Determination of Fipronil and Its Metabolites in Fresh Jujube by Low Temperature Liquid-Liquid Extraction/Ultra High Liquid Chromatography-Tandem Mass Spectrometry
LIN Tao,FAN Jian-lin,YANG Dong-shun,LIU Xing-yong,SHAO Jin-liang,LI Yan-gang,LIU Hong-cheng*
1.云南省农业科学院质量标准与检测技术研究所;2.农业部农产品质量安全风险评估实验室（昆明）
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Abstract:
An analytical method for the qualitative and quantitative analyses of fipronil and its metabolites residues in fresh jujube was developed by using low temperature liquid-liquid extraction and ultra high liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）. The fresh jujube sample was extracted with acetonitrile，followed by liquid-liquid extraction at -25 ℃. The analysis of fipronil and its metabolites was performed under negative ion mode and multiple reaction monitoring(MRM),quantified by the external standard method. Under the optimized conditions，the fipronil and its metabolites showed good linearities in the range of 0.02 - 10 μg/L，with correlation coefficients(r2) higher than 0.999. The limits of detection of the method were in the range of 0.005-0.02 μg/kg. The average recoveries of fipronil and its metabolites in fresh jujube matrices were in the range of 78.5%-95.8% with relative standard deviations of 3.4%-6.9%. The method is simple and highly sensitive，and is suitable for the rapid determination of fipronil and its metabolites in fresh jujube.