Determination of nitroimidazoles and their metabolites in milk by ultra-high performance liquid chromatography-tandem mass spectrometry
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(1.Key Laboratory of Health Risk Factors for Seafood of Zhejiang Province,Zhoushan Municipal District Center for Disease Control and Prevention,Zhejiang Zhoushan 316021,China;2.Daishan Center for Disease Control and Prevention,Zhejiang Zhoushan 316200,China)

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    Abstract:

    Objective A method for the quantitative analysis of eight kinds of nitroimidazoles and their metabolites in milk by ultra-performance liquid chromatography-tandem mass spectrometry coupled with simple protein precipitation was established. Methods One gram milk sample was precipitated by trichloroacetic acid, and then stratified by high-speed centrifugation. The middle layer of the supernatant was filtered through a hydrophilic polytetrafluoroethylene membrane. The analytes were separated on a Hypersil GOLD C18 column (100 mm×2.1 mm, 1.9 μm), and detected in selected reaction monitoring (SRM) mode via positive electrospray ionization. The matrix matching and internal standard method was used for quantification. Results The nitroimidazoles and their metabolites showed good linearity in the range of 0.3-10.0 ng/ml, and correlation coefficients were above 0.998 5. The limits of detection of the nitroimidazoles and their metabolites in milk were between 0.1 and 0.2 μg/kg. The recoveries at spiked levels of 0.5,2.0 and 5.0 μg/kg were within 83.6%-111.8%, the intra-day relative standard deviation(RSD)were within 2.7%-9.1%, and the inter-day RSD were within 1.0%-9.3%. Conclusion The method was accurate, fast, cheap, easy, and could satisfy the requirements of high-throughput monitoring nitroimidazoles in milk.

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FANG Li, QIU Fengmei, YU Xingwei, ZHANG Zhichao. Determination of nitroimidazoles and their metabolites in milk by ultra-high performance liquid chromatography-tandem mass spectrometry[J].中国食品卫生杂志,2019,31(1):17-22.

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  • Received:January 08,2019
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  • Online: March 22,2019
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