| 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 |
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| 引用本文： | 刘佳,朱京科.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[J].分析试验室,2012(3):105-109. |
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| 作者姓名： | 刘佳 朱京科 |
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| 作者单位： | 同济大学浙江学院;浙江大学化工系 |
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| 摘 要： | 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。
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| 关 键 词： | 气相色谱-质谱联用 6-溴-去氢甲基睾丸素 质谱解析 |
Identification of impurities in 6-bromo-methandrostenolone by gas chromatography-mass spectrometry |
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| LIU Jia,and ZHU Jing-ke.Identification of impurities in 6-bromo-methandrostenolone by gas chromatography-mass spectrometry[J].Chinese Journal of Analysis Laboratory,2012(3):105-109. |
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| Authors: | LIU Jia and ZHU Jing-ke |
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| Institution: | 1.Tongji Zhejiang College,Jiaxing 314000;2.Department of Chemical Engineering,Zhejiang University,Hangzhou 310027) |
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| Abstract: | 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℃.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. |
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| Keywords: | Gas chromatography-mass spectrometry 6-bromo-methandrostenolone |
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