关键词：
快速滤过型净化;氟虫腈及其代谢物;超高效液相色谱-串联质谱;茶叶
摘 要：
建立了快速滤过型净化(m-PFC)结合超高效色谱-串联质谱(UPLC-MS/MS)同时检测茶叶中氟虫腈及其代谢物残留量农药残留的方法.样品加水浸润后经过乙酸乙腈均质提取,QuEChERS盐包分层,取上层提取液经m-PFC柱净化,液相色谱-质谱联用仪测定.质谱采用电喷雾负离子模式(ESI-)和多反应监测模式(MRM)进行分析,基质外标法定量.结果表明:氟虫腈及其代谢物在 1.00~100 μg/L范围内线性关系良好,线性相关系数均>0.999,定量限为 5 μg/kg,检出限为 1.2~1.8 μg/kg.在 5.00~500 μg/kg添加水平范围内,回收率为 76.4%~104.1%,相对标准偏差(RSD)为 2.7%~6.4%.该方法具有操作简便、灵敏度高、准确度良好等优点,可适用于大批量茶叶中氟虫腈及其代谢物的快速定量检测.
译 名：
Determination of Fipronil and Its Metabolites Residue in Tea by Multi-Plug Filtration Purification Cleanup Method Combined With Ultra Performance Liquid Chromatography-tandem Mass Spectrometry
关键词：
multi-plug filtration cleanup(m-PFC)%fipronil and its metabolites%UPLC-MS/MS%tea
摘 要：
A method for the determination of fipronil and its metabolites pesticide residues in tea was established by multi-plug filtration cleanup(m-PFC)method combined with Ultra Perform-ance Liquid Chromatography-tandem Mass Spectrometry(UPLC-MS/MS).The samples were ex-tracted with acetic acid acetonitrile after being thorough wetted with water.QuEChERS salt packs were introduced into the system to separate the organic and aqueous phases.Subsequently,the up-per fraction was purified on an m-PFC column before analysis by UPLC-MS/MS.The target pesti-cide residues were determined by multiple reaction monitoring(MRM)mode with negative electros-pray ionization(ESI-),and quantified by the matrix-matched external standard method.The re-sults showed a robust linearity for fipronil and its metabolites within the range of 1.00~100 μg/L,with correlation coefficients higher than 0.999.The detection limits were in the range of 1.2~1.8 μg/kg,and the quantitation limit was 5.0 μg/kg.At the addition level of 5.00~100 μg/kg,the recoveries ranged from 76.4%to 104.1%,with relative standard deviations(RSDs)of 2.7%~6.4%(n=3).The proposed method is simple,rapid,sensitive and reproducible,making it suit-able for the simultaneous determination of fipronil and its metabolites pesticide residues in a large quantity of tea.
