食品科学 ›› 2019, Vol. 40 ›› Issue (2): 318-323.doi: 10.7506/spkx1002-6630-20170830-359

• 安全检测 • 上一篇    下一篇

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

郝杰1,邵瑞婷1,姜洁1,*,贺小蔚2   

  1. (1.北京市食品安全监控和风险评估中心,北京 100041;2.沃特世科技有限公司,北京 100026)
  • 出版日期:2019-01-25 发布日期:2019-01-22
  • 基金资助:
    北京市科技计划重大项目(D151100003815002)

Determination of Fipronil and Its Metabolites Residues in Chicken Meat and Eggs by QuEChERS-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

HAO Jie1, SHAO Ruiting1, JIANG Jie1,*, HE Xiaowei2   

  1. (1. Beijing Municipal Center for Food Safety Monitoring, Beijing 100041, China;2. Waters Technology Co. Ltd., Beijing 100026, China)
  • Online:2019-01-25 Published:2019-01-22

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?C18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1?μg/kg,在1~100?μg/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。

关键词: 氟虫腈, 动物源性食品, 超高效液相色谱-质谱联用法

Abstract: 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 C18 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.

Key words: fipronil, animal-derived foods, QuEChERS, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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