全自动固相萃取-气相色谱-三重四极杆质谱法同时测定水中多类型农药残留  

Simultaneous determination of multi-types of pesticide residues in water by gas chroma-tography-triple quadrupole mass spectrometry with automated solid phase extraction

作　　者：钱晓敏 万玲 李卫国 薛爱龙 QIAN Xiaomin;WAN Ling;LI Weiguo;XUE Ailong(Wujiang Center for Disease Prevention and Control,Suzhou 215200,China)

机构地区：[1]苏州市吴江区疾病预防控制中心,苏州215200

出　　处：《分析试验室》2025年第4期502-510,共9页Chinese Journal of Analysis Laboratory

基　　金：苏州市吴江区“科教兴卫”项目(WWK202118)资助。

摘　　要：应用全自动固相萃取-气相色谱-串联质谱建立了同时测定水中除草剂、杀虫剂、杀菌剂、植物生长调节剂等4大类15小类59种农药残留的方法。水样经HLB固相萃取柱净化富集,HP-5MS色谱柱分离,多反应监测模式下质谱测定,经分析保护剂改进的基质匹配内标法定量。结果表明,5种氨基甲酸酯类目标物分别在4~80 ng/mL,6~120 ng/mL,15~300 ng/mL浓度范围内,8种六六六(HCH)、滴滴涕(DDT)同分异构体在5~100 ng/mL浓度范围内,其余46种目标物在10~200 ng/mL范围内,线性关系良好;检出限为0.051~3.864 ng/L;14种目标物回收率低于70%,采用前置标准系列抵消回收影响,线性相关系数R^(2)>0.99;其余45种目标物回收率为74.7%~111%。该方法可应用于饮用水及水源水中超痕量多类型农药残留的同时测定。A method has been developed for the simultaneous determination of 59 kinds of pesticide residues in 4 major categories and 15 subcategories,including herbicides,insecticides,fungicides,and plant growth regulators,in water samples by gas chromatography-tandem mass spectrometry with automated solid-phase extraction.The targets in water samples were purified and enriched by HLB solid-phase extraction column,separated by HP-5MS capillary column,and subjected to mass spectrometry analysis using a multi reaction monitoring mode.Matrix matching standard solutions improved by analytical protectant were carried out for quantification with heptachlor epoxideas internal standard.The results showed that the linear ranges of 5 amino acid esters were 4-80 ng/mL,6-120 ng/mL,and 15-300 ng/mL,that of 8 isomers of HCH and DDT were 5-100 ng/mL,while that of other 46 target compounds were 10-200 ng/mL.59 target compounds showed good linear relationships,and the detection limits of these 59 target compounds were 0.051-3.864 ng/L.Due to the recoveries of 14 pesticide residues being below 70%,a pre-standard series were used to offset the recovery effects,and the correlation coefficients(R^(2))were better than 0.99.The recoveries of the remaining 45 target compounds were between 74.7%and 111%.This method can be applied for the simultaneous determination of multiple types of pesticide residues at ultra-trace level in drinking water and source water.

关 键 词：农药残留 气相色谱-串联质谱法 饮用水 固相萃取 分析保护剂 内标 

分 类 号：O657.63[理学—分析化学] R123.1[理学—化学]