Solans A, Carnicero M, de la Torre R, Segura J
Department of Pharmacology and Toxicology, Universitat Autònoma de Barcelona, Spain.
J Anal Toxicol. 1995 Mar-Apr;19(2):104-14. doi: 10.1093/jat/19.2.104.
An analytical procedure for the detection of stimulants, narcotics, beta-blockers, beta-agonists, and many of their metabolites in urine using a solid-phase extraction procedure and gas chromatography-mass spectrometry (GC-MS) is described. These substances have been specifically banned by the Medical Commission of the International Olympic Committee (IOC) in order to prevent their abuse in sports. Urine samples are submitted to an enzymatic hydrolysis (beta-glucuronidase arylsulfatase) and extracted by means of Bond-Elut Certify columns. The residues are then selectively derivatized with N-methyl-N-trimethylsilyl-trifluoroacetamide (MSTFA), which enables the formation of trimethylsilyl derivatives of hydroxyl, acidic, and phenolic groups, and N-methyl-bis-trifluoroacetamide (MBTFA), which enables the formation of trifluoroacetamide derivatives of primary and secondary amines. A GC-MS system working in scan mode is sensitive and specific enough to detect and identify approximately 100 compounds and metabolites in urine for at least 24 h after the administration of doses typically encountered in therapeutics. Detection in selected ion monitoring mode is needed for the determination of beta-agonist agents. The method was successfully used in doping control of urine samples during the 25th Olympic Games, July 1992, in Barcelona, Spain.
描述了一种使用固相萃取程序和气相色谱 - 质谱联用仪（GC - MS）检测尿液中兴奋剂、麻醉药品、β - 受体阻滞剂、β - 激动剂及其许多代谢物的分析程序。国际奥委会医学委员会已明确禁止这些物质，以防止其在体育运动中被滥用。尿液样本先进行酶水解（β - 葡萄糖醛酸苷酶芳基硫酸酯酶），然后通过Bond - Elut Certify柱进行萃取。接着，残留物用N - 甲基 - N - 三甲基硅烷基 - 三氟乙酰胺（MSTFA）进行选择性衍生化，它能使羟基、酸性和酚基形成三甲基硅烷基衍生物，还用N - 甲基 - 双 - 三氟乙酰胺（MBTFA）进行衍生化，它能使伯胺和仲胺形成三氟乙酰胺衍生物。在扫描模式下工作的GC - MS系统灵敏且特异，足以在给予治疗中常见剂量后至少24小时内检测和鉴定尿液中约100种化合物和代谢物。对于β - 激动剂的测定，需要在选择离子监测模式下进行检测。该方法在1992年7月于西班牙巴塞罗那举行的第25届奥运会期间的尿液样本兴奋剂检测中得到成功应用。
