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

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4.5 μg/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.

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

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 than 10％,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.