| 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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| 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) |
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| 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0005~04 mg/L范围内线性关系良好，方法检出限(LOD)为0005~01 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502%~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) |
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| Simultaneous Determination of 508 Pesticide Residues in Panax notoginseng by Liquid Chromatography-Tandem Mass Spectrometry |
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| 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 0005-04 mg/L with limits of detection(LOD) of 0005-01 mg/kg.Except for 8 pesticides,the recoveries for other 500 pesticides at spiked level of 100 μg/kg were in the range of 502%-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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