Method Development of Simultaneous Determination of Organophosphorus and Synthetic Pyrethroid Pesticide Residues in Some Food by Gas Chromatographic Technique
Keywords:
GC - FPD/GC - ECD, multiclass pesticides, AOAC 2007.01, fatty foodAbstract
Separation of pesticides residues from food matrices prior to subsequent steps in the analytical process remains a challenging issue, and much effort has been invested to further improve methods. The present study was aimed to develop a simple multiresidue method modified from AOAC 2007.01 extraction method for the determination of 21 organophosphorus (OPs) and 8 synthetic pyritroid (SPs) pesticide residues in some food matrices, including milk, milk powder, soy milk and egg. Gas chromatography coupled with flame photometric detector (GC - FPD) and electron capture detector GC - ECD) were simultaneously used for identification and quantification steps. The calibration curve and working range for the analytes of interest were linear over the concentration ranges of 20 - 300 ng/ml and 10 - 150 μg/kg, respectively, with excellent correlation coefficients (r) ranging from 0.995 to 0.999. For all of the tested pesticides in four matrices, the mean recoveries at three fortification levels (10, 30 and 100 μg/kg) ranged from 25.5 and 173.8% with RSD ranging from 1.1 to 30.4% but some pesticides could not be determined. The limit of detection (LOD) and the limit of quantitation (LOQ) of the method were 5 and 10 μg/kg, respectively. Comparing with Onley method, currently used in labolatories, the developed method is fast, inexpensive and suitable for the determination of the target pesticides. In addition, this method can be easily extended to other compounds and matrices. The protocol developed is also useful for routine analysis and rapid detection of a large number of samples.
References
พระราชบัญญัติอาหาร พ.ศ. 2522 ประกาศกระทรวงสาธารณสุข เลขที่ 387 (พ.ศ. 2560) เรื่องอาหารที่มีสารพิษตกค้าง. ราชกิจจานุเบกษา เล่ม 134 ตอนพิเศษ 228 ง (วันที่ 18 กันยายน 2560).
ยุวดี เลิศเรืองเดช, อรวรรณ พัฒนกิจจารักษ์. วิธีวิเคราะห์สารเคมีกำจัดแมลงกลุ่มสารประกอบคลอรีนในนมโดยแก๊สโครมาโทกราฟ ชนิดไมโครอีซีดี. ว กรมวิทย พ 2551; 50(3): 185-96.
พระราชบัญญัติอาหาร พ.ศ. 2522 ประกาศกระทรวงสาธารณสุข ฉบับที่ 350 (พ.ศ. 2556) เรื่องนมโค. ราชกิจจานุเบกษา เล่ม 130 ตอนพิเศษ 87 ง (วันที่ 24 กรกฎาคม 2556).
Holstege DM, Scharberg DL, Tor ER, Hart LC, Galey FD. A rapid multiresidue screen for organophosphorus, organochlorine, and N-methyl carbamate insecticides in plant and animal tissues. J AOAC Int 1994; 77(5): 1263-74.
Bennett DA, Chung AC, Lee SM. Multiresidue method for analysis of pesticides in liquid whole milk. J AOAC Int 1997; 80(5): 1065-77.
Sheridan RS, Meola JR. Analysis of pesticide residues in fruits, vegetables, and milk by gas chromatography/tandem mass spectrometry. J AOAC Int 1999; 82(4): 982-90.
Lehotay SJ, Lightfield AR, Harman-Fetcho JA, Donoghue DJ. Analysis of pesticide residues in eggs by direct sample introduction/gas chromatography/tandem mass spectrometry. J Agric Food Chem 2001; 49(10): 4589-96.
Schenck FJ, Wagner R. Screening procedure for organochlorine and organophosphorus pesticide residues in milk using matrix solid phase dispersion (MSPD) extraction and gas chromatographic determination. Food Addit Contam 1995; 12(4): 535-41.
Di Muccio A, Pelosi P, Camoni I, Attard Barbini D, Dommarco R, Generali T, et al. Selective, solid-matrix dispersion extraction of organophosphate pesticide residues from milk. J Chromatogr A 1996; 754(1-2): 497-506.
Anastassiades M, Lehotay SJ, Štajnbaher D, Schenck FJ. Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solid-phase extraction” for the determination of pesticide residues in produce. J AOAC Int 2003; 86(2): 412-31.
Lehotay SJ, de Kok A, Hiemstra M, Van Bodegraven P. Validation of a fast and easy method for the determination of residues from 229 pesticides in fruits and vegetables using gas and liquid chromatography and mass spectrometric detection. J AOAC Int 2005; 88(2): 595-614.
Koesukwiwat U, Lehotay SJ, Mastovska K, Dorweiler KJ, Leepipatpiboon N. Extension of the QuEChERS method for pesticide residues in cereals to flaxseeds, peanuts, and doughs. J Agric. Food Chem 2010; 58(10): 5950-8.
Onley JH. Rapid method for chlorinated pesticide residues in fluid milk. J AOAC 1964; 47(2): 317-21.
Ellison SLR Rosslein M, Williams A, editors. EURACHEM/CITAC guide quantifying uncertainty in analytical measurement. 2nd ed. United Kingdom: EURACHEM; 2000.
AOAC guidelines for single laboratory validation of chemical methods for dietary supplements and botanicals. [Online]. 2002 [cited 2016 Nov 12]; [38 screens]. Available from: URL: https://www.aoac.org/aoac_prod_imis/AOAC_Docs/StandardsDevelopment/SLV_Guidelines_Dietary_Supplements.pdf.
Guidance document on analytical quality control and method validation procedures for pesticides residues analysis in food and feed. SANTE/11945/2015. [Online]. 2015 [cited 2017 Nov 13]; [46 screens]. Available from: https://www.accredia.it/app/uploads/2015/12/6215_plant_pesticides_mrl_guidelines_wrkdoc_11945_en.pdf.
กองโภชนาการ กรมอนามัย กระทรวงสาธารณสุข. กรดไขมันและคอเลสเตอรอลในอาหารไทย. [ออนไลน์]. 2556 [สืบค้น 12 พย. 2556]; [170 หน้า]. เข้าถึงได้ที่ : URL: https://nutrition2.anamai.moph.go.th/images/design2016/กรดไขมันและคอเลสเตอรอลในอาหารไทย.pdf.
Sangster J. Octanol-water partition coefficients of simple organic compounds. J Phys Chem Ref Data 1989; 18(3): 1111-227.
U.S. Department of Agriculture/Agricultural Marketing Service. Acceptability Criteria of Process Control and Fortification Recoveries, PDP-QC-04. [Online]. 2002 [cited 2016 Nov 12]. Available from: URL: https://www.ams.usda.gov/science/pdp/Qc04.pdf.
Lehotay SJ, Lee CH. Evaluation of a fibrous cellulose drying agent in supercritical fluid extraction and pressurized liquid extraction of diverse pesticides. J Chromatogr A 1997; 785: 313-27.
Downloads
Published
How to Cite
Issue
Section
License

This work is licensed under a Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International License.
