DETERMINATION OF CHLORPYRIFOS IN LETTUCE (LACTUCA SATIVA L.) BY MICROWAVE-ASSISTED EXTRACTION COUPLED WITH HEADSPACE SINGLE DROP MICROEXTRACTION

  • Naruephon Watthanaphap Faculty of Pharmaceutical Sciences, Chiang Mai University, Thailand
  • Surapol Natakankitkul Faculty of Pharmaceutical Sciences, Chiang Mai University, Thailand
  • Nuchnart Jonglaekha Plant Protection Center, Royal Project Foundation, Thailand

Abstract

Objective: The objective of this research was to improve the method of extracting pesticide residue from vegetable by using microwave-assisted extraction, headspace single drop microextraction (MAE-HS-SDME) and analysed by gas chromatograph-mass spectrometer (GC-MS).

Methods: Microwave-assisted extraction (MAE) coupled with headspace single drop microextraction (HS-SDME) was used for extraction of chlorpyrifos insecticide residues in lettuce. The optimum conditions for obtaining efficient extraction have been tried; kind and quantity of solvent, extraction time, microwave irradiation power, pH value and the amount of salt added in the sample followed the method of Plackett–Burman. Optimum conditions for efficient analysis were evaluated by using a central composite design (CCD) combined with a response surface methodology (RSM).

Results: The optimum extract conditions from CCD for the MAE-HS-SDME method were: using 1.5 µl of n-butyl acetate, 460 W of the microwave power, 4.5 min of the extraction time, no pH adjustment and no salt addition. Verification of the optimized experimental conditions showed that validation of the determination coefficient ranges from the concentrations of 0.01 to 0.10 mg/l, equal to 0.999; the percentages of variation coefficient were ranges from 4.6 to 7.7%; the recoveries ranges from 70.0 to 79.5%; limit of detection was 0.003 mg/kg and limit of quantitation was 0.01 mg/kg.

Conclusion: In this study, the MAE-HS-SDME method coupled with GC-MS was found most suitable for chlorpyrifos analysis. The results obtained from analyzing chlorpyrifos in lettuce samples indicated that this method is rapid, simple, sensitive, reducible cost and safety for the analyst and the environment.

Keywords: Chlorpyrifos, Headspace single drop microextraction, Microwave-assisted extraction

Downloads

Download data is not yet available.

References

1. Jeannot MA, Cantwell FF. Solvent microextraction into a single drop. Anal Chem 1996;68:2236-40.
2. Zhang M, Huang J, Wei C, Yu B, Yang X, Chen X. Mixed liquids for single-drop microextraction of organochlorine pesticides in vegetables. Talanta 2008;74:599-604.
3. Amvrazi EG, Tsiropoulos NG. Chemometric study and optimization of extraction parameters in single-drop. J Chromatogr A 2009;1216:7630-8.
4. Amvrazi EG, Tsiropoulos NG. Application of single-drop microextraction coupled with gas chromatography for the determination of multiclass pesticides in vegetables with nitrogen phosphorus and electron capture detection. J Chromatogr A 2009;1216:2789-97.
5. Xiao Q, Hu B, He M. Speciation of butyltin compounds in environmental and biological samples using headspace single drop microextraction coupled with gas chromatography-inductively coupled plasma mass spectrometry. J Chromatogr A 2008;1211:135-41.
6. Abdelmohsen MM, Nazif NM, Seif el Nasr MM. Microwave-assisted extraction of bio-active compounds (phenolics and alkamides) from Echinacea purpurea. Int J Pharm Pharm Sci 2014;6:265-8.
7. Kormin F, Khan M, Chandra AI. Microwave assisted extraction; Phytochemical evaluation of Malaysian palm oil trunk epiphytes ferns. Int J Pharm Pharm Sci 2016;8:174-80.
8. Pramanik T, Majia P. Microwave assisted green synthesis of pharmaceutically important dihydropyrimidinones in fruit juice medium. Int J Pharm Pharm Sci 2015;7:376-9.
9. Rebbapragada D, Kalyanaraman R. Statistical optimization of the medium of components by Plackett-Burman design and response surface methodology for enhanced antioxidant activity by Xylaria feejeensis HMJAU22039. Int J Pharm Pharm Sci 2016;8:159-64.
10. Kuchekar SB, Mohite KS. Design and evaluation of extended release ranolazine liauisoloid tablets using placket-burman screening design. Asian J Pharm Clin Res 2015;8:292-300.
11. Sumithra S. Application of quality by design (CCD technique) for simultaneous estimation of cefixime and ofloxacin by HPTLC methods. Int J Pharm Pharm Sci 2016;8:200-8.
12. Kumar GN, Kuma S, Vimalan S, Prakash P, Nandagopal S, Kumar RB. Optimization of growth promoters on Desmodium gangeticum (L) DC using RSM-CCD and its antioxidants activity. Int J Pharm Pharm Sci 2014;6:503-7.
13. Satishkumar PJ, Singh PP, Javeer S, Purnima D. Use of Placket-Burman statistical design to study the effect of formulation variables on the release of drug from hot melt sustained release extrudates. AAPS PharmSciTech 2010;11:936-44.
14. Codex Alimentarius Commission. Guideline on good laboratory practice in pesticide residue analysis CAC/GL 40-1993; 2003. p. 1-36.
15. Lehotay SJ. Determination of pesticides residues in food by acetonitrile extraction and partitioning with magnesium sulfate: Collaborative study. J AOAC Int 2007;90:485-517.
16. EN 15662:2008 standard, foods of plant origin determination of pesticide residues using GC-MS and/or LC-MS/MS following acetonitrile extraction/partitioning and clean-up by dispersive SPE-QuEChERS-method; 2008.
17. Cortada C, Vidal L, Tejada S, Romo A, Canals A. Determination of organochlorine pesticides in complex matrices by single-drop microextraction coupled to gas chromatography–mass spectrometry. Anal Chim Acta 2009;638:29-35.
18. Lorena Vidal, Domini CE, Gran N, Psillakis E, Canals A. Microwave-assisted headspace single-drop microextraction of chlorobenzenes from water samples. Anal Chim Acta 2007;592:5-15.
19. Kumar PV, Jen JF. Rapid determination of dichlorodiphenyltrichloroethane and its main metabolites in aqueous samples by one-step microwave-assisted headspace controlled-temperature liquid-phase microextraction and gas chromatography with electron capture detection. Chemosphere 2011;83:200-7.
20. Pinheiro AS, de Andradea JB. Development, validation and application of an SDME/GC-FID methodology for the multi residue determination of organophosphate and pyrethroid pesticides in water. Talanta 2009;79:1354-9.
21. Pinheiro AS, Rocha GO, de Andrade JB. A SDME/GC-MS methodology for determination of organophosphate and pyrethroid pesticides in water. Microchem J 2011;99:303-8.
22. Garbi A, Sakkas V, Fiamegos YC, Stalika CD, Albanis T. Sensitive determination of pesticides residues in wine samples with the aid of single-drop microextraction and response surface methodology. Talanta 2010;82:1286–91.
Statistics
282 Views | 1269 Downloads
Citatons
How to Cite
Watthanaphap, N., S. Natakankitkul, and N. Jonglaekha. “DETERMINATION OF CHLORPYRIFOS IN LETTUCE (LACTUCA SATIVA L.) BY MICROWAVE-ASSISTED EXTRACTION COUPLED WITH HEADSPACE SINGLE DROP MICROEXTRACTION”. International Journal of Pharmacy and Pharmaceutical Sciences, Vol. 9, no. 5, May 2017, pp. 248-55, doi:10.22159/ijpps.2017v9i5.16849.
Section
Original Article(s)