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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。
An online gel permeation chromatography-gas chromatography-mass spectrometry (GPC-GC / MS) was developed for the determination of fipronil in fruits and vegetables. The sample was purified by QuEChERS method, that is, acetonitrile as extract, anhydrous sodium sulfate and N-propyl ethylenediamine (PSA) as scavenger to remove matrix interference. The sample was analyzed by online GPC-GC / MS system. Negative chemical ionization, SIM quantitative detection. The detection limits (LOD) and limit of quantification (LOQ) of the method were 1.5 and 4.5 μg / kg, respectively, for fruits, vegetables, etc., with recoveries of 86.0% -108.1% and relative standard deviations (RSDs) Parts of the test. The method has the advantages of simple and rapid pretreatment, high sensitivity, and application to the detection of fipronil in fruits and vegetables.