QuEChERS联合LC-MS/MS测定土壤及蚯蚓中吡虫啉及异丙甲草胺13种代谢产物  

Determination of 13 Metabolites of Imidacloprid and Metolachlor in Soil and Earthworm by QuEChERS Combined with LC-MS/MS

作　　者：符芙蓉 赵丽霞 李晓晶 叶会科 孙扬 李永涛[2] FU Fu-rong;ZHAO Li-xia;LI Xiao-jing;YE Hui-ke;SUN Yang;LI Yong-tao(Agro-Environmental Protection Institute,Ministry of Agriculture and Rural Affairs,Tianjin 300191,China;College of Natural Resources and Environment,South China Agricultural University,Guangzhou 510642,China)

机构地区：[1]农业农村部环境保护科研监测所,天津300191 [2]华南农业大学资源环境学院,广东广州510642

出　　处：《化学试剂》2023年第7期136-143,共8页Chemical Reagents

基　　金：青海省科技计划项目(2019-NK-A11);国家自然科学基金面上项目(42177034)。

摘　　要：建立土壤及蚯蚓基质中吡虫啉及异丙甲草胺两种农药的13种代谢产物分析测试方法。通过筛选提取溶剂的种类、净化方式,优化高效液相色谱及质谱条件建立了QuEChERS联合LC-MS/MS的处理及测定方法。该方法使用含1%甲酸的乙腈溶液提取土壤及蚯蚓中两种常见农药的13种代谢物,以稀释2倍的方式削弱土壤浸提液中的基质效应、以稀释3.2倍及添加PSA、GCB、C18的方式净化蚯蚓浸提液。在土壤介质中,方法的平均回收率为68.0%~114.8%,相对标准偏差为1.3%~10.7%,检出限范围为0.008 6~0.40μg/kg,定量限为0.029~2.00μg/kg。蚯蚓介质中,方法的平均回收率为67.1%~93.8%,相对标准偏差为2.0%~7.8%,检出限为0.11~5.00μg/kg,定量限为0.36~25.0μg/kg。本研究方法相对简便高效、检出限低、稳定性高,适于科学实验和田间实际土壤及蚯蚓样品中吡虫啉及异丙甲草胺代谢产物的定性、定量分析。To determine 13 metabolites of imidacloprid and metolachlor in soil and earthworm,a method was established by adjusting the conditions of liquid phase chromatography and mass spectrometry,optimizing the types of extraction solvents and purification methods.The method used acetonitrile containing 1%formic acid to extract 13 metabolites from soil and earthworm,weakened the matrix effect of soil extract by diluting 2 times,and purified earthworm extract by diluting 3.2 times and adding PSA,GCB and C18.In soil matrix,the average recovery of the method was 68.0%~114.8%with RSD as 1.3%~10.7%,the limit of detection at 0.0086~0.40μg/kg,and the limit of quantitation at 0.029~2.00μg/kg.In earthworm matrix,the average recovery of the method was 67.1%~93.8%with RSD as 2.0%~7.8%,the limit of detection as 0.11~5.00μg/kg,and the limit of quantitation at 0.36~25.0μg/kg.The method is simple,efficient,sensitive and stable and is suitable for the qualitative and quantitative analysis of metabolites of imidacloprid and metolachlor in soil and earthworm samples from scientific experiments and actual field.

关 键 词：土壤 蚯蚓 吡虫啉 异丙甲草胺 代谢物 QUECHERS LC-MS/MS 

分 类 号：R917[医药卫生—药物分析学]