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液相色谱-串联质谱法同时测定三七中508种农药残留
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作者单位
苗水,李雯婷,陈铭,周恒,兰岚,毛秀红,季申 上海市食品药品检验所 
基金项目: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)
中文摘要:采用液相色谱-串联质谱(LC-MS/MS)建立了可在20 min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4 mg/L范围内线性关系良好,方法检出限(LOD)为0005~01 mg/kg;在100 μg/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。
中文关键词:三七  农药残留  QuEChERS方法  液相色谱-串联质谱(LC-MS/MS)
 
Simultaneous Determination of 508 Pesticide Residues in Panax notoginseng by Liquid Chromatography-Tandem Mass Spectrometry
Abstract: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.
Key Words:Panax notoginseng  pesticide residue  QuEChERS  liquid chromatography-tandem mass spectrometry(LC-MS/MS)
引用本文:苗水,李雯婷,陈铭,周恒,兰岚,毛秀红,季申.液相色谱-串联质谱法同时测定三七中508种农药残留[J].分析测试学报,2019,(7):761-774.
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