Hemmersbach P, de la Torre R
Hormone Laboratory, Aker Hospital, Oslo, Norway.
J Chromatogr B Biomed Appl. 1996 Dec 6;687(1):221-38. doi: 10.1016/s0378-4347(96)00276-9.
More than 25 years of developing doping control methods have led to comprehensive screening and confirmation procedures for stimulants, narcotics and beta-blockers. Much of this work has been initiated and/or improved by the late Prof. Dr. Manfred Donike. The methodological approach covered in this overview was applied to doping control procedures during the XXV Summer Olympics in Barcelona, Spain, in 1992 and the XVII Winter Olympics in Lillehammer, Norway, in 1994. Urine samples are screened through a combination of two analytical methods that are complementary: (a) gas chromatographic analysis of the parent compound and unconjugated metabolites, following single-step sample extraction and detection by a nitrogen-specific detector based on a retention index identification system and (b) gas chromatographic analysis including also conjugated drugs and metabolites after hydrolysis, solid-phase extraction, derivatisation and mass spectrometric detection. Confirmation and identification is always performed by gas chromatographic separation and full scan mass spectrometric detection. These methods facilitate the rapid screening and confirmation of more than 100 stimulants, narcotic analgesics and beta-blockers in urine for at least 24 h after the intake of a pharmaceutical dose. Application of the methods ensures high quality standards for the unequivocal identification of doping agents as well as a rapid turnaround time for sample analyses.
25 年多来兴奋剂检测方法的发展已形成了针对兴奋剂、麻醉药品和β-受体阻滞剂的全面筛查与确证程序。这项工作的大部分是由已故的曼弗雷德·多尼克教授发起和/或改进的。本综述中涵盖的方法学途径应用于 1992 年在西班牙巴塞罗那举行的第 25 届夏季奥运会和 1994 年在挪威利勒哈默尔举行的第 17 届冬季奥运会的兴奋剂检测程序。尿液样本通过两种互补的分析方法进行筛查:(a) 对母体化合物和未结合代谢物进行气相色谱分析,采用单步样品萃取,并通过基于保留指数识别系统的氮特异性检测器进行检测;(b) 气相色谱分析,包括水解、固相萃取、衍生化和质谱检测后的结合药物和代谢物。确证和鉴定始终通过气相色谱分离和全扫描质谱检测进行。这些方法有助于在服用药物剂量后至少 24 小时内对尿液中 100 多种兴奋剂、麻醉性镇痛药和β-受体阻滞剂进行快速筛查和确证。这些方法的应用确保了明确鉴定兴奋剂的高质量标准以及样本分析的快速周转时间。