超高效液相色谱-串联质谱法测定鱼肉中多种雄性激素和孕激素
目的 建立超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)检测鱼肉组织中10种雄性激素和孕激素的分析方法。方法 样品经乙酸铵提取, 乙酸-乙腈再提取, 无水硫酸钠吸水, QuEChERS净化, 经C18柱分离后进行UPLC-MS/MS选择电喷雾ESI正离子模式多反应监测模式下定量分析。结果 线性范围在0.4~8.0 μg/kg, 相关系数达到0.99以上, 10种激素的检出限在0.0100~0.200 μg/kg之间, 方法的回收率在77.3%~114.4%之间, 相对标准偏差在0.9%~10.3%之间。结论 该方法简单、快速、准确, 且检出限低、回收率高, 适用于鱼肉组织中雄性激素和孕激素的测定。
Objective To establish a method for the determination of 10 male hormones and progesterone in fish tissue by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Samples were extracted by ammonium acetate, then extracted with acetic acid and acetonitrile, and after the water absorbed by anhydrous sodium sulfate, the samples were purified by QuEChERS. After separation by C18 column, UPLC-MS/MS was selected for quantitative analysis by electrospray ESI positive ion mode multi-reaction monitoring mode. Results The linear range of the experiment was from 0.4 μg/kg to 8.0 μg/kg, the correlation coefficients were above 0.99, the average detection limits of 10 hormones were 0.0100–0.200 μg/kg, the recovery rates of the method were between 77.3% and 114.4%, and the relative standard deviations were between 0.9% and 10.3%. Conclusion This method is simple, rapid and accurate, and has low detection limit and high recovery rate, which is suitable for the detection of androgens and progesterones in aquatic products.
标题：超高效液相色谱-串联质谱法测定鱼肉中多种雄性激素和孕激素
英文标题：Determination of various androgens and progesterones in fish meat by ultra performance liquid chromatography-tandem mass spectrometry
作者：
李凯华 深圳市农产品质量安全检验检测中心；广东省市场监督管理局食用农产品监管重点实验室
肖曼 深圳市农产品质量安全检验检测中心；广东省市场监督管理局食用农产品监管重点实验室
张玲 深圳市农产品质量安全检验检测中心；广东省市场监督管理局食用农产品监管重点实验室
张杨 深圳市农产品质量安全检验检测中心；广东省市场监督管理局食用农产品监管重点实验室
徐媛原 深圳市农产品质量安全检验检测中心；广东省市场监督管理局食用农产品监管重点实验室
林敏霞 深圳市农产品质量安全检验检测中心；广东省市场监督管理局食用农产品监管重点实验室
张微 深圳市农产品质量安全检验检测中心；广东省市场监督管理局食用农产品监管重点实验室
钟仕花 深圳市农产品质量安全检验检测中心；广东省市场监督管理局食用农产品监管重点实验室
张兵 深圳市农产品质量安全检验检测中心；广东省市场监督管理局食用农产品监管重点实验室
中文关键词:超高效液相色谱-串联质谱法,水产品,雄性激素,孕激素,
英文关键词:ultra performance liquid chromatography tandem mass spectrometry,aquatic products,androgen,progesterone,
发表日期：2020-04-20
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