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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%。
Gas chromatography - high resolution mass spectrometry was used to establish a method for the determination of 21 doping agents in human urine including nandrolone, coumarone and meropenem. Samples were subjected to liquid-liquid extraction, concentration and trimethylsilylation derivatization. 21 kinds of stimulants were simultaneously detected by gas chromatography / high resolution mass spectrometry and multi-ion detection (MID). The method was validated by the WADA accredited laboratory method. The detection limit was ng.mL-1. The recoveries ranged from 66% to 103% (n = 6). The recoveries The relative standard deviations (RSDs) were less than 10.0%. The precision test of quantitative detection of samples at three different concentrations was carried out. The results showed that the RSDs of precision were lower than 9.5%, 10.0% and 9.7% respectively.