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高效液相色谱-串联质谱法同时测定动物尿液中48种兴奋剂
贾寒冰,冯瑞雪,王苑桃,何亚琴,董曼曼,李敏,梁红月,张亚锋
0
(西安市食品药品检验所)
摘要:
建立了高效液相色谱-串联质谱(HPLC-MS/MS)法同时检测动物尿液中中β-受体激动剂类、利尿剂类、糖皮质激素类、蛋白同化制剂类等48种兴奋剂的检测方法。样品经1%甲酸乙腈提取,加氯化钠使其分层后,40℃下氮气吹干,乙腈水溶液(V/V,5:5,含0.1%甲酸)复溶,采用C18色谱柱分离,用电喷雾正(ESI+)负(ESI-)模式扫描,多反应监测模式(MRM)进行检测分析,单点内标或外标法进行定量。克仑特罗等48种兴奋剂能实现很好的分离,重复性良好,加标水平为定量限时,目标化合物的回收率在60%~120%之间,相对标准偏差为1.0% ~ 19.3%。该方法简单、快速、准确,极大地提高了检测效率,已应用于实验室常规兴奋剂检测,为保障体育赛事的顺利进行提供了有力的技术支撑。
关键词:  高效液相色谱-串联质谱(HPLC-MS/MS)  动物尿液  兴奋剂
DOI:
投稿时间:2023-09-12修订日期:2024-06-03
基金项目:陕西省市场监督管理局科技计划项目(2021KY14),陕西省创新能力支撑计划(2021PT-044),陕西省市场监督管理局科技计划项目(2023KY17),陕西省市场监督管理局科技计划项目(2022KY13)
Simultaneous Detection of 48 Doping Agents in Animal Urine by High Performance Liquid Chromatography - tandem Mass Spectrometry
(Xi''an Institute for Food and Drug Control)
Abstract:
A high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was established for the simultaneous detection of 48 stimulants such as β-receptor agonists, diuretics, glucocorticoids, and anabolic agents in animal urine. The sample was extracted with 1% formic acid acetonitrile, added sodium chloride to make the layers, dried under nitrogen at 40°C, redissolved in acetonitrile aqueous solution (V/V, 5:5, containing 0.1% formic acid), and separated by C18 chromatographic column. 48 kinds of stimulants such as Clenbuterol can achieve good separation and good repeatability. When the spiked level is the limit of quantification, the recovery rate of the target compound is between 60% and 120%, and the relative standard deviation is 1.0% to 19.3%. The method is simple, fast and accurate, which greatly improves the detection efficiency. It has been applied to routine doping detection in laboratories, and provides strong technical support for ensuring the smooth progress of sports events.
Key words:  High performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)  Animal urine  Doping

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