利用红外光谱、核磁共振氢谱、紫外光谱以及质谱等表征手段对一种新型蛋白同化激素(AAS)口服药物的主成分进行了研究和鉴定,推定主成分为甲基-1-睾酮(methyl-1-testosterone, M1T, 17β-hydroxy-17α-methyl-5α-androst-1-en-3-one).在此基础上,建立了M1T的气相色谱-质谱联用检测方法.方法的检出限(信噪比(S/N)为3)为2 ng/mL,定量限(S/N=10)为10 ng/mL;7次平行测定前处理后的加内标尿样的相对标准偏差为9.8% .用该方法测定了该药物在尿样中的排泄曲线.该方法的建立为AAS新药的发现、检测和监控做了很有意义的基础研究工作.
A new oral drug containing an unknown anabolic androgenic steroid (AAS) was studied. The principal constituent of the unknown anabolic hormone was studied by infrared spectrum (IR), nuclear magnetic resonance spectroscopy (~1H NMR), ultraviolet spectroscopy (UV), and mass spectroscopy (MS). It was inferred to be methyl-1-testosterone (M1T,17β-hydroxy-17α-methyl-5α-androst-1-en-3-one) which was just added to the prohibited list in 2006. In addition, a monitoring, screening and confirmation of methyl-1-testosterone was established. The detection limit (S/N=3)was 2 ng/mL, and the limit of quantification (S/N=10) was 10 ng/mL. The relative standard deviation was 9.8% (n=7) for the determination of pretreated urine sample with internal standard. This method was successfully applied in the identification of M1T positive urine. The excretion curve of M1T in human urine is described. It is a significant work for the discovery, determination and monitoring of the new AAS.
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