气相色谱-质谱联用法对6-溴-去氢甲基睾丸素合成过程中杂质的分析

Identification of impurities in 6-bromo-methandrostenolone by gas chromatography-mass spectrometry

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。

Impurities in 6-bromo-methandrostenolone were identified by gas chromatography-mass spectrometry. Separation was carried out on a 30m ×0. 25mm, 0. 5μm ZB -5MS capillary column with helium gas as carrier gas （flow rate at 0. 8 mL/min） at injection tempera of 270~C. By raising oven temperature from 100 to 250℃ at the ramp of 20℃/min, compounds in analyte were separated and identified by elucidating the corresponding MS spectra through manual analysis. The seven by-products in 6-bromo-methandrostenolone were methandrostenolone, 6-ene-methandrostenolone, four conformational isomers of 6-bromine-17-methyl-androst-1, 4,16-triene-3-ketone and 6-bromine-8-ene-methandrostenolone.