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目的:本实验基于液相色谱-串联质谱(LC-MS/MS)技术和简单的样品前处理过程,建立迅速、准确定性检测人尿中多种违禁药物的方法,包括以下8种药物:雄1,4,6-三烯-3,17-二酮(androst-1,4,6-trien-3,17-dione)、勃拉睾酮(bolasterone)、氧雄龙(oxandrolone)、4-羟基睾酮(4-hydroxytestosterone)、表甲雄二醇(epimetnandiol)、2-(4-((2-(4-(三氟甲基)苯基)-5-甲基噻唑-4-基)甲基硫基)-2-甲基苯氧基)乙酸(GW501516)、甲基司腾勃龙(methylstenbolone)、S-3-(4-乙酰氨基)-2-羟基-2-甲基-N-(4-硝基-3-三氟甲基苯基)丙酰胺(o-dephenylostarine)。方法:采用液相色谱串接质谱、Zorbax XDB-C18色谱柱;尿样经液液萃取后上样分析。结果:筛查药物最低检测限在0.5~2 ng/ml之间,回收率均高于50%,日内精密度、日间精密度均低于20%。稳健度均低于15%。结论:本工作对样品前处理方法、质谱条件等方面进行了优化,建立同时检测这8种化合物的液相色谱-串联质谱方法。采用该方法检测这8种药物,能达到世界反兴奋剂机构技术文件对最低检测下限及日内、日间精密度的要求,保证本实验室能够通过世界反兴奋剂机构(WADA)每季度水平考试,从而保证本实验室具有检测国际比赛样品的资格。
OBJECTIVE: To establish a rapid and accurate method for the qualitative and quantitative detection of various illicit drugs in human urine based on liquid chromatography-tandem mass spectrometry (LC-MS / MS) and simple sample preparation, including the following eight drugs: male Androst-1,4,6-trien-3,17-dione, bolasterone, oxandrolone, 4-hydroxy 4-hydroxytestosterone, epimetnandiol, 2- (4- ((2- (4- (trifluoromethyl) phenyl) -5-methylthiazol- Methyl) -2- methylphenoxy) acetic acid (GW501516), methylstenbolone, S-3- (4-acetamido) -2- hydroxy-2-methyl-N- -nitro-3-trifluoromethylphenyl) propionamide (o-dephenylostarine). Methods: Zorbax XDB-C18 column was used for liquid chromatography tandem mass spectrometry. The urine samples were analyzed by liquid-liquid extraction. Results: The minimum detection limit of screening drugs was between 0.5-2 ng / ml, the recovery rates were higher than 50%. The intra-day precision and intra-day precision were less than 20%. Robustness is less than 15%. Conclusion: In this work, the methods of sample preparation and mass spectrometry were optimized, and the simultaneous determination of eight compounds by liquid chromatography-tandem mass spectrometry was established. Using this method for the detection of these 8 drugs, the WADA Technical Documents meet the minimum and maximum daily and intraday precision requirements, ensuring that our labs pass the World Anti-Doping Agency (WADA) Quarterly Proficiency Test , So as to ensure that the laboratory has the qualifications to test samples of international competitions.