Rapid determination of fipronil and its metabolites in egg and chicken by QuEChERS-solid phase extraction-high performance liquid chromatography-tandem mass spectrometry
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(1.Tianjin Center for Disease Control and Prevention, Tianjin 300011, China;2.Tianjin Hexi District Center for Disease Control and Prevention,Tianjin 300201,China)

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    Abstract:

    Objective To develop a method for determination of fipronil and its metabolites in egg and chicken by QuEChERS-solid phase extraction(SPE)-high performance liquid chromatography-tandem mass spectrometry. Methods Egg and chicken samples were extracted by water-acetonitrile, the organic phase were salted out by QuEChERS,then cleaned up by SPE, loaded on a shimadzu XR-ODS column (50 mm×3.0 mm, 2.0 μm). Acetonitrile-water was used as the mobile phase gradient elution with negative ion spray mode ionization and multi-reactive ion monitoring (MRM) method for qualitative and quantitative detection. Results The matrix-matched calibration curve of fipronil and its metabites showed a good linear within the concentration range from 0.5 to 20.0 μg/L(r>0.999 2), the average recovery of fipronil and its metabolites at the spiked levels of 0.5,2.0 and 10.0 μg/kg was from 84.1%to 105.2%,and the relative standard deviation (RSD) was between 1.3% and 6.1%.The detection limits of fipronil, fipronil sulfone, fipronil sulfide, fluoronitrile were 0.2,0.05,0.05,0.05 μg/kg, respectively. Conclusion The method is simple rapid, highly sensitive and accurate. It is suitable for the detection of fipronil and its metabolites in egg and chicken.

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XIA Yi-ping, YIN Xiao-bing, LIN Xiao-hui, TIAN Yang-guang. Rapid determination of fipronil and its metabolites in egg and chicken by QuEChERS-solid phase extraction-high performance liquid chromatography-tandem mass spectrometry[J].中国食品卫生杂志,2018,30(4):395-400.

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  • Received:February 09,2018
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  • Online: August 16,2018
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