosis of
related inborn errors or metabolism by GC- and
HPLC-MS / Giancarlo la Marca and Cristiano Rizzo --
HPLC analysis for the clinical-biochemical diagnosis

of inborn errors of metabolism of purines and

pyrimidines / Giuseppe Lazzarino ... [et al.] -- Bile
acid analysis in various biological samples using ultra
performance liquid chromatography/electrospray
ionization-mass spectrometry (UPLC/ESI-MS) /
Masahito Hagio, Megumi Matsumoto, and Satoshi
Ishizuka -- Analysis of glycolytic intermediates with
ion chromatography- and gas chromatography-mass
spectrometry / Jan C. van Dam, Cor Ras, and Angela
ten Pierick -- Analysis of the citric acid cycle
intermediates using gas chromatography-mass
spectrometry / Rajan S. Kombu, Henri Brunengraber,
and Michelle A. Puchowicz -- Quantification of
pentose phosphate pathway (PPP) metabolites by
liquid chromatography-mass spectrometry (LC-MS) /
Amber Jannasch, Miroslav Sedlak, and Jiri Adamec.
High-performance liquid chromatography-mass
spectrometry (HPLC-MS)-based drug metabolite
profiling / Ian D. Wilson -- Gas chromatography-mass
spectrometry (GC-MS)-based metabolomics / Antonia
Garcia and Coral Barbas -- Use of two-dimensional
gas chromatography-time-of-flight mass spectrometry
(GCxGC-TOF-MS) for metabolomic analysis of polar
metabolites / Kimberly Ralston-Hooper ... [et al.] --
LC-MS-based metabolomics / Sunil Bajad and
Vladimir Shulaev -- Capillary electrophoresis-
electrospray ionization-mass spectrometry (CE-ESI-
MS)-based metabolomics / Philip Britz-McKibbin --
Liquid chromatography-mass spectrometry (LC-MS)-
based lipidomics for studies of body fluids and tissues
/ Heli Nygren ... [et al.] -- Electrospray ionization
tandem mass spectrometry (ESI-MS/MS)- based
shotgun lipidomics / Giorgis Isaac -- Processing and
analysis of GC/LC-MS based metabolomics data /
Elizabeth Want and Perrine Masson -- Nuclear
magnetic resonance (NMR)-based drug metabolite
profiling / Eva M. Lenz -- Nuclear magnetic resonance
(NMR)-based metabolomics / Hector C. Keun and
Toby J. Athersuch -- Slow magic angle sample

spinning: a non- or minimally invasive method for

high-resolution ¹H nuclear magnetic resonance (NMR)
metabolic profiling / Jian Zhi Hu -- Processing and
modeling of nuclear magnetic resonance (NMR)
metabolic profiles / Timothy M. D. Ebbels, John C.
Lindon, and Muireann Coen.
Subjects Metabolites--Laboratory manuals.
Metabolic profile tests--Laboratory manuals.
Metabolism--Disorders--Laboratory manuals.
Spectrum analysis--Laboratory manuals.
Metabolic Diseases.
Metabolism, Inborn Errors.
Form/Genre Laboratory Manuals.
Notes Includes bibliographical references and index.
Additional formats Online version: Metabolic profiling. New York, N.Y.:
Humana Press, c2011 (OCoLC)697514106
Series Methods in molecular biology; v. 708
Springer protocols.
Methods in molecular biology (Clifton, N.J.): v. 708.
1064-3745
Springer protocols.

Metabonomics: methods and protocols

LCCN 2015931074
Type of material Book
Main title Metabonomics: methods and protocols / edited by
Jacob T. Bjerrum, Department of Gastroenterology,
Medical Section, Herlev Hospital, University of
Copenhagen, Copenhagen, Denmark.
Published/Produced New York: Humana Press, [2015]
©2015
Description x, 259 pages: illustrations (some color); 26 cm.
ISBN 9781493923762 (alk. paper)
1493923765 (alk. paper)
LC classification QR171.G29 M48 2015
QH506 .M45 v.1277
Related names Bjerrum, Jacob T., editor.
Springer Science+Business Media, copyright holder.
Contents Metabonomics: analytical techniques and associated

chemometrics / Jacob T. Bjerrum -- Sample collection

and preparation of biofluids and extracts for NMR
spectroscopy / Gwénaëlle Le Gall -- NMR
sprectroscopy of biofluids and extracts / Gwénaëlle Le
Gall -- High-resolution magic-angle-spinning NMR
spectroscopy of intact tissue / Guro F. Giskeødegård,
Maria D. Cao, and Tone F. Bathen -- Sample
collection and preparation of biofluids and extracts for
liquid chromatography-mass spectrometry / Peiyuan
Yin [and three others] -- Liquid chromatography-mass
spectrometry of biofluids and extracts / Xinjie Zhao
[and three others] -- Sample collection and preparation
of biofluids and extracts for gas chromatography-mass
spectrometry / Abdul-Hamid M. Emwas, Zeyad A. Al-
Talla, and Najeh M. Kharbatia -- Gas chromatography-
mass spectrometry of biofluids and extracts / Abdul-
Hamid M. Emwas [and three others] -- Capillary
electrophoresis-mass spectrometry / Masataka
Wakayama, Akiyoshi Hirayama, and Tomoyosji Soga
-- Preprocessing of raw metabonomic data / Riyas
Vettukattil -- Extracting meaningful information from
metabonomic data using multivariate statistics / Max
Bylesjö -- Combining metabonomics and other -omics
data / Mattias Rantalainen -- The strengths and
weaknesses of NMR-spectroscopy and mass
spectrometry with particular focus on metabolomics
research / Abdul-Hamid M. Emwas -- Metabonomics
and drug development / Pranov Ramana [and three
others] -- Metabonomics and toxicology / Liang Zhao
and Thomas Hartung -- Metabonomics and diagnostics
/ Lucy C. Hicks, Simon J.L. Ralphs, and Horace R.T.
Williams -- Metabonomics and systems biology /
Vicky De Preter.
Subjects Gastrointestinal system--Microbiology--Laboratory
manuals.
Microbial metabolites--Laboratory manuals.
Nuclear magnetic resonance spectroscopy--Laboratory
manuals.
Analytical biochemistry--Technique--Laboratory

manuals.
Metabolomics--methods--Laboratory Manuals.
Cell Extracts--analysis--Laboratory Manuals.
Metabolome--Laboratory Manuals.
Form/Genre Laboratory Manuals.
Notes Includes bibliographic references and index.
Series Methods in molecular biology, 1064-3745; 1277
Springer protocols
Methods in molecular biology (Clifton, N.J.); v. 1277.
Springer protocols (Series)

Natural products from marine algae: methods and protocols

LCCN 2015940760
Type of material Book
Main title Natural products from marine algae: methods and
protocols / edited by Dagmar B. Stengel, Botany and
Plant Science, School of Natural Sciences, Ryan
Institute for Environmental, Marine and Energy
Research, National University of Ireland Galway,
Galway, Ireland, Solène Connan, Photobiotechnology,
INTECHMER, Conversative National des Arts et
Métiers, Cherbourg, Cedex, France, CNRS, GEPEA,
UMR6144, Boulevard de l'Université, Saint Nazaire,
Cedex, France.
Published/Produced New York, NY: Humana Press Springer, [2015]
©2015
Description xiv, 439 pages: illustrations (some color); 27 cm.
ISBN 9781493926831 (alk. paper)
1493926837 (alk. paper)
(eBook)
(eBook)
LC classification QK570.2 .N38 2015
Related names Stengel, Dagmar B., editor.
Connan, Solène, 1976- editor.
Contents Marine algae: A source of biomass for
biotechnological applications -- Structure and function
of macroalgal natural products -- Spectrophotometric
assays of major compounds extracted from algae --
Extraction and enrichment of protein from red and

green macroalgae -- Extraction and purification of r-

phycoerythrin from marine red algae -- Extraction and
analysis of mycosporine-like amino acids in marine
algae -- Extraction and purification of phlorotannins
from brown algae -- Enzyme-enhanced extraction of
antioxidant ingredients from algae -- Microwave-
assisted extraction of fucoidan from marine algae --
Extraction and analysis of oxylipins from macroalgae
illustrated on the example gracilaria vermiculophylla --
Lipids and fatty acids in algae: Extraction,
fractionation into lipid classes, and analysis by gas
chromatography coupled with flame ionization
detector (GC-FD) -- HRMAS NMR analysis of algae
and identification of molecules of interest via
conventional 1d and 2d nmr: Sample preparation and
optimization of experimental conditions -- Extraction,
purification, and NMR analysis of terpenes from
brown algae -- Extraction, isolation, and identification
of sesquiterpenes from laurencia species -- The use of
HPLC for the characterization of phytoplankton
pigments -- Characterization of phlorotannins from
brown algae by lc-hrms -- Analysis of betaines from
marine algae using lc-ms-ms -- Analysis of marine
biotoxins using lc-ms/ms -- Fucoidan analysis by
tandem maldi-tof and esi mass spectrometry --
Determination of substitution patterns of galactans
from green seaweeds of the bryopsidales -- Structural
characterization of a hybrid carrageenan-like sulfated
galactan from a marine red alga furcellaria lumbricalis
-- Characterization of alginates by nuclear magnetic
resonance (NMR) and vibrational spectroscopy (IR,
NIR, RAMAN) in combination with chemometrics --
Imaging and identification of marine algal bioactive
compounds by surface enhanced raman spectroscopy
(SERS) -- In vitro protocols for measuring the
antioxidant capacity of algal extracts -- Disk diffusion
assay to assess the antimicrobial activity of marine
algal extracts -- Screening of a marine algal extract for
antifungal activities -- Protocol for assessing

antifouling activities of macroalgal extracts.

Subjects Marine natural products--Laboratory manuals.
Marine algae--Laboratory manuals.
Marine algae--Biotechnology.
Seaweed.
Marine algae.
Marine algae--Biotechnology.
Marine natural products.
Form/Genre Laboratory Manuals.
Laboratory manuals.
Notes Includes bibliographical references and index.
Series Methods in molecular biology, 1940-6029; 1308
Springer protocols
Methods in molecular biology (Clifton, N.J.); v. 1308.
1940-6029
Springer protocols (Series) 1949-2448

Optimization of chromatographic technique for regular monitoring of

greenhouse gases
LCCN 2011323178
Type of material Book
Main title Optimization of chromatographic technique for regular
monitoring of greenhouse gases [microform] / by S.K.
Sahu ... [et al.].
Published/Created Mumbai: Bhabha Atomic Research Centre, 2010.
Description 29 p.: ill.; 29 cm.
LC classification Microfiche 2013/60096 (Q)
Related names Sahu, S. K.
Bhabha Atomic Research Centre.
Subjects Gas chromatography.
Greenhouse gases.
Notes At head of title: Government of India, Atomic Energy
Commission.
"BARC report"--Cover.
Includes bibliographical references (p. 29).
Abstract in English and Hindi.

Pharmaceutical analysis: a textbook for pharmacy students and

pharmaceutical chemists
LCCN 2012021958
Type of material Book
Personal name Watson, David G., 1952-
Main title Pharmaceutical analysis: a textbook for pharmacy
students and pharmaceutical chemists / David G.
Watson; with a contribution by RuAngelie Edrada-
Ebel.
Edition 3rd ed.
Published/Created Edinburgh; New York: Churchill Livingstone Elsevier,
2012.
Description xi, 427 p.: ill.; 26 cm.
ISBN 9780702046216
0702046213
LC classification RS403 .W38 2012
Contents Control of the quality of analytical methods -- Physical
and chemical properties of drug molecules --
Titrimetric and chemical analysis methods --
Ultraviolet and visible spectroscopy -- Infrared
spectrophotometry -- Atomic spectrophotometry --
Molecular emission spectroscopy -- Nuclear magnetic
resonance spectroscopy -- Mass spectrometry --
Chromatographic theory -- Gas chromatography --
High-pressure liquid chromatography -- Thin layer
chromatography -- High-performance capillary
electrophoresis -- Extraction methods in
pharmaceutical analysis.
Subjects Pharmaceutical chemistry.
Drugs--Analysis.
Pharmaceutical Preparations--analysis.
Chromatography--methods.
Spectrophotometry--methods.
Spectrum Analysis--methods.
Notes Includes bibliographical references and index.

Pheromone signaling: methods and protocols

LCCN 2013947162
Type of material Book

Main title Pheromone signaling: methods and protocols / edited

by Kazushige Touhara, Department of Applied
Biological Chemistry, Graduate School of Agricultural
and Life Sciences. The University of Tokyo, Japan.
Published/Created New York: Humana Press: Springer, c2013.
Description xv, 399 p.: ill. (some col.); 26 cm.
ISBN 9781627036184 (alk. paper)
1627036180 (alk. paper)
LC classification QP572.P47 P44 2013
Related names Touhara, Kazushige, editor.
Contents Female moth pheromones / Tetsu Ando -- Pheromones
in the fruit fly / Jacqueline S.R. Chin and Joanne Y.
Yew -- Analysis of volatile mouse pheromones by gas
chromatography mass spectrometry / Milos V.
Novotny and Helena A. Soini -- Murine nonvolatile
pheromones: isolation of exocrine-gland secreting
peptide 1 / Hiroko Kimoto and Kazushige Touhara --
Chemical analysis of aquatic pheromones in fish /
Michael Stewart, Cindy F. Baker, and Peter W.
Sorensen -- Analysis of ascarosides from
Caenorhabditis elegans using mass spectrometry and
NMR spectroscopy / Xinxing Zhang ... [et al.] --
Identification of chemosensory receptor genes from
vertebrate genomes / Yoshihito Niimura -- Functional
assays for insect olfactory receptors in Xenopus
oocytes / Tatsuro Nakagawa and Kaushige Touhara --
A protocol for heterologous expression and functional
assay for mouse pheromone receptors / Sandeepa Dey,
Senmiao Zhan, and Hiroaki Matsunami -- Genetic
manipulation to analyze pheromone responses:
knockouts of multiple receptor genes / Tomohiro Ishii
-- Electroantennogram and single sensillum recording
in insect antennae / Shannon B. Olsson and Bill S.
Hansson -- Calcium imaging of pheromone responses
in the insect antennal lobe / Susy M. Kim and Jing W.
Wang -- Live cell calcium imaging of dissociated
vomeronasal neurons / Angeldeep Kaur, Sandeepa De,
and Lisa Stowers -- Whole-mount imaging of
responses in mouse vomeronasal neurons / Pei Sabrina

Xu and Timothy E. Holy -- Calcium imaging of

vomeronasal organ response using slice preparations
from transgenic mice expressing G-CaMP2 / C. Ron
Yu -- The electrovomeronasogram: field potential
recordings in the mouse vomeronasal organ / Trese
Leinders-Zufall and Frank Zufall -- Electrical
recordings from the accessory olfactory bulb in VNO-
AOB ex vivo preparations / Julian P. Meeks and
Timothy E. Holy -- Pheromone -induced expression of
immediate early genes in the mouse vomeronasal
sensory system / Sachiko Haga-Yamanaka and
Kazushige Touhara -- Insect pheromone behavior: fruit
fly / Daisuke Yamamoto, Soh Kohatsu, and Masayuki
Koganezawa -- Quantitative assessment of pheromone-
induced dauer formation in Caenorhabditis elegans /
Scott J. Neal, Kyuhyung Kim, and Piali Sengupta --
Acute behavioral responses to pheromones in C.
elegans (adult behaviors: attraction, repulsion) / Heeun
Jang and Cornelia I. Bargmann -- Behavioral analysis
of pheromones in fish / Peter W. Sorensen -- Analysis
of male aggressive and sexual behavior in mice /
Takefumi Kikusui -- Assessment of urinary pheromone
discrimination, partner preference, and mating
behaviors in female mice / Olivier Brock, Julie Bakker,
and Michael J. Baum.
Subjects Pheromones.
Semiochemicals.
Animal communication.
Pheromones.
Animal communication.
Pheromones.
Semiochemicals.
Notes Includes bibliographical references and index.
Series Methods in molecular biology, 1064-3745; 1068
Springer protocols, 1949-2448
Methods in molecular biology (Clifton, N.J.); v. 1068.
Springer protocols (Series), 1949-2448

Plant cold acclimation: methods and protocols

LCCN 2014938067
Type of material Book
Main title Plant cold acclimation: methods and protocols / edited
by Dirk K. Hincha, Max-Planck-Institute für
Molekulare Pflanzenphysiologie, Potsdam, Germany,
Ellen Zuther, Max-Planck-Institute für Molekulare
Pflanzenphysiologie, Potsdam, Germany.
Published/Produced New York: Humana Press, [2014]
©2014
Description xi, 282 pages: illustrations (some color), still
photographic images (black and white); 26 cm
Links http://www.springerimages.com/videos/978-1-4939-
0843-1
ISBN 9781493908431 (alk. paper)
149390843X (alk. paper)
LC classification QK913 .P559 2014
Related names Hincha, Dirk K., editor.
Zuther, Ellen, editor.
Contents Introduction: plant cold acclimation and freezing
tolerance / Dirk K. Hincha and Ellen Zuther --
Measuring freezing tolerance: survival and regrowth
assays / Daniel Z. Skinner and Kimberly Garland-
Campbell -- Measuring freezing tolerance: electrolyte
leakage and chlorophyll fluorescence assays / Anja
Thalhammer, Dirk K. Hincha, and Ellen Zuther --
Conducting field trials for frost tolerance breeding in
cereals / Luigi Cattivelli -- A whole-plant screening
test to identify genotypes with superior freezing
tolerance / Annick Bertrand, Yves Castonguay, and
Josée Bourassa -- Mapping of quantitative trait loci
(QTL) associated with plant freezing tolerance and
cold acclimation / Evelyne Téoulé and Carine Géry --
Common garden experiments to characterize cold
acclimation responses in plants from different climatic
regions / Andrey V. Malyshev, Hugh A.L. Henry, and
Juergen Kreyling -- Identification of Arabidopsis
mutants with altered freezing tolerance / Carlos Perea-
Resa and Julio Salinas -- Infrared thermal analysis of

plant freezing processes / Gilbert Neuner and Edith

Kuprian -- Cryo-scanning electron microscopy to study
the freezing behavior of plant tissues / Seizo Fujikawa
and Keita Endoh -- Three-dimensional reconstruction
of frozen and thawed plant tissues from microscopic
images / David P. Livingston III and Tan D. Tuong --
Proteomic approaches to identify cold-regulated
soluble proteins / Stefanie Döll, Rico Lippmann, and
Hans-Peter Mock -- Proteomic approaches to identify
cold-regulated plasma membrane proteins / Daisuke
Takahashi [and four others] -- Profiling methods to
identify cold-regulated primary metabolites using gas
chromatography coupled to mass spectrometry /
Frederik Dethloff [and eigt others] -- A lipidomic
approach to identify cold-induced changes in
Arabidopsis membrane lipid composition / Hieu Sy Vu
[and three others] -- Quantification of superoxide and
hydrogen peroxide in leaves / Ilona Juszczak and
Margarete Baier -- Estimating ice encasement
tolerance of herbage plants / Bjarni E. Gudleifsson and
Brynhildur Bjarnadottir -- Characterization of ice
binding proteins from sea ice algae / Maddalena
Bayer-Giraldi, EonSeon Jin, and Peter W. Wilson --
Isolation and characterization of ice-binding proteins
from higher plants / Adam J. Middleton [and five
others].
Subjects Acclimatization (Plants)--Laboratory manuals.
Plants--Frost resistance--Laboratory manuals.
Plants--Effect of cold on--Laboratory manuals.
Acclimatization--Laboratory Manuals.
Plant Physiological Processes--Laboratory Manuals.
Cold Temperature--Laboratory Manuals.
Acclimatization (Plants)
Plants--Effect of cold on.
Plants--Frost resistance.
Plantes.
Plantes--génétique.
Reproduction sélective.
Acclimatation.

Phénomènes physiologiques des plantes.

Température froide.
Plantes--Acclimatation.
Génétique végétale.
Plantes--Écophysiologie.
Form/Genre Laboratory Manuals.
Handbooks, manuals, etc.
Notes "Vidoes to this book can be accessed at:
http://www.springerimages.com/videos/978-1-4939-
0843-1" --Title page verso.
Includes bibliographical references and index.
Series Methods in molecular biology, 1064-3745; 1166
Springer protocols
Methods in molecular biology (Clifton, N.J.); v. 1166.
1064-3745
Springer protocols (Series) 1949-2448

Plant isoprenoids: methods and protocols

LCCN 2014936605
Type of material Book
Main title Plant isoprenoids: methods and protocols / edited by
Manuel Rodríguez-Concepción, Center for Research in
Agricultural Genomics (CRAG), CSIC-IRTA-UAB-
UB, Barcelona, Spain.
Published/Produced New York: Humana Press, [2014]
©2014
Description xi, 303 pages: illustrations (some color); 26 cm.
Links Table of contents http://www.loc.gov/catdir/
enhancements/fy1407/2014936605-t.html
ISBN 9781493906055 (alk. paper)
1493906054 (alk. paper)
LC classification QK898.I76 P58 2014
Related names Rodríguez-Concepción, Manuel, editor.
Springer Science+Business Media, copyright holder.
Contents Plant isoprenoids: A General Overview -- Measuring
the Activity of 1-Deoxy-D-Xylulose 5-Phosphate
Synthase, the First Enzyme in the MEP Pathway, in
Plant Extracts -- Determination of 3-Hydroxy-3-
methylglutaryl CoA Reductase Activity in Plants --

Farnesyl Diphosphate Synthase Assay -- Metabolite

Profiling of Plastidial Deoxyxylulose-5-Phosphate
Pathway Intermediates by Liquid Chromatography and
Mass Spectrometry -- Analysis of Carotenoids and
Tocopherols in Plant Matrices and Assessment of
Their In Vitro Antioxidant Capacity -- Simultaneous
Analyses of Oxidized and Reduced Forms of
Photosynthetic Quinones by High-Performance Liquid
Chromatography -- Determination of Sterol Lipids in
Plant Tissues by Gas Chromatography and Q-TOF
Mass Spectrometry -- Analysis of Plant
Polyisoprenoids -- Analysis of Diterpenes and
Triterpenes from Plant Foliage and Roots -- Gas
Chromatography Mass-Spectrometry Method for
Determination of Biogenic Volatile Organic
Compounds Emitted by Plants -- Analysis of Steroidal
Alkaloids and Saponins in Solanaceae Plant Extracts
using UPLC-qTOF Mass Spectrometry -- Isoprenoid
and Metabolite Profiling of Plant Trichomes -- Sample
Preparation for Single Cell Transcriptomics --
Essential Oil Glands in Citrus Fruit Peel as an
Example -- Prenylquinone Profiling in Whole Leaves
and Chloroplast Subfractions -- Confocal Laser
Scanning Microscopy Detection of Chlorophylls and
Carotenoids in Chloroplasts and Chromoplasts of
Tomato Fruit -- Heterologous Expression of Triterpene
Biosynthetic Genes in Yeast and Subsequent
Metabolite Identification Through GC-MS -- High
Throughput Testing of Terpenoid Biosynthesis
Candidate Genes Using Transient Expression in
Nicotiana benthamiana -- Heterologous Stable
Expression of Terpenoid Biosynthetic Genes Using the
Moss Physcomitrella patens -- Quantification of Plant
Resistance to Isoprenoid Biosynthesis Inhibitors -- A
Flexible Protocol for Targeted Gene Co-Expression
Network Analysis.
Subjects Isopentenoids--Laboratory manuals.
Terpenes--metabolism--Laboratory Manuals.
Plants--metabolism--Laboratory Manuals.

Terpenes--analysis--Laboratory Manuals.
Terpenes--pharmacology--Laboratory Manuals.
Form/Genre Laboratory Manuals.
Notes Includes bibliographical references and index.
Series Methods in molecular biology, 1064-3745; 1153
Springer protocols
Methods in molecular biology (Clifton, N.J.); 1153.
1064-3745
Springer protocols (Series) 1949-2448

Plant lipid signaling protocols

LCCN 2013934702
Type of material Book
Main title Plant lipid signaling protocols / edited by Teun
Munnick, Swammerdam Institute for Life Sciences,
Section Plant Physiology, University of Amsterdam,
Amsterdam, The Netherlands, Ingo Heilmann,
Department of Cellular Biochemistry, Institute for
Biochemistry and Biotechnology, Martin-Luther-
University Halle-Wittenberg, Halle, Germany.
Published/Created New York: Humana Press, c2013.
Description xi, 305 p.: ill.; 27 cm.
ISBN 9781627034005 (alk. paper)
1627034005 (alk. paper)
LC classification QK725 .P4754 2013
QH506 .M45 v.1009
Related names Munnik, Teun.
Heilmann, Ingo.
Summary As scientist begin to understand the complexity of
lipid signaling and its roles in plant biology, there is an
increasing interest in their analysis. Due to the low
abundancy and transient nature of some of these
hydrophobic compounds, this is not always easy. In
Plant Lipid Signaling Protocols, expert researchers in
the field detail experimental approaches by which
plant signaling lipids can be studied. These methods
and techniques include analysis of plant signaling
lipids, including detailed protocols to detect various
relevant compounds by targeted or non-targeted

approaches; to assay relevant enzyme activities in

biological material or using recombinant enzymes; to
test for specific binding of signaling lipids to protein
partners; or to visualize signaling lipids or lipid-
derived signals in living plant cells. Written in the
highly successful Methods in Molecular Biology series
format, chapters include introductions to their
respective topics, lists of the necessary materials and
reagents, step-by-step, readily reproducible laboratory
protocols, and key tips on troubleshooting and
avoiding known pitfalls. Authoritative and practical,
Plant Lipid Signaling Protocols aids plant researchers
in the continuing to study the roles of lipid signals.
Contents Analyzing plant signaling phospholipids through 32Pi-
labeling and TLC / Teun Munnik and Xavier Zarza --
Analysis of D3-,4-,5-phosphorylated
phosphoinositides using HPLC / Teun Munnik -- Mass
measurement of polyphosphoinositides by thin-layer
and gas chromatography / Mareike Heilmann and Ingo
Heilmann -- Measurement of inositol (1,4,5)
trisphosphate in plant tissues by a competitive receptor
binding assay / Ingo Heilmann and Imara Y. Perera --
Quantification of diacylglycerol by mass spectrometry
/ Katharina vom Dorp, Isabel Dombrink, and Peter
Dörmann -- Distinguishing phosphatidic acid pools
from de novo synthesis, PLD, and DGK / Steven A.
Arisz and Teun Munnik -- Use of phospholipase A2
for the production of lysophospholipids / Steven A.
Arisz and Teun Munnik -- Analysis and quantification
of plant membrane lipids by thin-layer
chromatography and gas chromatography / Vera
Wewer, Peter Dörmann, and Georg Hölzl -- Lipidomic
analysis of plant membrane lipids by direct infusion
tandem mass spectrometry / Sunitha Shiva ... [et al.] --
Detection and quantification of plant sphingolipids by
LC-MS / Jonathan E. Markham -- Analysis of defense
signals in Arabidopsis thaliana leaves by ultra-
performance liquid chromatography/tandem mass
spectrometry: jasmonates, salicylic acid, abscisic acid /

Nadja Stingl ... [et al.] -- Analysis of fatty acid amide

hydrolase activity in plants / Sang-Chul Kim, Lionel
Faure, and Kent D. Chapman -- Ionization behavior of
polyphosphoinositides determined via the preparation
of pH titration curves using solid-state 31P NMR /
Zachary T. Graber and Edgar E. Kooijman --
Phosphatidylinositol synthase activity from plant
membrane fractions and from E. coli- expressed
recombinant peptides / Sylvie Collin and Françoise
Cochet -- Phosphatidylinositol 4-kinase and
phosphatidylinositol 4-phosphate 5-kinase assays /
Yang Ju Im ... [et al.] -- Assaying inositol and
phosphoinositide phosphatase enzymes / Janet L.
Donahue, Mustafa Ercetin, and Glenda E. Gillaspy --
Determination of phospholipase C activity in vitro /
S.M. Teresa Hernández-Sotomayor and J. Armando
Muñoz-Sanchez -- Assaying nonspecific
phospholipase C activity / P řemysl Pejchar, Günther
F.E. Scherer, and Jan Martinec -- Assaying different
types of plant phospholipase D activities in vitro / Kirk
L. Pappan and Xuemin Wang -- Measuring PLD
activity in vivo / Teun Munnik and Ana M. Laxalt --
Assaying plant phosphatidic acid phosphatase activity
/ Yuki Nakamura -- Assay of phospholipase A activity
/ Michael Heinze and Werner Roos -- Lipid-binding
analysis using a fat blot assay / Teun Munnik and
Magdalena Wierzchowiecka -- Liposome-binding
assays to assess specificity and affinity of
phospholipid-protein interactions / Magdalena M.
Julkowska, Johanna M. Rankenberg, and Christa
Testerink -- Lipid affinity beads: from identifying new
lipid binding proteins to assessing their binding
properties / Fionn McLoughlin and Christa Testerink --
Using genetically encoded fluorescent reporters to
image lipid signalling in living plants / Joop E.M.
Vermeer and Teun Munnik -- Imaging changes in
cytoplasmic calcium using the yellow cameleon 3.6
biosensor and confocal microscopy / Sarah J. Swanson
and Simon Gilroy.

Subjects Plant cellular signal transduction--Laboratory manuals.

Plant lipids--Laboratory manuals.
Lipids--biosynthesis--Laboratory Manuals.
Lipid Metabolism--Laboratory Manuals.
Plants--chemistry--Laboratory Manuals.
Plant cellular signal transduction.
Plant lipids.
Subject keywords Life sciences.
Botany.
Plant Sciences.
Form/Genre Handbooks, manuals, etc.
Notes Includes bibliographical references and index.
Series Methods in molecular biology, 1064-3745; 1009
Springer protocols, 1949-2448
Methods in molecular biology (Clifton, N.J.); v. 1009.
1064-3745
Springer protocols (Series) 1949-2448

Plant metabolomics: methods and protocols

LCCN 2011945849
Type of material Book
Main title Plant metabolomics: methods and protocols / edited by
Nigel W. Hardy, Robert D. Hall.
Published/Created New York: Humana Press: Springer, c2012.
Description xiii, 340 p.: ill. (some col.); 27 cm.
Links Publisher description http://www.loc.gov/catdir/
enhancements/fy1306/2011945849-d.html
Table of contents only http://www.loc.gov/catdir/
enhancements/fy1306/2011945849-t.html
ISBN 9781617795930
1617795933
LC classification QK887 .P53 2012
Related names Hardy, Nigel W.
Hall, Robert D. (Robert David), 1958-
Contents Practical applications of metabolomics in plant biology
/ Robert D. Hall and Nigel W. Hardy -- Part I Material
preparation -- Aspects of experimental design for plant
metabolomics experiments and guidelines for growth
of plant material / Yves Gibon and Dominique Rolin --

Separating the inseparable: the metabolomic analysis

of plant-pathogen interactions / J. William Allwood ...
[et al.] -- Precautions for harvest, sampling, storage,
and transport of crop plant metabolomics samples /
Benoît Biais ... [et al.] -- Tissue preparation using
arabidopsis / Aimee M. Llewellyn ... [et al.] -- Part II
Chemical analysis approaches -- Solid phase micro-
extraction GC-MS analysis of natural volatile
components in melon and rice / Harrie A. Verhoeven
... [et al.] -- Profiling primary metabolites of tomato
fruit with gas chromatography/mass spectrometry /
Sonia Osorio, Phuc Thi Do, and Alisdair R. Fernie --
High-performance liquid chromatography-mass
spectrometry analysis of plant metabolites in
brassicaceae / Ric C.H. De Vos, Bert Schipper, and
Robert D. Hall -- UPLC-MS-based metabolite analysis
in tomato / Ilana Rogachev and Asaph Aharoni -- High
precision measurement and fragmentation analysis for
metabolite identification / Madalina Oppermann ... [et
al.] -- Fourier transform ion cyclotron resonance mass-
spectrometry for plant metabolite profiling and
metabolite identification / J. William Allwood ... [et
al.] -- Combined NMR and flow injection ESI-MS for
brassicaceae metabolomics / John M. Baker, Jane L.
Ward, and Michael H. Beale -- ICP-MS and LC-ICP-
MS for analysis of trace elements content and
speciation in cereal grains / D.P. Persson ... [et al.] --
The use of genomics and metabolomics methods to
quantify fungal endosymbionts and alkaloids in
grasses / Susanne Rasmussen ... [et al.] -- Part III Data
analysis -- Data (pre- )processing of nominal and
accurate mass LC-MS or GC-MS data using MetAlign
/ Arjen Lommen -- TagFinder: preprocessing software
for the fingerprinting and the profiling of gas
chromatography-mass spectrometry based metabolome
analyses / Alexander Luedemann ... [et al.] -- Chemical
identification strategies using liquid chromatography-
photodiode array-solid phase extraction-nuclear
magnetic resonance/mass spectrometry / Sofia Moco

and Jacques Vervoort -- A strategy for selecting data

mining techniques in metabolomics / Ahmed Hmaidan
BaniMustafa and Nigel W. Hardy.
Subjects Plant metabolites--Laboratory manuals.
Plants--Metabolism--Laboratory manuals.
Methode.
Pflanzen.
Stoffwechselphysiologie.
Methode.
Pflanzen.
Stoffwechselphysiologie.
Form/Genre Aufsatzsammlung.
Notes Includes bibliographical references and index.
Series Methods in molecular biology; 860
Springer protocols
Methods in molecular biology (Clifton, N.J.); v. 860.
Springer protocols.

Polyamines: methods and protocols

LCCN 2011921314
Type of material Book
Main title Polyamines: methods and protocols / edited by
Anthony E. Pegg, Robert A. Casero, Jr.
Published/Created New York: Humana Press/Springer, c2011.
Description xiv, 523 p.: ill.; 27 cm.
Links Publisher description http://www.loc.gov/catdir/
enhancements/fy1113/2011921314-d.html
Table of contents only http://www.loc.gov/catdir/
enhancements/fy1113/2011921314-t.html
ISBN 9781617790331 (alk. paper)
1617790338 (alk. paper)
9781617790348 (e-ISBN)
1617790346 (e-ISBN)
LC classification QP801.P638 P6488 2011
Related names Pegg, Anthony E.
Casero, Robert Anthony.
Contents Current status of the polyamine research field /
Anthony E. Pegg and Robert A. Casere, Jr. --
Exploring polyamine biosynthetic diversity through

comparative and functional genomics / Anthony J.

Michael -- Characterization of genes for polyamine
modulon / Kazuei Igarashi and Keiko Kashiwagi --
Posttranscriptional regulation of gene expression in
epithelial cells by polyamines / Lan Xiao and Jian-
Ying Wang -- Identification, chemical synthesis, and
biological functions of unusual polyamines produced
by extreme thermophiles / Tairo Oshima, Toshiyuki
Moriya, and Yusuke Terui -- Polyamine block of
inwardly rectifying potassium channels / Harley T.
Kurata, Wayland W.L. Cheng, and Colin G. Nichols --
Carcinogenesis studies in mice with genetically
engineered alterations in polyamine metabolism /
David J. Feith -- Transgenic rodents with altered SSAT
expression as models of pancreatitis and altered
glucose with lipid metabolism / Anne Uimari ... [et al.]
-- Use of (gyro) gy and spermine synthase transgenic
mice to study functions of spermine / Xiaojing Wang
and Anthony E. Pegg -- Simple assay for mammalian
spermine oxidase: a polyamine catabolic enzyme
implicated in drug response and disease / Andrew C.
Goodwin, Tracy R. Murray-Stewart, and Robert A.
Casero, Jr. -- Characterization, assay, and substrate
specificity of plant polyamine oxidases / Panagiotis N.
Moschou and Kalliopi A. Roubelakis-Angelakis --
Assay of deoxyhypusine synthase activity / Jong Hwan
Park, Edith C. Wolff, and Myung Hee Park --
Identification and assay of allosteric regulators of S-
adenosylmethionine decarboxylase / Erin K. Willert,
Lisa N. Kinch, and Margaret A. Phillips -- Protocols
for studying antizyme expression and function /
Noriyuki Murai, Yasuko Murakami, and Senya
Matsufuji -- Identification, assay and functional
analysis of the antizyme inhibitor family / Chaim
Kahana -- Posttranscriptional regulation of ornithine
decarboxylase / Shannon L. Nowotarski, Sofia
Origanti, and Lisa M. Shantz -- Identification and
assays of polyamine transport systems in Escherichia
coli and Saccharomyces cerevisiae / Keiko Kashiwagi

and Kazuei Igarashi -- Genetic and biochemical

analysis of protozoal polyamine transporters / Marie-
Pierre Hasne and Buddy Ullman -- Heparan sulfate
proteoglycan-mediated polyamine uptake / Johanna
Welch ... [et al.] -- Polyamine transport sysems in
mammalian cells and tissues / Takeshi Uemura and
Eugene W. Gerner -- Procedures to evaluate the
importance of dietary polyamines / Paul Acheampong,
Mary J. Macleod, and Heather M. Wallace --
Determination of N¹,N¹²-diacetylspermine in urine: a
novel tumor marker / Masao Kawakita ... [et al.] --
Spermidine/spermine-N¹-acetyltransferase in kidney
ischemia reperfusion injury / Kamyar Zahedi and
Manoocher Soleimani -- Use of polyamine metabolites
as markers for stroke and renal failure / Kazuei
Igarashi and Keiko Kashiwagi -- Methods to evaluate
alterations in polyamine metabolism caused by
Helicobacter pylori infection / Alain P. Gobert, Rupesh
Chaturvedi, and Keith T. Wilson -- High-resolution
capillary gas chromatography in combination with
mass spectrometry for quantification of three major
polyamines in postmortem brain cortex / Gary Gang
Chen ... [et al.] -- Spermine synthase deficiency
resulting in X-linked intellectual disabiltiy (Snyder-
Robinson Syndrome) / Charles E. Schwartz, Xaiojing
Wang, Roger E. Stevenson, and Anthony E. Pegg --
Methylated polyamines as research tools / Alex R.
Khomutov ... [et al.] -- Fluorescent substrates for
polyamine catabolic enzymes and transport / Koichi
Takao and Akira Shirahata -- Use of polyamine
derivatives as selective histone deacetylase inhibitors /
Patick M. Woster -- Measurement of polyamine pKa
values / Ian S. Blagbrough, Abdelkader A. Metwally,
and Andrew J. Geall -- Polyamine analysis by LC-MS
/ Merja R. Hakkinen.
Subjects Polyamines.
Polyamines.
Spermine.
Notes Includes bibliographical references and index.

Series Methods in molecular biology, 1064-3745; v. 720

Springer protocols
Methods in molecular biology (Clifton, N.J.); v. 720.
1064-3745
Springer protocols.

Practical gas chromatography: a comprehensive reference

LCCN 2014952603
Type of material Book
Main title Practical gas chromatography: a comprehensive
reference / [edited by] Katja Dettmer-Wilde.
Published/Produced New York: Springer, 2014.

Practical approaches to method validation and essential instrument

qualification
LCCN 2009054243
Type of material Book
Main title Practical approaches to method validation and essential
instrument qualification / edited by Chung Chow
Chan, Herman Lam, Xue Ming Zhang.
Published/Created Hoboken, N.J.: Wiley, c2010.
Description xiv, 399 p.: ill.; 25 cm.
ISBN 9780470121948 (hardback)
0470121947 (hardback)
LC classification RS189 .P66 2010
Related titles Method validation and instrument performance
verification.
Related names Chan, Chung Chow.
Lam, Herman.
Zhang, Xue-Ming.
Summary "The objective of this book is provide information in
same practical, hands-on manner as the first book
"Analytical Method Validation and Instrument
Performance Verification", on important, but more
advance topics. It will focus on additional and
supplemental methods, instruments, and electronic
systems that are used in pharmaceutical,
biopharmaceutical, and clinical testings. These tests
will generate reliable data that is in compliance with

current Good Manufacturing Practices (cGMP) and

will follow Good Analytical Practices"--Provided by
publisher.
Contents (Publisher-supplied data) Overview of Risk Based
Approach to Phase Appropriate Validation and
Instrument Qualification / Phase Appropriate Method
Validation / Analytical Method Verification, Method
Revalidation, and Method Transfer / Validation of
PAT Applications / The Validation of Near Infrared
Systems for Raw Material Identification / Cleaning
Validation / Risk Based Validation of laboratory
Information Management Systems (LIMS) /
Performance Qualification and Verification of Balance
/ Performance Verification of NIR Spectrophotometers
/ Operational Qualification in Practice for Gas
Chromatography Instruments / Performance
Verification on RI, Fluorescence, Evaporative Light
Scattering Detection / Instrument Qualification and
Performance Verification for Particle Size Instruments
/ Method Validation, Qualification, and Performance
Verification for Total Organic Carbon (TOC)
Analyzers / Instrument Performance Verification ?
Micro Pipettes / Instrument Qualification and
Performance Verification for Automated Liquid
Handling Systems / Performance Qualification and
Verification in Powder X-ray Diffraction.
Subjects Drugs--Analysis--Methodology--Evaluation.
Laboratories--Equipment and supplies--Evaluation.
Laboratories--Instruments--Evaluation.
Chemistry, Pharmaceutical--instrumentation.
Chemistry, Pharmaceutical--methods.
Clinical Laboratory Techniques--standards.
Technology, Pharmaceutical--methods.
Notes Complement to: Method validation and instrument
performance verification / edited by Chung Chow
Chan ... [et al.]. c2004.
Includes bibliographical references and index.

Principles and practice of analytical techniques in geosciences

LCCN 2015458264
Type of material Book
Main title Principles and practice of analytical techniques in
geosciences / edited by Kliti Grice, Curtin University,
Perth, Australia.
Published/Produced Cambridge: Royal Society of Chemistry, [2015]
©2015
Description xviii, 393 pages: illustrations (some color); 24 cm.
ISBN 9781849736497 (print)
1849736499 (print)
LC classification QE516.3 .P75 2015
Related names Grice, Kliti, editor.
Contents Nanoscale secondary ion mass spectrometry
(NanoSIMS) as an analytical tool in the geosciences /
Matt R. Kilburn and David Wacey -- Clumped isotope
geochemistry / Allan R. Chivas and Florian W. Dux --
Application of radiogenic isotopes in geosciences:
overview and perspectives / Svetlana Tessalina, Fred
Jourdan, Laurie Nunes, Allen Kennedy, Steven
Denyszyn, Igor Puchtel, Mathieu Touboul, Robert
Creaser, Maud Boyet, Elena Belousova and Anne
Trinquier -- Advances in fluorescence spectroscopy for
petroleum geosciences / Keyu Liu, Neil Sherwood and
Mengjun Zhao -- Time-of-flight secondary ion mass
spectrometry (TOF-SIMS): principles and practice in
the biogeosciences / Volker Thiel and Peter Sjövall --
Development and use of catalytic hydropyrolysis
(HyPy) as an analytical tool for organic geochemical
applications / Will Meredith, Colin E. Snape and
Gordon D. Love -- Microscale sealed vessel pyrolysis /
Brian Horsfield, Franz Leistner and Keith Hall --
High-precision MC-ICP-MS measurements of đ¹¹B:
matrix effects in direct injection and spray chamber
sample introduction systems / Michael Holcomb, Kai
Rankenburg and Malcolm McCulloch -- Radioactive
carbon in environmental science / John Dodson --
Development and initial biogeochemical applications
of compound-specific sulfur isotope analysis / P.F.

Greenwood, A. Amrani, A. Sessions, M.R. Raven, A.

Holman, G. Dror, K. Grice, M.T. McCulloch and J.F.
Adkins -- Applications of liquid chromotography-
isotope ratio mass spectrometry in geochemistry and
archaeological science / Alison J. Blyth and Colin I.
Smith -- Advances in comprehensive two-dimensional
gas chromatography (GCxGC) / Christiane Eiserbeck,
Robert K. Nelson, Christopher M. Reddy and Kliti
Grice.
Subjects Analytical geochemistry.
Analytical geochemistry.
Notes Includes bibliographical references and index.
Series RSC detection science series, 2052-3068; 4
RSC detection science series; 4. 2052-3068

Pyrolysis-GC/MS data book of synthetic polymers: pyrograms,

thermograms and MS of pyrolyzates
LCCN 2012419730
Type of material Book
Personal name Tsuge, Shin.
Main title Pyrolysis-GC/MS data book of synthetic polymers:
pyrograms, thermograms and MS of pyrolyzates /
Tsuge Shin, Ohtani Hajime, Watanabe Chuichi.
Edition 1st ed.
Published/Created Amsterdam; Boston: Elsevier, c2011.
Description xiv, 390 p.: ill.; 25 cm.
Links Publisher description http://www.loc.gov/catdir/
enhancements/fy1606/2012419730-d.html
ISBN 9780444538925
0444538925
LC classification TP156.P9 .T78 2011
Related names Ohtani, Hajima.
Watanabe, Chuichi.
Subjects Pyrolysis.
Mass spectrometry.
Gas chromatography.
Polymers--Analysis.
Notes Includes bibliographical references and index.

Quartz: deposits, mineralogy and analytics

LCCN 2012933435
Type of material Book
Main title Quartz: deposits, mineralogy and analytics / Jens
Götze, Robert Möckel, editors.
Published/Created Berlin; New York: Springer, c2012.
Description xv, 360 p.: ill. (some col.), maps (some col.); 24 cm.
ISBN 9783642221606 (alk. paper)
3642221602 (alk. paper)
9783642221613 (electronic)
LC classification QE391.Q2 Q36 2012
Related names Götze, Jens.
Möckel, Robert.
Contents Classification, mineralogy and industrial potential of
SiO₂ minerals and rocks / Jens Götze -- Assessment of
high purity quartz resources / Reiner Haus, Sebastian
Prinz and Christoph Priess -- Quality requirements of
quartz sand in the building industry / Hartmut B.
Walther -- Petrological and chemical characterisation
of high-purity quartz deposits with examples from
Norway / Axel Müller, Jan Egil Wanvik and Peter M.
Ihlen -- Evaluation of the potential of the pegmatitic
quartz veins of the Sierra de Comechigones
(Argentina) as a source of high purity quartz by a
combination of LA-ICP-MS, ICP,
cathodoluminescence, gas chromatography, fluid
inclusion analysis, Raman and FTIR spectroscopy /
Giulio Morteani ... [et al.] -- Brazilian quartz deposits
with special emphasis on gemstone quartz and its color
treatment / Ricardo Scholz ... [et al.] -- First-principles
calculations of the Eʹ₁ center in quartz: structural
models, ²₉Si hyperfine parameters and association with
Al impurity / Zucheng Li and Yuanming Pan --
Gamma-irradiation dependency of EPR and TL-
spectra of quartz / Michael Plötze, Dieter Wolf and
Matthias R. Krbetschek -- Analysis of low element
concentrations in quartz by electron microprobe /
Andreas Kronz, Alfons M. Van den Kerkhof and Axel
Müller -- In situ analysis of trace elements in quartz

using laser ablation inductively coupled plasma mass

spectrometry / Belinda Flem and Axel Müller --
Cathodoluminescence microanalysis of the defect
microstructures of bulk and nanoscale ultrapure silicon
dioxide polymorphs for device applications / Marion
A. Stevens-Kalceff -- Trace element characteristics,
luminescence properties and real structure of quartz /
Thomas Götte and Karl Ramseyer -- Mineralogy,
geochemistry and cathodoluminescence of authigenic
quartz from different sedimentary rocks / Jens Götze --
Cathodoluminescent textures and trace elements in
hydrothermal quartz / Brian Rusk -- Quartz
regeneration and its use as a repository of genetic
information / Ulf Kempe ... [et al.].
Subjects Quartz.
Notes Includes bibliographical references and index.
Series Springer geology
Springer geology.

Quick guide to organic acid interpretation

LCCN 2011035262
Type of material Book
Personal name Jones, Patricia M., 1954-
Main title Quick guide to organic acid interpretation / Patricia M.
Jones, Dinesh Rakheja.
Published/Created Washington D.C.: AACC Press, c2011.
Description vi, 147 p.: ill.; 16 cm.
ISBN 9781594251269 (alk. paper)
1594251266 (alk. paper)
LC classification RC632.A45 J66 2011
Related names Rakheja, Dinesh, 1969-
American Association for Clinical Chemistry.
Subjects Amino acids--Metabolism--Disorders.
Amino Acid Metabolism, Inborn Errors--diagnosis--
Handbooks.
Amino Acids--analysis--Handbooks.
Gas Chromatography-Mass Spectrometry--methods--
Handbooks.
Notes Includes bibliographical references and index.

Temperature-programmed gas chromatography

LCCN 2011499093
Type of material Book
Personal name Blumberg, Leonid M.
Main title Temperature-programmed gas chromatography /
Leonid M. Blumberg.
Published/Created Weinheim: Wiley-VCH, c2010.
Description xix, 340 p.: ill.; 25 cm.
Links http://d-nb.info/1000973999/04 Inhaltsverzeichnis
http://deposit.d-nb.de/cgi-bin/dokserv?id=3443178&
prov=M&dok_var=1&dok_ext=htm Inhaltstext
ISBN 9783527326426 (hbk.: alk. paper)
3527326421 (hbk.: alk. paper)
LC classification QD79.C45 B585 2010
Subjects Gas chromatography.
Gaschromatographie
Temperaturabhängigkeit
Notes Includes bibliographical references and index.

Understanding pottery function

LCCN 2012939621
Type of material Book
Personal name Skibo, James M.
Main title Understanding pottery function / James M. Skibo.
Published/Created New York, NY: Springer, [2013]
Description ix, 192 p.: ill. (some col.), maps.; 24 cm.
Links Contributor biographical information http://www.loc.
gov/catdir/enhancements/fy1306/2012939621-b.html
Publisher description http://www.loc.gov/catdir/
enhancements/fy1306/2012939621-d.html
Table of contents only http://www.loc.gov/catdir/
enhancements/fy1403/2012939621-t.html
ISBN 9781461441984
1461441986
LC classification GN799.P6 S585 2013
Summary "The 1992 publication of Pottery Function applied
ethnoarchaeological data collected among the Kalinga
and experiments to set forth the principles for the
creation of pottery use-alteration traces (residue,

carbonization, and abrasion). Analogous to lithic use-

wear analysis, this study developed the method and
theory making the connections between pottery use
traces and function. At the 20th anniversary of the
book, it is time to assess what has been done and
learned. One of the concerns of those working in
pottery analysis is that they are unsure how to "do"
use-alteration analysis on their collection. Another
common concern is understanding intended pottery
function--the connections between technical choices
and function. This book is designed to answer these
questions using case studies from the author and many
others who are applying use-alteration analysis to infer
actual pottery function. The focus of Understanding
Pottery Function is on how practicing archaeologists
can infer function from their ceramic collection."--
Publisher's website.
Contents Understanding Pottery Function. The Joys of Pottery;
Actual Versus Intended Pottery Function; An
Approach to Pottery Function; Performance-Based
Life History Approach; Life-History/Behavioral
Chain; Activities and Interactions; Technical Choices
and Compromises; Performances Characteristics; The
Approach to the Writing in This Book; A Story of
Pottery and People: Origins of Pottery Making on
Grand Island; Review of the Book's Contents;
References. -- Intended Function: Inferring
Manufacturing Performance; Understanding Technical
Choices and Performance; Morphology; Paste
Composition: Temper (Type, Size, Shape, Quantity)
and Clay (Type, Chemistry); Firing Temperature;
Surface Treatments; Inferring Intended Function:
Primary and Secondary Performance Characteristics,
and Derivative Choices; Is It Just About Techno-
function?; From Sherds to Intended Function;
Reference. -- Sooting and Carbonization. Kalinga
Vessels and Internal and External Carbonization; The
Kalinga; The Kalinga Ethnoarchaeological Project;

Kalinga Internal and External Carbonization Patterns;

Principles for External Sooting; What Is Soot; Soot
Patches; Temperature of Fire; Distance from Fire;
Mode of Cooking; Case Study: Late Archaic Pottery
and Exterior Sooting; Principles for Internal
Carbonization; Mode of Cooking: Wet/Dry; Other
Factors; Case Study: Origins of Pottery on the
Colorado Plateau; Recording External and Internal
Carbonization on Prehistoric Collections; Start with
Whole Vessels; Recording Use Carbonization and
Sooting Patterns on Whole Vessels; Recording Use-
Alteration Traces on Sherds; Trickery; Inferences;
References. -- Attrition. Principles of Ceramic
Attrition; Use-Attrition: Abrasive Processes; Use
Attrition: Nonabrasive Processes; Use-Attrition Terms;
Case Study: Kalinga; Kalinga Pottery Surfaces and
Other Relevant Technical Properties; Use Attrition on
Kalinga Pots; Summary; Case Study: Griffiths and
Bray; Case Study: Hardin and Mills; Case Study:
Sherds as Tools; Case Study: Alcohol Fermentation;
Recording Attritional Traces on Prehistoric Pottery;
References. -- Residue; Co-authored by Mary
Malainey Kalinga Study; British Invasion; Approaches
to Lipid Residue Analysis; Sample Selection; Sample
Processing Techniques; Gas Chromatography for the
Analysis of Archaeological Lipid Residues; The
Problem of Diagenesis; Compound-Specific Stable
Isotope Analysis; Infrared and Raman Spectroscopy;
Case Study: Origins of Pottery in the Upper Great
Lakes; Case Study: Late Prehistoric Pottery Function
from Western Canada; Case Study: Finding Evidence
of Maize Processing in North America; Case Study:
Origins of Pottery in Southeastern Arizona; Final
Recommendations; A Concluding Comment;
References.
Subjects Pottery, Prehistoric--Analysis.
Ethnoarchaeology.
Notes Includes bibliographical references and index.

EBSCO Publishing : eBook Collection (EBSCOhost) - printed on 10/5/2018 10:09 AM via UNIVERSIDAD DE
ANTIOQUIA
AN: 1540094 ; Warren, Valerie.; Gas Chromatography : Analysis, Methods and Practices
Account: s1175444
190 Bibliography

Series Manuals in archaeological method, Theory and

technique, 1571-5752
Manuals in archaeological method, theory, and
technique.

SAFETY ANALYSIS OF SOY SAUCE SQUEEZING

RESIDUE AND FISH MEAL STORAGE BY THERMAL
ANALYSIS AND GAS CHROMATOGRAPHY*

Naoharu Murasawa†
Faculty of Risk and Crisis Management,
Chiba Institute of Science, Choshi, Japan

An increased demand for recycling has prompted the food industry to

become more efficient in its handling of waste. However, there are some cases
in which food wastes or products manufactured by recycling have
spontaneously ignited during transport or storage, or else have depleted
oxygen in their storage area, causing the deaths of workers. This study
investigated heat generation and oxygen levels during the storage of soy sauce
squeezing residue and fish meal, by-products of soy sauce and fish production
and processing, respectively, by thermal analysis and gas chromatography.

*
The full version of this chapter can be found in Food Waste: Practices, Management and
Challenges, edited by Garrett Leonard Riley, published by Nova Science Publishers, Inc, New
York, 2016.
† Corresponding author: Naoharu Murasawa. Faculty of Risk and Crisis Management, Chiba
Institute of Science, 3 Shiomi-Cho, Choshi, 288-0025, Japan. E-mail: [email protected].
jp.

Results suggest that oxygen deficiency may occur in a well-sealed storage

facility due to fermentation. However, if oxygen is continuously cycled and
the facility stores large deposits in an insulated environment, fermentation can
cause the temperature to increase, leading to the oxidation of fatty acid esters
and, eventually, fire.

APPLICATION OF PYROLYSIS -
GAS CHROMATOGRAPHY/MASS SPECTROMETRY IN
FAILURE ANALYSIS IN THE AUTOMOTIVE INDUSTRY*

Peter Kusch†
Hochschule Bonn-Rhein-Sieg, University of Applied Sciences,
Department of Applied Natural Sciences, Rheinbach, Germany

The increasing use of polymeric materials, rubbers and chemical fluids,

like mineral oils or brake fluids in the automotive industry, demands analytical
techniques for the identification of high molecular weight organic compounds.
For failure analysis in motor vehicles there is often a lack of information about
the component itself, such as chemical composition, temperature resistance,
possible contaminants or mechanical properties. The damage range is usually
limited and not always homogeneous. Very often only small amounts of
samples are available, which may be important for recognizing the cause of
damage.
Traditional analytical techniques used for characterization of high
molecular weight organic compounds, such as thermal analysis (TA) and
Fourier transform infrared spectroscopy (FTIR), are limited or not sufficiently
sensitive to demonstrate the change of the structure and the resulting
dysfunction of used materials. Analytical pyrolysis technique hyphenated to
gas chromatography/mass spectrometry (Py-GC/MS) has extended the range
of possible tools for characterization of synthetic polymers/copolymers or

*
The full version of this chapter can be found in Automobiles and the Automotive Industry:
Emerging Technologies, Environmental Impact and Safety Analysis, edited by Aaron T.
Evans, published by Nova Science Publishers, Inc, New York, 2015.
† Corresponding author. E-mail address: [email protected] (Dr. Peter Kusch).

rubbers. Under controlled conditions at elevated temperature (500 – 1400 °C)

in the presence of an inert gas, reproducible decomposition products
characteristic for the original sample are formed. Pyrolysis methods eliminate
the need for pre-treatment by performing analyses directly on the solid or
liquid sample.
This book chapter describes application examples of gas chromatography/
mass spectrometry and pyrolysis – gas chromatography/mass spectrometry in
failure analysis for the identification of chemical materials like mineral oils
and nitrile rubber gaskets. Furthermore, failure cases demanding identification
of polymers/copolymers in fouling on the compressor wall of a car air
conditioner and identification of fouling on the surface of a bearing race from
the automotive industry are demonstrated. The obtained analytical results were
then used for troubleshooting and remedial action of the technological process.

MULTI RESIDUE METHOD FOR DETERMINATION

OF 55 PESTICIDE RESIDUES IN POMEGRANATE SAMPLES
BY GAS CHROMATOGRAPHY COUPLED TO TRIPLE
QUADRUPOLE TANDEM MASS SPECTROMETRY USING
QUECHERS EXTRACTION METHOD*

Dinesh C. Bilehal1,†, M. B. Chetti2, G. T. Deepa2,

Mahadev Khetagoudar2 and P. T. Goroji2
1
Reva Institute of Technology and Management, Kattigenahalli,
Yelahanka, Bengaluru, Karnataka, India
2
University of Agricultural Sciences, Dharwad, Karnataka, India

A multi-residue method has been developed and validated for the

simultaneous determination and quantification of around 55 multiclass
pesticides in pomegranate samples by GC-MS/MS with a triple quadrupole
analyzer. Compounds have been selected from different chemical families

*
The full version of this chapter can be found in Advances in Chemistry Research. Volume 24,
edited by James C. Taylor, published by Nova Science Publishers, Inc, New York, 2015.
† Corresponding Author: [email protected]

including organochlorines, organophosphorus, carbamates, pyrethroids,

triazines, triazoles and pyrazoles, etc. Samples were extracted by using
QuEChERS solvent extraction method with ethyl acetate. An additional clean
up step by using Primary secondary amine (PSA) and Graphitized carbon
black (GCB). Determination was performed by using GC-MS/MS in electron
ionization mode acquiring two MS/MS transitions for each analyte. The
intensity ratio between quantitation transition (Q) and confirmation transition
(q) was used as confirmatory parameter (Q/q ratio). Accuracy and precision
were evaluated by means of recovery experiments in pomegranate samples
spiked at two different concentration levels i.e., (0.02 and 0.05 mg/kg).
Recoveries in most cases obtained between 65% and 100%. Matrix effects
were tested by comparison of reference standards in pure solvent with matrix-
matched standards.

HYDRODISTILLATION: HEADSPACE SOLVENT

MICROEXTRACTION AND CHEMICAL
COMPOSITION OF KOREAN GINGER BY GAS
CHROMATOGRAPHY AND MASS SPECTROMETRY*

Dinesh C. Bilehal1,† and Yong H. Kim2,‡

1
Department of Chemistry, Reva Institute of Technology and Management,
Yalhanka, Bangalore India
2
Department of Biomedical Laboratory Science, Inje University, Kimhae,
Gyeongnam, South Korea

In this study, a gas chromatography–mass spectrometry method in EI

mode is developed for the analysis of dried Korean ginger. Hydro distillation–
headspace solvent microextraction with polar and non-polar solvents is used.
Forty-nine compounds are separated and identified. Some of the ginger

*
The full version of this chapter can be found in Ginger: Antioxidant Properties, Functions and
Medicinal Benefits, edited by Janine L. Perry, published by Nova Science Publishers, Inc,
New York, 2015.
† E-mail: [email protected].
‡ E-mail: [email protected].

compounds partially or completely were thermally decomposed. Some of these

decomposition products likely produced when ginger is used in cooking at
high temperatures and subsequently eaten. The major compounds in the
rhizome identified are α-zingiberene, curcumene, camphene, β-phellandrene,
(E)-citral, α-farnesene, β-bisabolene, β-sesquiphellandrene, zingerone, and [6]-
gingerol. This method will be useful for rapid screening purpose of plant
samples for finding of high quality ginger under the plant breeding program,
genotypes assessment, and also export quality of ginger species.

SORPTION IN LIQUID CRYSTALLINE

POLY(PROPYLENEIMINE) DENDRIMERS
BY INVERSE GAS CHROMATOGRAPHY*

Svetlana V. Blokhina†, Marina V. Ol’khovich and

Angelica V. Sharapova
Institute of Solution Chemistry, Russian Academy of Sciences,
Ivanovo, Russia

Thermodynamic characteristics of infinitely diluted solutions of n-alkanes

and n-alcohols in the columnar and isotropic phases of poly(propyleneimine)
dendrimers, generations 1–3, have been investigated by inverse gas
chromatography. Effects of the dendrimer structure, the chemical nature and
molecular size of the non-mesogenes on the ability to get dissolved in the
liquid crystalline phases are discussed. The compatibility of the low-molecular
compounds with the anisotropic phases is stated to increase with number of
generation. A binary system composed of the liquid crystalline
poly(propyleneimine) dendrimer and nematic p-n-pentyloxy-p’-cyanobyphenyl
has been studied by thermomicroscopy, scanning calorimetry, and inverse gas
chromatography. In this system, there is the columnar phase being stable
within broad ranges of temperature and component ratio. Dependences of the

*
The full version of this chapter can be found in Dendrimers: Synthesis, Applications and Role
in Nanotechnology, edited by Heather B. Harris and Brian L. Turner, published by Nova
Science Publishers, Inc, New York, 2013.
† E-mail: [email protected]

retention volumes of various solutes, namely, hydrocarbons, alcohols, and

amines, on composition of the sorbents are revealed to exhibit the maximum.
Thermodynamic functions of sorption of n-alkanes and n-alcohols on the
binary sorbents composed of the said liquid crystals have been calculated
specifically. Thermodynamic solute-sorbent compatibility characterized by the
activity coefficients of the solutes is dependent on the sorbent composition;
namely, it is controlled by counterbalancing of the enthalpy or entropy factors.
The non-additive mode of the solute-sorbent interaction is explained by arising
of the microdomain nematic structure enclosed in the columnar structure of
the dendrimers.

131, 138, 142, 143, 160, 164, 170, 172,

A 186, 189, 193, 195
carboxyhemoglobin (CO-Hb), 111, 112,
additional procedure, 108
116, 117
alkaloid, 2, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13,
chromatography, vii, viii, 1, 2, 6, 7, 8, 10,
14, 16, 18, 20, 25, 26, 27, 28, 29, 30, 33,
11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 25,
34, 36, 41, 42
26, 27, 28, 29, 30, 31, 32, 33, 35, 36, 37,
Alkaloids, vii, 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11,
38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48,
20, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32,
49, 51, 54, 58, 61, 62, 63, 64, 65, 66, 69,
33, 34, 35, 36, 37, 38, 40, 41, 42, 43, 44,
70, 71, 72, 74, 75, 77, 78, 79, 80, 81, 82,
133, 172, 177
83, 84, 85, 86, 87, 88, 89, 90, 91, 92, 93,
94, 95, 96, 97, 98, 99, 100, 101, 102,
B 103, 106, 111, 113, 116, 118, 119, 122,
123, 124, 125, 126, 129, 130, 135, 136,
biological sample, viii, 2, 7, 9, 10, 36, 38, 137, 138, 139, 141, 142, 143, 144, 145,
41, 106, 116, 124, 158, 160 146, 147, 149, 150, 151, 152, 153, 154,
botany, 163, 176 155, 156, 158, 159, 160, 162, 164, 165,
butane, 108, 109, 113, 119 166, 167, 170, 172, 174, 177, 180, 181,
182, 184, 185, 186, 187, 189, 191, 192,
193, 194, 195
C
cryogenic oven trapping, 111
carbon, viii, 7, 18, 46, 61, 62, 69, 70, 76, 84,
90, 93, 102, 106, 107, 109, 111, 112, D
114, 116, 117, 118, 122, 131, 138, 142,
143, 160, 164, 170, 172, 186, 189, 193, derivatization, 7, 10, 20, 145, 158
195 detection, viii, 6, 8, 9, 10, 11, 12, 14, 16, 18,
carbon monoxide (CO), viii, 7, 18, 46, 61, 25, 30, 32, 36, 37, 38, 39, 42, 48, 69, 71,
62, 69, 70, 76, 84, 90, 93, 102, 106, 107, 89, 103, 111, 112, 113, 117, 118, 128,
109, 111, 112, 114, 116, 117, 118, 122, 133, 141, 153, 158, 172, 174, 182, 184

diffusion, vii, 45, 46, 53, 54, 55, 56, 61, 62, gas chromatography-mass spectrometry
63 (GC/MS), viii, 18, 20, 25, 31, 38, 39, 40,
diffusion coefficients, vii, 45, 46, 53, 54, 55, 41, 42, 43, 69, 70, 71, 75, 77, 78, 80, 81,
56, 61, 62, 63 82, 83, 84, 85, 86, 87, 88, 89, 90, 91, 92,
93, 94, 95, 96, 97, 98, 99, 100, 101, 102,
103, 106, 111, 113, 118, 119, 123, 125,
E 126, 130, 138, 139, 145, 149, 152, 154,
156, 158, 160, 162, 177, 184, 186, 192
ethanol, vii, 7, 10, 11, 12, 13, 14, 15, 16, 17,
18, 19, 39, 45, 47, 53, 54, 55, 57, 58, 59,
106, 107, 109, 111, 114 H
evaporation, vii, 45, 46, 47, 51, 53, 54, 55,
57, 58, 59, 60, 62, 64, 66, 108 handling, 107, 108, 114, 116, 148, 182, 191
extraction, viii, 7, 10, 30, 32, 38, 39, 43, 69, head-space (HS), viii, 69, 70, 71, 74, 75, 76,
70, 71, 73, 74, 75, 76, 89, 100, 131, 141, 79, 89, 90, 91, 93, 94, 95, 96, 99, 102,
147, 148, 156, 164, 166, 177, 193, 194 106, 111, 113, 119
head-space (HS) method, viii, 106
head-space solid phase microextraction
F (HS-SPME), viii, 69, 70, 71, 74, 102,
111
fire related cases, 113
Helium, 8, 70, 77, 112, 117
flame ionization detector, 8, 9, 48, 164
hydrocarbons, 63, 101, 106, 107, 109, 113,
forensic medicine, vii, ix, 105, 106, 115
118, 145, 157, 196
fragmentation pathways, 20
hydrogen sulfide, 106, 107, 109
fragmentogram, 2, 20

G I

identification, 2, 8, 9, 27, 31, 33, 35, 36, 38,

gas chromatography (GC), vii, viii, 1, 2, 6,
41, 70, 78, 80, 81, 84, 89, 90, 91, 93, 96,
7, 8, 10, 11, 12, 13, 14, 15, 16, 17, 18,
99, 100, 101, 103, 107, 112, 113, 130,
19, 20, 25, 26, 27, 28, 29, 30, 31, 32, 33,
149, 156, 164, 167, 169, 172, 177, 179,
35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45,
182, 192, 193
46, 47, 48, 49, 51, 54, 58, 61, 62, 63, 64,
inert gas, 109, 112, 193
65, 66, 69, 70, 71, 72, 74, 75, 77, 78, 79,
intratracheal and stomach gas, 112
80, 81, 82, 83, 84, 85, 86, 87, 88, 89, 90,
intratracheal gas or contents, 113
91, 92, 93, 94, 95, 96, 97, 98, 99, 100,
ionization, 8, 9, 48, 164
101, 102, 103, 106, 111, 113, 116, 118,
119, 122, 123, 124, 125, 126, 129, 130,
135, 136, 137, 138, 139, 141, 142, 143, K
144, 145, 146, 147, 149, 150, 151, 152,
153, 154, 155, 156, 158, 159, 160, 162, Kerosene, 113, 118
164, 165, 166, 167, 170, 172, 174, 177,
180, 181, 182, 184, 185, 186, 187, 189,
191, 192, 193, 194, 195

L R

Life sciences, 167, 173, 176 rate coefficients, 46, 55, 62, 63
liquid pollutants, vii, 45, 46, 47, 54, 59, 63

S
M
sample collection and handling, 107
mass fragmentogram, 2, 20 sampling, vii, viii, ix, 48, 49, 50, 51, 60, 63,
mass spectrometry, viii, 18, 20, 25, 31, 38, 69, 70, 71, 73, 74, 84, 105, 106, 107,
39, 40, 41, 42, 43, 69, 70, 71, 75, 77, 78, 112, 113, 114, 117, 147, 177
80, 81, 82, 83, 84, 85, 86, 87, 88, 89, 90, sampling procedure, vii, ix, 48, 106
91, 92, 93, 94, 95, 96, 97, 98, 99, 100, separation, 2, 6, 7, 8, 10, 11, 40, 46, 61, 124
101, 102, 103, 106, 111, 113, 118, 119, simple asphyxic agent, 112
123, 125, 126, 130, 138, 139, 145, 149, solid phase, viii, 10, 69, 70, 71, 74, 102,
152, 154, 156, 158, 160, 162, 177, 184, 111, 131, 156, 177
186, 192 solid phase extraction, 10, 131, 156, 177
methanol, vii, 7, 10, 11, 12, 13, 14, 15, 16, source, 3, 9, 30, 41, 77, 113, 126, 163, 185
17, 18, 19, 45, 47, 53, 54, 55, 57, 58, 59, stationary phase, 7, 11, 12, 14, 16, 18, 46,
64, 109, 113, 119 47, 74, 77, 146
MS detector, 9 stomach, 112
storage, 79, 81, 88, 108, 114, 116, 124, 177,
191
N surfactants, vii, 45, 46, 47, 61, 62, 64, 66,
72, 78
nitrogen-phosphorus detector, 8, 9, 38

O T

toxicity, 3, 4, 5, 10, 27, 28, 29, 32, 84, 119

odor, 107, 141
toxicological analysis, 38, 106, 107, 112,
117, 139
P

phosphorus, 8, 9, 38 V
poisoning, vii, 2, 3, 4, 6, 10, 25, 26, 27, 28,
vitreous humour, 110, 111
29, 33, 38, 39, 44, 106, 107, 108, 112,
volatile and gaseous substances, vii, ix, 106,
114, 118, 119
107, 108, 109, 111, 114
polymers, viii, 69, 70, 71, 78, 81, 84, 88, 89,
volatile organic compounds, vii, viii, 70, 71,
90, 93, 100, 102, 136, 148, 184, 192, 193
78, 80, 81, 83, 84, 88, 89, 92, 96, 99,
postmortem ethanol production, 111
101, 102, 103, 158, 172
post-mortem lividity, 107
proper sample collection, 107, 108
pulse-heating, 111, 116

volatile organic compounds (VOCs), vii,

viii, 70, 71, 78, 80, 81, 83, 84, 88, 89, 92,
X
96, 99, 101, 102, 103, 158, 172
xylene, 80, 92, 109, 113, 119
volatile substances, 25, 106, 108, 110, 115,
116, 118

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BIOCHEMISTRY RESEARCH TRENDS

NOTICE TO THE READER

Library of Congress Cataloging-in-Publication Data

ISBN:  H%RRN

Published by Nova Science Publishers, Inc. † New York

Chapter 4 Sampling of the Postmortem Specimen

AN ANALYSIS OF TOXIC ALKALOIDS OF

Ana Claudia Fernandes Amaral1,*,

Keywords: alkaloid, gas chromatography, poisoning, mass fragmentogram,

SOURCE OF TOXIC ALKALOIDS

mode of action of colchicine relies on its inhibitory effect over cellular

SEPARATION, DETECTION AND METHODS

53], herbal medicines and pharmaceutical preparations [54-58], foods [59-63],

resulting gas chromatograms, such as lipids and cholesterol esters from

ANALYSIS OF BIOLOGICAL SAMPLES

ADVANTAGES AND DISADVANTAGES OF THE GAS

Analyses by gas chromatography/mass spectrometry in full scan or

Figure 1. Fragmentogram of diterpenoid alkaloid.

Figure 2. Fragmentograms of indole alkaloids.

Figure 3. Fragmentograms of pyrrolizidine alkaloids.

Aconitine must be extracted and derivatized before analysis by GC-MS.

[20] Pomilio, A.B.; Vitale, A.A.; Ciprian-Ollivier, J.; Cetkovich-Bakmas,

pyrrolizidine alkaloids: a whole genome transcriptome analysis. Toxicol.

Narcissus broussonetti: mass spectral studies. J. Pharm. Biomed. Anal.

[72] Ogalde, J. P., Arriaza, B.T., Soto, E.C., (2009). Identification of

[145] McKenna, D.J., Towers, G.H.N., Abbott, F., (1984). Monoamine

[157] Gallagher, C.A., Hough, L.B., Keefner, S.M., Seyed-Mozaffari, A.,

[178] Comparini, B., Centini, F., Pariali, A., (1983). Simultaneous

Reviewed by Fiona Pellew, Portuguese - English translator.

THE INFLUENCE OF SURFACTANT

H. H. Mohammad1,*, Rashid Atta Khan1 and

published literature values, while the diffusion coefficients with compare

Keywords: evaporation, diffusion coefficients, rate coefficients, surfactants,

The solutes used as evaporating liquids (stationary phase) were methanol,

supplied by Malaysian Oxygen Berhad (MOX). Hydrogen and compressed air

Figure 1 shows the experimental setup of the reverse-flow gas

Figure1. The apparatus of the Reverse-Flow Gas Chromatography system.

The reversal of the flow creates extra chromatography peaks on the

 h = height of the peak = concentration of vapors at x = l’ junction

Mathematical treatment of the RF-GC system for study of liquid-gas

shown in figure 4. A steady-state situation is achieved after a period of time

By using the above approximation, one obtains (Karaiskakis & Katsanos,

A plot of ln (h∞- h) vs t0 is expected to be linear, at long enough times, for

4. RESULT AND DISCUSSION

2 51.15 ± 0.29a 52.3 204.68 ± 0.03a 205.41 223.53 0.4* 8.4#

3 7.38 ± 0.25a 93.1 212.57 ± 0.02a 205.41 223.53 3.4* 4.9#

4 7.10 ± 0.07a 93.4 209.75 ± 0.02a 205.41 223.53 2.1* 6.2#

2 106.33 ± 0.25a 45.50 155.22 ± 0.03a 156.30 158.26 0.8* 1.9#

Figure 8. Plots of the % reduction of evaporation of methanol (rectangle) and ethanol

2013). Drastic retardation of the evaporation is due to the presence of adsorbed

Figure 9. Movement of the liquid molecules through the surfactant monolayer(s).

aL free surface area of the liquid

2 power of two (squared)

Gavril, D., Atta, K. R. & Karaiskakis, G. (2006). Study of the Evaporation of

Karaiskakis, G., Niotis, A. & Katsanos, N. A. (1984). Characterization of

Methodologies. Studia Universitatis Babes-Bolyai Chemia, 56(2), 149-

Mohammad Hafiz Bin Hamzah (H.H. Mohammad) was born on 15

Penyelidikan), IPPP, Universiti Malaya (UM), Kuala Lumpur Malaysia. He

2. Rashid Atta Khan

Khalisanni Khalid was born in Ipoh in 1985. He pursued his studies in

THE APPLICATION OF HEADSPACE:

spectrometry (GC/MS) and successfully applied to a wide variety of

Keywords: HS-SPME, GC/MS, polymers, volatile organic compounds

In SPME, a small amount of the extracting phase associated with a solid

Mi,SPME~Ki,SPME VSPMECi (1)

where Ki,SPME is an aggregate solute distribution constant between the SPME

volumes, would imply correspondingly smaller minimum sample volumes

Table 1. Summary of commercially available SPME fibres [15, 19]

Fibre coating Film Polarity Coating Maximum Technique Compounds

Figure 2. Schematic illustration of a SPME device. A) SPME device with sampling

Figure 3. Steps of typical SPME extraction and thermal desorption in GC injector.

is directly related to the concentration of the analyte in the sample according to

n = mass of analyte absorbed by coating

n = KfsVfC0Vs/KfsVf + KhsVh + Vs (3)

n = mass of analyte absorbed by coating

Samples (A and B) of commercially available expanded polystyrene

ISBN: H%RRN