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
Simultaneous Detection of 48 Doping Agents in Animal Urine by High Performance Liquid Chromatography-tandem Mass Spectrometry
贾寒冰 1冯瑞雪 1王苑桃 1何亚琴 1董曼曼 1李敏 1梁红月 1张亚锋1
作者信息
- 1. 西安市食品药品检验所,西安 710100
- 折叠
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β2-激动剂类、β-阻断剂类、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.
Abstract
A high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method was established for the simultaneous detection of 48 stimulants such as β2-agonists,β-blockers,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℃,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.
关键词
高效液相色谱-串联质谱(HPLC-MS/MS)/动物尿液/兴奋剂Key words
high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)/animal urine/doping引用本文复制引用
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)
出版年
2024
国家科技期刊平台
NSTL
万方数据