超高效液相色谱-串联质谱法检测牛奶中硝基咪唑类药物及其代谢物残留
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(1.舟山市疾病预防控制中心 浙江省海产品健康危害因素关键技术研究重点实验室,浙江 舟山 316021;2.岱山县疾病预防控制中心,浙江 舟山 316200)

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方力 男 工程师 研究方向为理化检验E-mail:fangli123@126.com

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基金项目:

舟山市科技计划项目(2017B31127);舟山市医药卫生科技计划项目(2017A01)


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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    摘要:

    目的 建立三氯乙酸诱导蛋白沉淀净化-超高效液相色谱-串联质谱快速定量检测牛奶中8种硝基咪唑类药物及其代谢物的方法。方法 牛奶样品经三氯乙酸蛋白沉淀后高速离心分层,中间层清液过0.22 μm聚四氟乙烯滤膜,Hypersil GOLD C18柱(100 mm×2.1 mm, 1.9 μm)分离,电喷雾离子化,选择反应监测(SRM)模式检测,基质匹配内标法定量。结果 在0.3~10.0 ng/ml浓度范围内,硝基咪唑类药物及其代谢物呈良好的线性关系,相关系数达到0.998 5以上;以3倍信噪比对应的浓度为检出限,方法检出限可达0.1~0.2 μg/kg;在0.5、2.0和5.0 μg/kg 的加标水平,方法回收率为83.6%~111.8%,日内相对标准偏差为2.7%~9.1%,日间相对标准偏差为1.0%~9.3%。结论 该检测方法准确、快速、高效、低成本、易操作,能满足牛奶中硝基咪唑类药物及其代谢物残留高通量检测要求。

    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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方力,邱凤梅,余新威,张志超.超高效液相色谱-串联质谱法检测牛奶中硝基咪唑类药物及其代谢物残留[J].中国食品卫生杂志,2019,31(1):17-22.

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  • 收稿日期:2019-01-08
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  • 在线发布日期: 2019-03-22
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