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采用气相色谱-质谱联用方法分析6-溴-去氢甲基睾丸素中的杂质。在30.0m×0.25mm,0.5μm的ZB-5MS毛细管柱上,柱温100℃保持3 min,后以20℃/min的速率程序升温至250℃,气化室温度270℃,载气氦气流量0.8 mL/min的条件下,6-溴-去氢甲基睾丸素及其中杂质获得很好分离。通过对各组分质谱图分析确定了6-溴-去氢甲基睾丸素中的七种杂质分别为去氢甲基睾丸素,6-烯-去氢甲基睾丸素,6-溴-17-甲基雄甾-1,4,16-三烯-3-酮的4种构象异构体以及6-溴-8-烯-去氢甲基睾丸素。
The impurities in 6-bromo-dehydro-methyltestosterone were analyzed by gas chromatography-mass spectrometry. The column temperature was maintained at 100 ℃ for 3 min on a 30.0m × 0.25mm, 0.5μm ZB-5MS capillary column. The temperature of the column was raised to 250 ℃ at a rate of 20 ℃ / min and the gasification chamber temperature was 270 ℃. The carrier gas helium With 0.8 mL / min of flow rate, 6-Bromo-Desmethyltestosterone and its impurities were well separated. Through the mass spectrometry analysis of each component, the seven impurities in 6-bromo-dehydro-methyl testosterone were determined as dehydrogenomethyltestosterone, 6-ene-dehydro-methyl testosterone, 6-bromo- 4 -constituent of methylandrost-1, 4,16-trien-3-one and 6-bromo-8-ene-dehydro-methyltestosterone.