High-throughput detection of organophosphorus pesticide residues in fresh meat by QuEChERS-GC-MS/MS

  • WANG Shasha ,
  • SHEN Xixi ,
  • LI Manman ,
  • SHEN Juan ,
  • TANG Changbo ,
  • WANG Wei
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  • 1(College of Food Science and Technology,Nanjing Agricultural University,Nanjing 210095,China)
    2(National Center of Meat Quality and Safety Control,Nanjing Agricultural University,Nanjing 210095,China)
    3(Supervision,Inspection and Testing Center for Quality of Meat-products(Nanjing),Ministry of Agriculture and Rural Affairs,Nanjing Agricultural University,Nanjing 210095,China)

Online published: 2022-04-06

Abstract

This study aimed to establish a rapid and effective QuEChERS-GC-MS/MS detection method for 18 organophosphorus pesticide residues in fresh meat. The sample was extracted with saturated n-hexane in acetonitrile and purified by dispersion solid-phase extraction with MgSO4, CH3COONa, N-propyl ethylenediamine (PSA) and octadecyl bonded silica gel (C18). Then DB-1701 capillary column was used for the separation, and GC-MS/MS was used for the detection. Organophosphorus pesticides showed a good linear relationship in the range of 1-100 μg/kg, and the square of correlation coefficient (R2) were all greater than 0.990 0. The detection limit was 0.02-0.74 μg/kg and the quantification limit was 0.08-2.48 μg/kg. Meanwhile, the recovery rate reached 76%-106% and the relative standard deviation was 0.50%-7.9%. The QuEChERS-GC-MS/MS method established in this study can simultaneously detect 18 organophosphorus pesticides. It is simple, fast, sensitive and accurate, which can meet the high throughput and rapidity of organophosphorus pesticide residues in fresh livestock and poultry meat.

Cite this article

WANG Shasha , SHEN Xixi , LI Manman , SHEN Juan , TANG Changbo , WANG Wei . High-throughput detection of organophosphorus pesticide residues in fresh meat by QuEChERS-GC-MS/MS[J]. Food and Fermentation Industries, 2022 , 48(5) : 262 -267 . DOI: 10.13995/j.cnki.11-1802/ts.029702

References

[1] 李雯雯,王岩,王盛男,等.植物源性食品中有机磷农药残留检测前处理技术的研究进展[J].食品安全质量检测学报,2020,11(6):1 852-1 858.
LI W W,WANG Y,WANG S N,et al.Research progress of pretreatment technology for detection of organophosphorus pesticide residues in plant-derived foods[J].Journal of Food Safety & Quality,2020,11(6):1 852-1 858.
[2] GRILO A,MOREIRA A,CARRAPIO B,et al.Epidemiological study of pesticide poisoning in domestic animals and wildlife in Portugal:2014-2020[J].Frontiers in Veterinary Science,2020,7:616293.
[3] 沙鸥,姚佳伟,许丽,等.有机磷农药中毒患者体内有机磷检测研究进展[J].化学试剂,2021,43(7):857-864.
SHA O,YAO J W,XU L,et al.Research progress on organophosphorus detection in patients with organophosphorus pesticide poisoning in diagnosis[J].Chemical Reagents,2021,43(7):857-864.
[4] 刘仁杰,赵悦,王玉华,等.有机磷农药残留现状及去除方法的研究进展[J].食品工业,2019,40(9):299-302.
LIU R J,ZHAO Y,WANG Y H,et al.Research progress of organophosphorus pesticide residues status and removal methods[J].The Food Industry,2019,40(9):299-302.
[5] 张峰祖,朴秀英,李富根.国际食品法典委员会动物源性食品中农药最大残留限量制定现状[J].农药学学报,2021,23(1):22-30.
ZHANG F Z,PIAO X Y,LI F G.Current situation on setting of pesticide maximum residue limits in food commodities of animal origin in Codex Alimentarius Commission[J].Journal of Pesticide Science,2021,23(1):22-30.
[6] 穆兰,朴秀英,陈晓初,等.韩国农药残留肯定列表制度对我国农产品出口贸易的影响[J].农药科学与管理,2019,40(4):12-15.
MU L,PIAO X Y,CHEN X C,et al.Influence on agricultural product export from China bysouth Korea PLS[J].Pesticide Science and Administration,2019,40(4):12-15.
[7] DALLEGRAVE A,PIZZOLATO T M,BARRETO F,et al.Methodology for trace analysis of 17 pyrethroids and chlorpyrifos in foodstuff by gas chromatography-tandem mass spectrometry[J].Analytical and Bioanalytical Chemistry,2016,408(27):7 689-7 697.
[8] MADEJ K,KALENIK T K,PIEKOSZEWSKI W.Sample preparation and determination of pesticides in fat-containing foods[J].Food Chemistry,2018,269:527-541.
[9] PANG G F,CAO Y Z,ZHANG J J,et al.Validation study on 660 pesticide residues in animal tissues by gel permeation chromatography cleanup/gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry[J].Journal of Chromatography.A,2006,1125(1):1-30.
[10] CASTILLO M,GONZLEZ C,MIRALLES A.An evaluation method for determination of non-polar pesticide residues in animal fat samples by using dispersive solid-phase extraction clean-up and GC-MS[J].Analytical and Bioanalytical Chemistry,2011,400(5):1 315-1 328.
[11] HU S P,ZHAO M,MAO Q Q,et al.Rapid one-step cleanup method to minimize matrix effects for residue analysis of alkaline pesticides in tea using liquid chromatography-high resolution mass spectrometry[J].Food Chemistry,2019,299:125146.
[12] ISLAM A,NOH HH,RO J H,et al.Optimization and validation of a method for the determination of acidic pesticides in cabbage and spinach by modifying QuEChERS procedure and liquid chromatography-tandem mass spectrometry[J].Journal of Chromatography B,2021,1173:122667.
[13] 郭思依,孙明娜,董旭,等.免疫分析技术在农药残留快速检测中的应用及研究进展[J].中国农学通报,2021,37(23):106-112.
GUO S Y,SUN M N,DONG X,et al.Application and research progress of immunoassay technology in rapid detection of pesticide residues[J].Chinese Agricultural Science Bulletin,2021,37(23):106-112.
[14] YANG L X,LI H L,ZENG F G,et al.Determination of 49 organophosphorus pesticide residues and their metabolites in fish,egg,and milk by dual gas chromatography-dual pulse flame photometric detection with gel permeation chromatography cleanup[J].Journal of Agricultural and Food Chemistry,2012,60(8):1 906-1 913.
[15] 段税优,卢专,杨昌彪,等.QuEChERS结合GC-MS法测定新鲜鸡蛋中15种农药残留[J].现代食品,2019(14):123-128.
DUAN S Y,LU Z,YANG C B,et al.Determination of 15 pesticide residues in fresh eggs byQuEChERS combined with GC-MS[J].Modern Food,2019(14):123-128.
[16] 吕青骎,王玮,梁丽姣,等.QuEChERS结合超高效液相色谱质谱法测定禽蛋及其制品中42种农药及其代谢物[J].食品与发酵工业,2020,46(5):255-262.
LV Q Q,WANG W,LIANG L J,et al.Determination of 42 pesticides and their metabolites in poultry eggs and products by QuEChERS-UPLC-MS/MS[J].Food and Fermentation Industries,2020,46(5):255-262.
[17] KILJANEK T,NIEWIADOWSKA A,MAYSIAK M,et al.Miniaturized multiresidue method for determination of 267 pesticides,their metabolites and polychlorinated biphenyls in low mass beebread samples by liquid and gas chromatography coupled with tandem mass spectrometry[J].Talanta,2021,235:122721.
[18] BARCI P E P,ALVES L D S,AVELLAR A S,et al.ModifiedQuEChERS method for multiresidue determination of pesticides in pecan nuts by liquid chromatography tandem mass spectrometry[J].Food Analytical Methods,2020,13(3):793-801.
[19] 李德青,石桂珍.有机磷农药残留检测方法研究进展与分析[J].煤炭与化工,2020,43(2):146-150.
LI D Q,SHI G Z.Research progress and analysis of organophosphorus pesticide residue detection methods[J].Coal and Chemical Industry,2020,43(2):146-150.
[20] SONG L,HAN Y T,YANG J,et al.Rapid single-step cleanup method for analyzing 47 pesticide residues in pepper,chili peppers and its sauce product by high performance liquid and gas chromatography-tandem mass spectrometry[J].Food Chemistry,2019,279:237-245.
[21] WALORCZYK S.Validation and use of a QuEChERS-based gas chromatographic-tandem mass spectrometric method for multiresidue pesticide analysis in blackcurrants including studies of matrix effects and estimation of measurement uncertainty[J].Talanta,2014,120:106-113.
[22] GIACINTI G,RAYNAUD C,CAPBLANCQ S,et al.Evaluation and prevention of the negative matrix effect of terpenoids on pesticides in apples quantification by gas chromatography-tandem mass spectrometry[J].Journal of Chromatography A,2017,1 483:8-19.
[23] 李敏青,安文佳,李菊,等.固相萃取/气相色谱法测定禽蛋中19种农药残留[J].分析测试学报,2020,39(4):520-525.
LI M Q,AN W J,LI J,et al.Determination of 19 pesticides residues in eggs by gas chromatography with solid phase extraction[J].Journal of Analytical Testing,2020,39(4):520-525.
[24] 吴卫东,吴凤琪,万志刚,等.在线凝胶渗透色谱-串联气质联用法测定植物油和猪肉中55种农药残留[J].食品安全质量检测学报,2014,5(11):3 400-3 409.
WU W D,WU F Q,WAN Z G,et al.Determination of 55 pesticide residues in vegetable oil and animal tissues using on-line gel permeation chromatography coupled with gas chromatography-mass spectrometry[J].Journal of Food Safety and Quality,2014,5(11):3 400-3 409.
[25] HAMADAMIN A Y,HASSAN K I.Gas chromatography-mass spectrometry based sensitive analytical approach to detect and quantify non-polar pesticides accumulated in the fat tissues of domestic animals[J].Saudi Journal of Biological Sciences,2020,27(3):887-893.
[26] KANG H S,KIM M,KIM E J,et al.Determination of 66 pesticide residues in livestock products using QuEChERS and GC-MS/MS[J].Food Science and Biotechnology,2020,29(11):1 573-1 586.
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