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

• Safety Detection • Previous Articles     Next Articles

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

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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