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当前位置: 首页 > 文章 > QuEChERS-超高效液相色谱-串联质谱法测定鸡蛋、鸡肉中氟虫腈及其代谢物残留 食品科学 2019 (2) 318-323
Position: Home > Articles > Determination of Fipronil and Its Metabolites Residues in Chicken Meat and Eggs by QuEChERS-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry FOOD SCIENCE 2019 (2) 318-323

QuEChERS-超高效液相色谱-串联质谱法测定鸡蛋、鸡肉中氟虫腈及其代谢物残留

作  者：
郝杰;邵瑞婷;姜洁;贺小蔚
单  位：
北京市食品安全监控和风险评估中心;沃特世科技有限公司
关键词：
氟虫腈;动物源性食品;超高效液相色谱-质谱联用法
摘  要：
建立一种基于QuEChERS法提取,超高效液相色谱分离,串联四极杆质谱法检测鸡蛋、鸡肉中氟虫腈及其代谢物残留量的方法。样品经加水分散后,用乙腈提取,柠檬酸缓冲盐脱水,稀释后上机测定。待测物经BEH C_(18)色谱柱分离,以甲醇-5 mmol/L乙酸铵溶液(含0.1%甲酸)进行梯度洗脱,质谱法采用电喷雾电离,负离子多反应监测模式检测。基质加标曲线定量。氟虫腈及3种代谢物的定量限为1μg/kg,在1～100μg/kg范围内线性关系良好。在鸡蛋、鸡肉基质中3个不同添加水平下,平均回收率为87.6%～117.7%,变异系数为3.6%～9.9%。该方法快速、灵敏、准确,适合作为禽蛋等动物源性食品中,氟虫腈及其代谢物残留总量的测定。
译  名：
Determination of Fipronil and Its Metabolites Residues in Chicken Meat and Eggs by QuEChERS-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
作  者：
HAO Jie;SHAO Ruiting;JIANG Jie;HE Xiaowei;Beijing Municipal Center for Food Safety Monitoring;Waters Technology Co.Ltd.;
单  位：
HAO Jie%SHAO Ruiting%JIANG Jie%HE Xiaowei%Beijing Municipal Center for Food Safety Monitoring%Waters Technology Co.Ltd.
关键词：
fipronil;;animal-derived foods;;QuEChERS;;ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)
摘  要：
A method for the determination of fipronil and its metabolites residues in chicken eggs and meat by quick easy cheap effective rugged safe (QuEChERS) extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established. Samples were dispersed in water and extracted with acetonitrile, followed by dehydration with citrate buffer. The extract was diluted before being injected. The analytes were separated on a BEH C_(18) column with gradient elution using a mobile phase made up of methanol and 5 mmol/L ammonium acetate (containing 0.1% formic acid). The MS analysis was performed using an electrospray ionization (ESI) source in the negative mode with multiple reaction monitoring (MRM). Quantification was performed with matrix-matched standard calibration curves. The limits of quantitation (LOQs) of fipronil and 3 metabolites were all 1 μg/kg. In the concentration range of 1 to 100 μg/kg, all the calibration curves showed good linear correlation. The average recoveries for chicken egg and meat at three different spiked levels were 87.6%–117.7%, with relative standard deviations (RSDs) between 3.6% and 9.9%. The method is rapid, sensitive and accurate, and it is suitable for the determination of fipronil and its metabolites residues in animal-derived food s such as chicken eggs and meat.

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