QuChERS在线凝胶色谱-气相色谱/质谱联用法测定水果蔬菜中氟虫腈农药残留  

Determination of Fipronil in Vegetables and Fruits by Qu ECh ERS-online Gel Permeation Chromatography Coupled with Gas Chromatography-mass Spectrometry

作　　者：胡贵祥[1] 夏祥[1] 朱惠芳[1] 

机构地区：[1]南昌市疾病预防控制中心,江西南昌330038

出　　处：《化学试剂》2017年第5期509-512,共4页Chemical Reagents

基　　金：江西省卫计委科技计划资助项目(20162009)

摘　　要：建立了在线凝胶色谱-气相色谱/质谱(GPC-GC/MS)联用法测定水果蔬菜中氟虫腈的残留。采用QuEChERS法对样品进行净化处理,即乙腈为提取液、无水硫酸钠和N-丙基乙二胺(PSA)为净化剂去除基质干扰,以在线GPC-GC/MS系统进样分析,采用负化学源电离,SIM方式定量检测。回收率为86.0%~108.1%,相对标准偏差(RSD)<10%,方法的检出限(LOD)和定量限(LOQ)分别为1.5和4.5μg/kg,已用于水果、蔬菜等220份样品的检测。该方法前处理简单快速、灵敏度高,适应于水果蔬菜中氟虫腈的检测。Fipronil residues in vegetables and fruits were determined by online GPC-GC/MS. The sample was cleaned up by QuEChERS,extracted with acetonitrile,removed chromatographic interferences by Na2SO4 and PSA,then analyzed by online GPCGC/MS with NCI,quantitated by SIM. The recovery rate was 86. 0% ～ 108. 1%,and the relative standard deviation was less than10%,the limits of detection（ LOD） was 1. 5 μg/kg,while the limits of quantification（ LOQ） was 4. 5 μg/kg. The method is simple,convenient,highly sensitive and satisfied for detection of fipronil residues in vegetables and fruits.

关 键 词：氟虫腈 QUECHERS 凝胶色谱气质联用 负化学源电离 

分 类 号：O657.63[理学—分析化学]