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GC-MS

Gas Chromatography-Mass Spectrometry (GC-MS) is an advanced analytical technique that combines gas chromatography's separation capabilities with mass spectrometry's structural analysis. It is used for identifying and characterizing organic compounds, particularly in small quantities, and involves various components such as injectors, ovens, and detectors. Applications of GC-MS include impurity profiling in pharmaceuticals, drug testing, and pesticide residue analysis.

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6 views5 pages

GC-MS

Gas Chromatography-Mass Spectrometry (GC-MS) is an advanced analytical technique that combines gas chromatography's separation capabilities with mass spectrometry's structural analysis. It is used for identifying and characterizing organic compounds, particularly in small quantities, and involves various components such as injectors, ovens, and detectors. Applications of GC-MS include impurity profiling in pharmaceuticals, drug testing, and pesticide residue analysis.

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qasimboy669
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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2022

Gas Chromatography-
Mass Spectrometry
Pharmaceutical Chemistry-III (Pharm.
Analysis)
Muhammad Wajid
Assistant Professor
Gulab Devi Institute of Pharmacy, Gulab Devi Educational Complex, Lahore

[Type text] Page 0


Gas Chromatography-Mass Spectrometry
GC-MS is an advance analytical instrumental technique that combines the physical separation
capability of GC with the mass analyzing capability of MS.

Gas chromatography is a technique capable of separating, detecting and partially characterizing


the organic compounds particularly when present in small quantity.

Mass spectroscopy provides some definite structural information. The separation and
identification of the components of complex natural and synthetic mixture are achieved more
quickly than any other technique with fewer samples.

Principle of GC-MS:

The sample solution is injected into the GC inlet where it is vaporized and swept onto a
chromatographic column by the carrier gas (usually helium).

The sample flows through the column and the compounds comprising the mixture of interest are
separated by virtue of their relative interaction with the coating of the column (stationary phase)
and the carrier gas (mobile phase).

The latter part of the column passes through a heated transfer line and ends at the entrance to ion
source where compounds eluting from the column are converted to ions.

SAMPLES:

Nature: Samples should be organics must be volatile or semi-volatile thermally stable.

State: Organic compounds must be in solution for injection into the gas chromatograph. The
solvent must be volatile and organic (for example, hexane or dichloromethane).

Amount: Depending on the ionization method, analytical sensitivities of 1 to 100 µg per


component are routine.

Preparation: Sample preparation can range from simply dissolving some of the sample in a
suitable solvent to extensive. Clean up procedures using various forms of liquid chromatography.

Muhammad Wajid, Assistant Professor, Gulab Devi Institute of Pharmacy, GDEC, Lahore Page 1
INSTRUMENTATION:

1. Pneumatic controls 2. Injector 3. Oven 4. Column 5. Interface 6. Ion Source 7. Mass


Analyser 8. Detector.
PNEUMATIC CONTROLS:

The gas supply is regulated to correct pressure (or flow) and then fed to the required part of the
instrument. Modern GC instruments have Electronic Pneumatic pressure controllers, older
instruments may have manual pressure control via regulators.

INJECTORS:

Septum type injectors are the most common. These are composed of a glass tube where
vaporization of the sample takes place. The sample is introduced into the injector through a self-
sealing silicone rubber septum. The carrier gas flows through the injector carrying vaporized
solutes. The temperature of the injector should be adjusted so that flash vaporization of all
solutes occurs.

Muhammad Wajid, Assistant Professor, Gulab Devi Institute of Pharmacy, GDEC, Lahore Page 2
OVEN:

Gas chromatography have ovens that are temperature programmable, the temperature of the gas
chromatographic ovens typically range from 5°C to 400°C but can go as low as -25°C with
cryogenic cooling.

COLUMN:

Column is one of the important parts of GC which decides the separation efficiency. In GCMS
support coated open tubular columns are mostly preferred.

INTERFACE:

The pressure incompatibility problem between GC and MS was solved by inserting an interface.
Interface joins GC with MS. There are many interfaces like jet, Electrospray, thermo spray,
direct electrical ionization, moving wire or belt interface. Commercially available interface are:

o Jet Interface
o Direct Interface
IONIZATION SOURCES:

The sources which are used separate the sample into individual ions through the bombardment
technique are called as “ionization sources.” Several types of ionization sources are available
such as follows

o Electron Ionization
o Chemical Ionization
o Atmospheric Pressure Ionization
o Desorption Ionization etc.
MASS ANYLYZER:

Sample has been ionized the beam of ions is accelerated by an electric field& then passes into
the mass analyzer, the region of the mass spectrophotometer where the ions are separated
according to their m/z ratio. In GCMS diiferent types of mass analyzers are used:

Muhammad Wajid, Assistant Professor, Gulab Devi Institute of Pharmacy, GDEC, Lahore Page 3
o Quadrapole mass analyzer
o Ion trap mass analyzer
o Time of flight mass analyzer
DETECTOR:

The ion beam that emerges from the mass analyzer, have to be detected and transformed into a
usable signal. The detector is an important element of the mass spectrometer that generates a
signal from incident ions by either generating secondary electrons, which are further amplified,
or by inducing a current. Various type of detectors are used in GCMS.

o Flame Ionization Detector (FID) Compounds containing Carbon


o Thermal Conductivity Detector (TCD) Universal detection for gases without Carbon
o Nitrogen Phosphorous Detector (NPD) Selective detection of N and P containing organic
compounds
o Electron Capture Detector (ECD) Selective detection of halogen containing compounds
o Atomic Emission Detector (AED) Selective detection of elemental composition
GC-MS APPLICATIONS:

o Elucidation of the structure of organic & biological molecules.


o Impurity profiling of pharmaceuticals.
o Identification of components in thin layer & paper chromatograms.
o Identification of drugs of abuse & metabolites of drugs of abuse in blood, urine & saliva.
o Testing for the presence of the drugs in blood in race horses & in Olympic athletic (in
forensic GC-MS).
o Analyzer of aerosol particles.
o Determination of pesticide residues in food.
o Polymer characterization (pyrolysis methods combined GCMS).
o Drug monitoring & toxicology studies

Muhammad Wajid, Assistant Professor, Gulab Devi Institute of Pharmacy, GDEC, Lahore Page 4

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