液相色谱串联质谱法测定植物食品中氟虫腈及其代谢物的残留量

Determination of Fipronil and Its Metabolite Residues in Plant Food by Liquid Chromatography Tandem Mass Spectrometry

目前,液相色谱串联质谱法检测植物源食品中氟虫腈及其代谢物的普适检测标准较少、适用范围较窄,为满足日常大批量检测工作,本实验建立了液相色谱串联质谱法分析植物食品中氟虫腈及其代谢物残留量的检测方法,拓展了检测适用范围。样品由乙腈提取,经净化包(50 mg PSA、50 mg C18、150 mg MgSO4)净化,采用C18色谱柱分离,液相色谱串联质谱电喷雾负离子(ESI-)模式下以MRM反应监测,外标法定量。并利用该方法对7种代表作物定量限加标回收率均在87.0%~114.6%,结果表明该方法样品前处理过程简单,净化效果好,能满足日常大批量样品检测的实际需求。

At present,the universal standard for the detection of fipronil and its metabolites in vegetative foods by liquid chromatography tandem mass spectrometry is less and the scope of application is narrow.In order to meet the daily mass detection work,a method was developed for the determination of fipronil and its metabolites residues in vegetative foods by liquid chromatography tandem mass spectrometry,and the scope of application was expanded.The samples were extracted by acetonitrile and purified by purification package(50 mg PSA、50 mg C18、150 mg MgSO4).The samples were separated by C18 chromatographic column,and detected by liquid chromatography tandem mass spectrometry MRM reaction monitoring under electrospray negative ion(ESI-)mode.The analyte was quantified by matrix-matched external standard legal method.By using this method,the average recoveries rages from 87.0%~114.6%.The results show that the pretreatment process of the method is simple,the purification effect is good,and which can meet the actual demand of daily mass sample detection.