气相色谱-高分辨质谱联用法检测人尿中21种兴奋剂

Determination of doping in human urine by gas chromatography-high resolution mass spectrometry

采用气相色谱-高分辨质谱联用技术建立人尿中包括诺龙、宝丹酮、美雄酮在内的21种兴奋剂的检测方法。样品经液液萃取,浓缩,三甲基硅烷化衍生,利用气相色谱/高分辨质谱及多离子检测技术(MID)同时检测21种兴奋剂。按照世界反兴奋剂组织(WADA)认可实验室方法验证程序进行验证,该方法的检出限为ng.mL-1水平;回收率为66%～103%之间(n=6),回收率的相对标准偏差小于10.0%;对3个不同浓度下样品定量检测的精密度测试。结果表明,精密度RSD分别低于9.5%,10.0%,9.7%。

A method was evaluated for determination of twenty-one doping （including nandrolone, boldenone and methandienone） in human urine by gas chromatography-high resolution mass spectrometry. Samples were prepared by liquid-liquid extraction, concentrated, TMS derivatization and limit of detection at ng.mL-1 by MID/GC/HRMS. According to the code of the World Anti-Doping Agency （WADA）, precision and recoveries of the procedure were evaluated by replicate analysis （n = 6）, the recoveries in the range of 66%-103%, with the RSD below 10.0%. The precision within the day of the method with three different concentrations was also determined, RSD were less than 9.5%, 10.0% and 9.7%.