基于气相色谱-静电场轨道阱高分辨质谱法快速筛查和确证农产品中222种农药残留  

Rapid Screening and Confirmation of 222 Pesticide Residues in Agricultural Products by Gas Chromatography-Electrostatic Field Orbitrap High Resolution Mass Spectrometry

作　　者：殷雪琰 朱佳明 堵燕钰 王洁琼 翟云忠 YIN Xue-yan;ZHU Jia-ming;DU Yan-yu;WANG Jie-qiong;ZHAI Yun-zhong(Agricultural Products Quality Safety Center of Changzhou,Changzhou 213002,China)

机构地区：[1]常州市农产品质量安全中心,江苏常州213002

出　　处：《分析测试学报》2022年第2期172-186,共15页Journal of Instrumental Analysis

基　　金：常州市现代农产业体系项目(2020034)。

摘　　要：该文在QuEChERS方法的基础上采用固相分散萃取样品处理一体机(Sio-dSPE)对样品进行前处理,结合气相色谱-静电场轨道阱高分辨质谱法(GC-Orbitrap MS)对农产品中多农药残留进行筛查和确证。对Sio-dSPE前处理方法中盐析剂和除水剂的种类、净化剂的种类与用量、基质效应等进行考察。在最优条件下,采用GC-Orbitrap MS对农产品中222种农药残留进行检测,线性范围为1~200μg/L,在莴苣、大米和茶叶中的定量下限分别为0.5~5μg/kg、1~10μg/kg、2.5~25μg/kg。在上述3种基质中分别进行10、20、50μg/kg浓度水平的加标回收实验,测得回收率分别为70.5%~121%、70.2%~119%、65.2%~125%,相对标准偏差(RSD)分别不大于11%、10%、12%。该方法具有样品处理简单、分析时间短、净化效果好等优点,适用于农产品中多农药残留的快速筛查与定量。A gas chromatography-electrostatic field orbitrap high resolution mass spectrometry(GC-Orbitrap MS)was developed for the rapid screening and confirmation of 222 kinds of pesticide residues in agricultural products,based on Qu ECh ERS method.The samples were preprocessed with an integrated solid phase dispersion extraction sample processing machine(Sio-d SPE).Experimental conditions including types of salting-out agent and water removal agent,type of cleaning agent and its amount,matrix effect were investigated and optimized in detail.Under the optimized conditions,the linear ranges of 222 pesticides were in the range of 1-200μg/L,the average recoveries for 222 pesticide residues in lettuce,rice and tea samples at three spiked levels of 10,20 and 50μg/kg were in the ranges of 70.5%-121%,70.2%-119%and 65.2%-125%,with their relative standard deviations(RSDs)not more than 11%,10%and 12%,respectively.The limits of quantitation(LOQs)of this method for lettuce,rice and tea were 0.5-5μg/kg,1-10μg/kg and 2.5-25μg/kg,respectively.With the advantages of simplicity,easy pretreatment and high purifying efficiency,the method was suitable for the fast screening and confirmation of pesticide residues in agricultural products.

关 键 词：气相色谱-静电场轨道阱高分辨质谱法(GC-Orbitrap MS) 固相分散萃取样品处理一体机法(Sio-dSPE) 快速筛查和确证 多农药残留 农产品 

分 类 号：O657.3[理学—分析化学] O614.243[理学—化学]