分散固相萃取净化与气相色谱-串联质谱法同时测定蔬菜中157种农药残留  

Determination of 157 pesticide residues in vegetables by using dispersive solid phase extraction purification coupled with gas chromatography-tandem mass spectrometry

作　　者：杨志敏 薛华丽[2] 李坚 丁辉 赵波 张新中 YANG Zhimin;XUE Huali;LI Jian;DING Hui;ZHAO Bo;ZHANG Xinzhong(Key Laboratory of Pesticide and Veterinary Drug Monitoring for State Market Regulation,Lanzhou Institute for Food and Drug Control,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,食品中农药兽药残留监控重点实验室,甘肃兰州730050 [2]甘肃农业大学理学院,甘肃兰州730070

出　　处：《甘肃农业大学学报》2024年第5期304-313,共10页Journal of Gansu Agricultural University

基　　金：甘肃省科技计划重大项目(21ZD4NA016);甘肃省市场监督管理局科技计划项目(SSCGJ-J202303,SSCJG-SP-A202308);兰州市青年科技人才创新项目(2023-QN-180)。

摘　　要：【目的】建立一种分散固相萃取净化结合气相色谱-串联质谱法测定蔬菜中157种农药化合物的分析方法。【方法】样品经过乙腈和QuEChERSEN-提取包提取,用无水硫酸镁150 mg、N-丙基乙二胺(primary secondary amine,PSA)75 mg、石墨化碳黑(graphitized carbon black,GCB)5 mg的填料管净化,在GC-MS/MS的动态多反应监测(dMRM)模式下检测,基质匹配标准曲线法定量分析。【结果】157种化合物在各自质量浓度范围内线性关系良好,相关系数均大于0.992 1,检出限范围为0.032~6.198μg/kg,定量限为0.107~19.496μg/kg。在0.01、0.02、0.10mg/kg加标水平下157种农药的平均回收率为74.5%~117.3%,RSD(n=6)为0.4%~10.5%。【结论】该方法前处理简单、快速、灵敏,能够满足多种农残的同时检测需求,可广泛应用于蔬菜等样品的筛查和定量检测。【Objective】The study aimed to develop a method of the determination of 157 pesticide compounds in vegetables by using the dispersive solid phase extraction purification combined with gas chromatography-tandem mass spectrometry(GC-MS/MS).【Method】The samples were extracted with acetonitrile and QuEChERS EN-extraction package,cleaned-up with purifying packing tubes including 150 mg MgSO4,75 mg PSA and 5 mg GCB,and then was detected by GC-MS/MS in dynamic multi-reaction monitoring(dMRM)mode,followed by quantitative analysis with the matrix-matched standard curve.【Result】The results showed that 157 pesticides had good linear relationships in the range their concentrations,the correlation coefficients were all greater than 0.9921,the limits of detection(LOD)were 0.032~6.198μg/kg,and the limits of quantification(LOQ)were 0.107~19.496μg/kg.The average rates of recovery for 157 pesticides were 74.5%~117.3%and RSDS(n=6)were 0.4%~10.5%at the markup levels of 0.01,0.02 and 0.10 mg/kg.【Conclusion】The method is simple,rapid and sensitive,and may meet the requirements for multiple pesticide residues detection,which can be widely used in the rapid screening and quantitative detection of vegetable samples.

关 键 词：蔬菜 分散固相萃取净化 气相色谱-串联质谱法(GC-MS/MS) 多种农药残留 

分 类 号：O657.63[理学—分析化学] TS255.7[理学—化学]