QuEChERS/高效液相色谱串联质谱法测定渔业饲料中敌百虫、敌敌畏、蝇毒磷的含量  

Simultaneous determination of trichlorfon, dichlorvos and coumaphos residues in fisheryfeed by QuEChERS/high performance liquid chromatography-tandem mass spectrometry

作　　者：肖维[1] 万译文[1] 伍远安 杨霄[1] 索纹纹[1] XIAO Wei;WAN Yiwen;WU Yuanan;YANG Xiao;SUO Wenwen(Hunan Fisheries Science Institute,Changsha,Hunan Province 410153,China;Collaborative Innovation Center for Efficient and Health Production of Fisheries in Hunan Province,Changde,Hunan Province 415000,China)

机构地区：[1]湖南省水产科学研究所,湖南长沙410153 [2]水产健康生产湖南省协同创新中心,湖南常德415000

出　　处：《中国饲料》2018年第23期68-71,共4页China Feed

基　　金：湖南省科技重大专项资金(2017NK1030);湖南省农业科技创新资金(2017XC02)

摘　　要：本文建立了一种简单、快速测定渔业饲料中敌百虫、敌敌畏、蝇毒磷的QuEChERS-液相色谱串联质谱分析方法。样品经酸化乙腈提取,C18与中性氧化铝净化后,采用HPLC-MS/MS选择反应监测(SRM)正离子模式测定进行定性、定量分析。结果表明:在2.0～200 ng/mL范围内,峰面积与浓度线性良好,相关系数均大于0.9992;方法的检出限(LOD)为2.0μg/kg,定量限(LOQ)为4.0μg/kg,检测结果的相对标准偏差为1.62%～8.68%(n=6),平均加标回收率82.3%～105.2%。该方法具有较高的重现性和选择性,适用于渔业饲料中敌百虫、敌敌畏、蝇毒磷的残留分析检测。A simple and quick analysis method was established for the determination of trichlorfon,dichlorvos and coumaphos residues in fishery feed by QuEChERS/liquid chromatography-tandem mass spectrometry.The sample was extracted with acetonitrile and cleaned by with C18 and Alumina-N.The mass spectrometer was operated in the positive ion mode using selected reaction monitoring for the qualitative and quantitative analysis.The external standard calibration curvers were used for the quantification.The linear ranges were from 2.0 to 200 ng/mL with a good linear relationship(R2> 0.9992).The detection limits of this method was 2.0 μg/kg, and the limits of quantification was 4.0 μg/kg.The relative standard deviations ranging from1.62% ~ 8.68%(n=6) and the average recovery rates were from 82.3% ~ 105.2%.The method was suitable for the identification and quantification of trichlorfon, dichlorvos and coumaphos residues in fishery feed due to higher producibility and selectivity.

关 键 词：QUECHERS 液相色谱-质谱/质谱法 敌百虫 敌敌畏 蝇毒磷 渔业饲料 

分 类 号：S816.17[农业科学—饲料科学]