See discussions, stats, and author profiles for this publication at: https://www.researchgate.

net/publication/335577195

Determination of Permethrin in Pharmaceutical Product by Gas

Chromatography

Article in IOSR Journal of Pharmacy and Biological Sciences · December 2017

DOI: 10.9790/3008-1206064245

CITATION READS

1 1,286

3 authors, including:

Mohamed Amin Mohamed Aly Abd El Aziz Aly El Degwy

Pt CELL for Pharmaceutical Industries Hi Pharm
19 PUBLICATIONS 46 CITATIONS 13 PUBLICATIONS 35 CITATIONS

SEE PROFILE SEE PROFILE

Some of the authors of this publication are also working on these related projects:

Supercritical Fluid Extraction View project

Application of Supercritical Fluid Extraction in Pharmaceutical Industry View project

All content following this page was uploaded by Mohamed Amin on 03 September 2019.

The user has requested enhancement of the downloaded file.

IOSR Journal of Pharmacy and Biological Sciences (IOSR-JPBS)
e-ISSN:2278-3008, p-ISSN:2319-7676. Volume 12, Issue 6 Ver. VI (Nov. – Dec. 2017), PP 42-45
www.iosrjournals.org

Determination of Permethrin in Pharmaceutical Product by Gas

Chromatography
'*
Mohamed A. Amin1, Mohamed A. El-Degwy1and Bassem A. Fayed2
1
Arab Company for Pharmaceuticals and Medicinal Plants, (Mepaco-Medifood), Egypt.
2
Future Pharmaceutical Industries, Egypt
*
Corresponding Author: Mohamed A. Amin
_____________________________________________________________________________________
Abstract: Gas chromatographic analysis was applied for the quantitative determination of permethrin present in
some pharmaceutical products.The calibration curve of permethrin was linear with determination coefficient
(R2) = 0.99998; over a concentration range of 1200 – 2800 mg/l; with a retention time of 31.599, 32.578
minutes for Cis-permethrin, Trans-permethrin; respectively. Thevalidated GC method was successfully applied
for the quantitative determination of the permethrin, either as a separate raw material or within the
pharmaceutical product.
Key words: GC, Permethrin, Method Validation.
----------------------------------------------------------------------------------------------------------------------------- ----------
Date of Submission: 28-11-2017 Date of acceptance: 30-12-2017
----------------------------------------------------------------------------------------------------------------------------- ----------

I. Introduction
Pyrethrum flower is the dried flower heads of Chrysanthemum cinerariaefolium containing not less
than 1% of pyrethrins of which not less than one-half consists of pyrethrin I. It has a faint but characteristic
odour (1). Pyrethrum, pyrethrins, and pyrethroids are also used as topical ectoparasiticides in veterinary practice
and as agricultural, horticultural, and household insecticides (2). Permethrin is a non-systemic pyrethroid
insecticide with some repellent effects. It is a viscous liquid at room temperature; it does not dissociate in water
and has extremely low water solubility and volatility. It is stable to hydrolysis at pH 4–7. Technical grade
permethrin is composed of 4 stereoisomers, due to the chirality at two carbon atoms in the cyclopropane ring,
leading to 2 cis and 2 trans isomers. Permethrin technical grade cis:trans ratio is either 25:75 or 40:60. (6)

Fig (1): Chemical structure of permethrin (6)

Permethrin is commercially available in the following dosage forms: Medicated Shampoo, topical
Cream, topical gel, topical Lotion, topical Spray. Permethrin is available in the following strengths: Topical
lotion and cream 5 % for the treatment of scabies, topical lotion 1 % and shampoo 1 % for head lice. Also
topical gel 2 % is present as well for scabies. Topical spray 0.25 and 0.5 % is also available as insect repellant,
applied on clothes (5, 6). Permethrin is active against mosquitoes and is widely used for the impregnation of
bednets and curtains in the control of malaria. It is also active against blackflies in the adult and larval stages
and is used for the larvicidal treatment of rivers in the control of onchocerciasis. It is also active against tsetse
flies. Permethrin is suitable for aircraft disinfection (4). Nowadays, due to its safety use, growing interest on its
use is vastly.

II. Materials& Methods

1. Equipment
 Gas Chromatography: Shimadzu GC, Model 2010, connected with FID detector auto injector, Kyoto,
Japan.
Column:DB-5 (0.25mm x 30 m), 0.25 umdf, Agilent, USA.

DOI: 10.9790/3008-1206064245 www.iosrjournals.org 42 | Page

 Determination of Permethrin in Pharmaceutical Product by GasChromatography

 Electronic Balance: Model AUY220, Shimadzu Instrument, Kyoto, Japan

 Ultrasonic bath: NSXX Sonics Model NS-A-12-7H, Germany.

2. Chemical Reagents:
All chemical reagents and standards used were GC grade. Pure standard of permethrin was obtained from
Hetero Drugs, Hyderabad.Hexane  97% was HPLC and GC grade from Sigma Aldrich.

III. Experimental
3.1 Chromatographic conditions:
The GC analysis was carried out using Shimadzu GC, Model 2010, connected with FID detector auto injector,
under the following condition:
Column: DB-5 (0.25mm x 30 m), 0.25 umdf, Agilent, USA.
Injection volume:1 µl.
Flow rate: 13.5 ml/min.
Injection Temp.: 300C.
Injection Mode: Splitless
Split ratio: 10
Carrier gas: Helium.
Oven Temperature Program:
Rate (C/min) Temperature (C) Hold Time (min)
---- 60 2
7 277 2

4.1. Method Validation:

4.1.1. Calibration curves:
The stock standard solution of purestandard was prepared as follows:
100 mg of the compound was accurately weighed and placed into a 50 ml volumetric flask. n-Hexane was added
and the solution was diluted to volume with the same solvent, then it was sonicated for 15 min.
Calibration curve was established on nine data points covering the concentration range of 1200– 2800µg/ml.
One microliter aliquots of each standard solution were used for GC analysis. Triplicate injections were made for
each standard solution. The calibration curve was obtained by plotting the peak area of the permethrin at each
level prepared versus the concentration of the sample.

Table (1): Statistical analysis for the calibration curve of the permethrin standards
Compound Linearity range (µg/ml) Slope, a Intercept, b R2
Permethrin 1200-2800 6,756.8578 -28,260.699 0.99998

S.D. values are given in parenthesis.

a for each curve the equation is y = ax + b, where y is the peak area, x is the concentration of the analyte (µg/ml),
a is the slope, b is the intercept and R2 is the determination coefficient.

4.1.2. Recovery
The accuracy of the method was evaluated with the recovery test. This involved the addition of known
quantities of permethrin standards to known amounts of sample. The percentage recovery was determined by
subtracting the values obtained for the control matrix preparation from those samples that were prepared with
the added standards, divided by the amount added; then multiplied by 100.

Table (2): Results of the recovery test for the used essential oil & extract
Compound Spiked amount (mg) Recovery (%) Mean (n = 5) R.S.D. (%)
Permethrin 0.530 99.88-101.42 100.82 1.60
R.S.D. (%) = (standard deviation/mean) ×100.

4.1.3. Limits of detection and quantification

Limits of detection (LOD) were calculated according to the expression 3.3σ/S, where σ is the standard
deviation of the response and S is the slope of the calibration curve. Limits of quantification (LOQ) were
established by using the expression 10σ/S. LOD and LOQ were experimentally verified by injections of pure
standard at the LOD and LOQ concentrations.

DOI: 10.9790/3008-1206064245 www.iosrjournals.org 43 | Page

 Determination of Permethrin in Pharmaceutical Product by GasChromatography

Table (3): Limit of detection (LOD) and limit of quantification (LOQ)

Compound LOD (µg/ml) LOQ (µg/ml)
Permethrin 33.33 100

4.2. Standard Preparation:

100 mg of the following standard was accurately weighed and transferred into 50 ml volumetric flask; then
dissolved in hexane and sonicated for 15 minutes. The volume was completed to 50 ml with hexane.
 (Dilutions were done case related).

IV. Results and Discussion

The used GC method for the analysis of pharmaceutical product proved that it is an accurate, precise,
fast and easy method for the quality control of complex pharmaceutical products containing mixture of cis and
trans-permethrin. This fact is clear and can be deduced from the obtained result of calibration curve table (1);
where the linearity was found to be (1200-2800 µg/ml), slope (6,756.8578), intercept (-28,260.699) and the
determination coefficient (0.99998).
The percentage recoveries table (2) range form (99.88-101.42%). Limit of detection (LOD) and limit of
quantification (LOQ)are shown in table (3);where we can value of LOD (33.33 µg/ml) and LOQ (100 µg/ml).

Fig (2): Specificity of assay of permethrin (standard injection)

Fig (3): Specificity of assay of permethrin (Test injection)

DOI: 10.9790/3008-1206064245 www.iosrjournals.org 44 | Page
 Determination of Permethrin in Pharmaceutical Product by GasChromatography

IV. Conclusion
The applied GC method is of great value for the quality control of the pharmaceutical products containing
mixture of cis and trans-permethrin.

References
[1]. British Pharmacopeia Veterinary 2005.
[2]. Sweetman, Sc. “Martindale” The complete drug reference, Pharmaceutical press.35st ed. 2007.
[3]. WHO. Permethrin health and safety guide. IPCS Health and Safety Guide 33. Geneva: WHO, 1989.
[4]. WHO. Permethrin. Environmental Health Criteria 94. Geneva: WHO, 1990.
[5]. Sweetman, Sc. “Martindale” The complete drug reference, 37st ed. 2009, Pharmaceutical press.
[6]. WHOspecifications for public health pesticides 40:60 cis:transpermethrin technical material. WHO specification 331/TC (March
2009).

Mohamed A. Amin "Determination of Permethrin in Pharmaceutical Product by Gas

Chromatography." IOSR Journal of Pharmacy and Biological Sciences (IOSR-JPBS) 12.6
(2017): 42-45.

DOI: 10.9790/3008-1206064245 www.iosrjournals.org 45 | Page

View publication stats