QuEChERS-UPLC-MS/MS法同时检测中药材半夏中31种农药残留  

Simultaneous determination of 31 pesticide residues in Pinellia ternata by QuEChERS-UPLC-MS/MS

作　　者：宋邦燕 张海艳 龙育鋆 廖国会[1,2] 陈湘燕 秦立新[1,2] 陈明贵 朱峰[1,2] 李春萍 SONG Bangyan;ZHANG Haiyan;LONG Yujun;LIAO Guohui;CHEN Xiangyan;QIN Lixin;CHEN Minggui;ZHU Feng;LI Chunping(Institute of Plant Protection,Guizhou Academy of Agricultural Sciences,Guiyang 550006,China;Pesticide Risk Monitoring Center of Guizhou Province,Guiyang 550006,China;Guiyang Customs,Guiyang 550081,China)

机构地区：[1]贵州省农业科学院植物保护研究所,贵阳550006 [2]贵州省农药风险监测中心,贵阳550006 [3]贵阳海关,贵阳550081

出　　处：《农药》2023年第10期735-740,共6页Agrochemicals

基　　金：贵州省优秀青年科技人才计划项目,黔科合平台人才—YQK[2023]026。

摘　　要：[目的]基于经典QuEChERS前处理方法,结合超高效液相色谱串联质谱(UPLC-MS/MS)建立同时检测半夏块茎中31种农药残留分析方法。[方法]样品经乙腈提取,100 mg PSA净化,以0.1%甲酸水-甲醇为流动相进行梯度洗脱,采用UPLC-MS/MS测定,基质外标法定量。[结果]31种农药在0.01~1000μg/L范围内色谱峰面积与质量浓度呈良好线性关系,决定系数(R2)大于0.9990;在3个添加水平(LOQ、10倍LOQ、100倍LOQ)下,31种农药在半夏中的平均添加回收率为72%~115%,相对标准偏差为1.19%~13.25%(n=7)。31种农药的定量限为0.00002~0.002 mg/kg。采用所建方法对贵州省赫章县23批半夏块茎样品进行残留检测,结果显示31种农药残留范围<LOQ~0.14374mg/kg。[结论]该方法简单、快速,方法的精密度、准确度和灵敏度均满足农药残留检测分析要求,适用于半夏中31种农药残留的同时检测.[Aims]This study aims to establish an ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)method to simultaneously determine 31 pesticide residues in Pinellia ternata tuber based on the classical QuEChERS pretreatment method.[Methods]The samples were extracted with acetonitrile,purified by 100 mg PSA,eluted with gradient 0.1%formic acid aqueous solution-methanol,and detected by UPLC-MS/MS using the external matrix standard method for quantitative analysis.[Results]The linear relationship between chromatographic peak area and mass concentration for the 31 pesticides was good in the range of 0.01-1000μg/L with the determination coefficient(R2)>0.9990.The average recoveries of 31 pesticides were 72%-115%with RSD of 1.19%-13.25%(n=7)under the three spiked levels(LOQ,10×LOQ,100×LOQ).The LOQs of 31 pesticides were 0.00002-0.002 mg/kg.The method developed was used to detect the residues of 23 batches of P.ternata tuber samples from Hezhang County,Guizhou Province.The results showed that the residues of 31 pesticides ranged from<LOQ to 0.14374 mg/kg.[Conclusions]This method is simple and rapid.The precision,accuracy and sensitivity of the method meet the requirements of pesticide residue detection and analysis.Therefore,the developed method is suitable for the simultaneous detection of 31 pesticide residues in P.ternata.

关 键 词：农药 残留 半夏 QUECHERS UPLC-MS/MS 

分 类 号：TQ450.2[化学工程—农药化工]