液相色谱-串联质谱法同时测定三七中508种农药残留  

Simultaneous Determination of 508 Pesticide Residues in Panax notoginseng by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：苗水[1] 李雯婷[1] 陈铭[1] 周恒[1] 兰岚[1] 毛秀红[1] 季申[1] MIAO Shui;LI Wen-ting;CHEN Ming;ZHOU Heng;LAN Lan;MAO Xiu-hong;JI Shen(Shanghai Institute of Food and Drug Control,Shanghai201203,China)

机构地区：[1]上海市食品药品检验所

出　　处：《分析测试学报》2019年第7期761-774,共14页Journal of Instrumental Analysis

基　　金：上海市科学技术委员会项目(15ZR1437700);国家中医药管理局(国家中药标准化项目ZYBZH-C-GX-09);国家药典委员会项目(ZG2016-2);广西壮族自治区科学技术厅重大专项计划(2015AC05038);上海市科学技术委员会扬帆计划项目(16YF1410200)

摘　　要：采用液相色谱-串联质谱(LC-MS/MS)建立了可在20min内快速测定三七中508种农药残留的方法。样品经改良的QuEChERS方法提取,分散固相萃取法(d-SPE)净化后,在多反应监测(MRM)模式下进行LC-MS/MS分析,内标法定量。在优化实验条件下,508种农药均在0.005~0.4mg/L范围内线性关系良好,方法检出限(LOD)为0.005~0.1mg/kg;在100μg/kg加标水平下,除8种农药外,其余500种农药的回收率均在50.2%~117%之间,且相对标准偏差(RSD)均不大于15%;其中有468种农药的回收率为70%~120%。该方法样品前处理简单快速,灵敏度、准确度和精密度均符合农药多残留检测技术的要求,适用于三七中508种农药残留的快速筛查。A method was established for the determination of 508 pesticide reisdues in Panax notoginseng by liquid chromatography-tandem mass spectrometry(LC-MS/MS).The samples were extracted by modified QuEChERS method,followed by the clean-up of d-SPE extraction.The extract was determined by LC-MS/MS in multi-reaction monitoring(MRM) mode,and quantified by the internal standard method.There were linear relationships for the 508 pesticides in the range of 0.005-0.4 mg/L with limits of detection(LOD) of 0.005-0.1 mg/kg.Except for 8 pesticides,the recoveries for other 500 pesticides at spiked level of 100 μg/kg were in the range of 50.2 %-117 % with relative standard deviations(RSD) not more than 15 %,in which,the recoveries for 468 pesticides were in the range of 70 %-120 %.With the advantages of simplicity,rapidness,good sensitivity and accuracy,the method could meet the requirements for multiple pesticide residues analysis,and is suitable for the determination of 508 pesticide residues in Panax notoginseng .

关 键 词：三七 农药残留 QuEChERS方法 液相色谱-串联质谱(LC-MS/MS) 

分 类 号：O657.7[理学—分析化学] R914.1[理学—化学]