增强型脂质去除分散固相萃取净化-气相色谱-串联质谱法测定动物性食品中146种农药残留  

Determination of 146 kinds of pesticide residues in animal derived food by enhanced matrix removal-lipid dispersion solid phase extraction purification coupled with gas chromatography-tandem mass spectrometry

作　　者：杨志敏 薛华丽[2] 潘秀丽 李运 李坚 丁辉 李赟 许晓辉 陈婷 YANG Zhi-Min;XUE Hua-Li;PAN Xiu-Li;LI Yun;LI Jian;DING Hui;LI Yun;XU Xiao-Hui;CHEN Ting(Lanzhou Institute for Food and Drug Control,Key Laboratory of Pesticide and Veterinary Drug Monitoring,State Administration for Market Regulation,Lanzhou 730050,China;College of Science,Gansu Agricultural University,Lanzhou 730070,China)

机构地区：[1]兰州市食品药品检验检测研究院,国家市场监督管理总局重点实验室/食品中农药兽药残留监控,兰州730050 [2]甘肃农业大学理学院,兰州730070

出　　处：《食品安全质量检测学报》2025年第6期114-121,共8页Journal of Food Safety and Quality

基　　金：甘肃省市场监督管理局科技计划项目(SSCJG-SP-A202308);兰州市青年科技人才创新项目(2023-QN-180);兰州市科技发展指导性计划项目(2023-ZD-234,2024-9-227);兰州市科技计划项目(2023-3-29)。

摘　　要：目的 建立一种基于增强型脂质去除分散固相萃取(enhanced matrix removal-lipid dispersion solid phase extraction,d SPE EMR-Lipid)净化技术结合气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)测定动物性食品中146种农药残留量的分析方法。方法 在5 g样品中加入2 m L超纯水,经乙腈提取,冷冻10 min,Qu ECh ERS-EN-盐包除水分离,采用d SPE EMR-Lipid净化技术,GC-MS/MS动态多反应监测(dynamic multi-reaction monitoring,DMRM)模式监测,基质匹配标准曲线法定量分析。结果 146种化合物在5~320μg/L范围内线性关系良好,相关系数均大于0.9939,方法的检出限为0.04~10.91μg/kg,定量限为0.11~32.72μg/kg。146种化合物在0.01、0.02和0.10 mg/kg 3个不同加标水平下的平均回收率范围在61.3%~119.3%之间,相对标准偏差为0.15%~16.02%。结论 该方法操作简便快速,灵敏准确,能够满足多种农药残留量的同时检测需求,适用于动物性食品中多种农药残留的定量筛查。Objective To establish an analytical method for the determination of 146 kinds of pesticide residues in animal derived foods by enhanced matrix removal-lipid dispersion solid phase extraction(dSPE EMR-Lipid)and purification technology coupled with gas chromatography-tandem mass spectrometry(GC-MS/MS).Methods The 5 g sample were added to 2 mL ultrapure water,extracted with acetonitrile,freezed for 10 min,separated with QuEChERS EN-extraction package,cleaned-up with dSPE EMR-Lipid,then was detected by GC-MS/MS in dynamic multi-reaction monitoring(DMRM)mode.The analytes were quantified by matrix-matched standard curve method.Results The results showed that 146 kinds of pesticides had good linearities in the concentration of 5–320μg/L,the linear correlation coefficient of the compounds were greater than 0.9939,and the limits of detection of the method were 0.04–10.91μg/kg,the limits of quantification were 0.11–32.72μg/kg.The average recoveries of 146 kinds of pesticides at the spiked level of 0.01,0.02 and 0.10 mg/kg ranged from 61.3%to 119.3%,relative standard deviations were 0.15%–16.02%.Conclusion The method is simple in pre-treatment,convenient in operation,rapid,sensitive and accurate in detection,can meet the simultaneous detection requirements for multiple pesticide residues.It is suitable for preliminary screening and quantitative detection of multiple pesticide residues in animal derived food.

关 键 词：动物性食品 增强型脂质去除分散固相萃取 气相色谱-串联质谱法 农药残留 

分 类 号：O657.63[理学—分析化学] TS207.53[理学—化学]