| 气相色谱-质谱联用法对3-氯亚氨基二苄中杂质的研究 |
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| 引用本文： | 刘佳,林伟锋,朱京科. 气相色谱-质谱联用法对3-氯亚氨基二苄中杂质的研究[J]. 化学世界, 2008, 49(10) |
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| 作者姓名： | 刘佳 林伟锋 朱京科 |
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| 作者单位： | 浙江大学材料与化工学院化工所,浙江,杭州,310027 |
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| 摘 要： | 应用气相色谱-质谱联用方法研究3-氯亚氨基二苄中的杂质。在30.0m×0.25mm,0.5μm的ZB-5MS毛细管柱上,柱温100°C保持3min,后以20°C/min的速率程序升温至250°C,气化室温度270°C,载气氦气流量0.8mL/min的条件下,3-氯亚氨基二苄及其中杂质获得很好分离。通过对各组分质谱图分析,并结合反应过程确定了3-氯亚氨基二苄中的四种杂质分别为亚氨基二苄,甲基亚氨基二苄酮,10-氯-5H-二苯并[b,f]氮杂和3,7-二氯-10,11-二氢-二苯并[b,f]氮杂。
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| 关 键 词： | 气相色谱-质谱联用 3-氯亚氨基二苄 质谱解析 |
Identification of Impurities in 3-Chloro-10,11-dihydro-5 H-dibenz[b,f]azepine by Gas Chromatography-Mass Spectrometry |
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| LIU Jia,LIN Wei-feng,ZHU Jing-ke. Identification of Impurities in 3-Chloro-10,11-dihydro-5 H-dibenz[b,f]azepine by Gas Chromatography-Mass Spectrometry[J]. Chemical World, 2008, 49(10) |
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| Authors: | LIU Jia LIN Wei-feng ZHU Jing-ke |
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| Abstract: | Impurities in 3-chloro-10,11-dihydro-5H-dibenz[b,f]azepine were identified by gas chromatography-mass spectrometry. Separation was carried on a 30m×0.25mm, 0.5μm ZB-5MS capillary column with helium gas as carrier(flow rate at 0.8 mL/min) and 270°C injection temperature. By raising oven temperature from 100 to 250°C at the ramp of 20°C/min, compounds in analyse were separated and identified by elucidating the corresponding MS spectra through manual analyzing and library matching. The four by-products in 3-chloro-10,11-dihydro-5H-dibenz[b,f]azepine were 10,11-dihydro-5H-dibenzo[b,f]azepine, 1-(10,11-dihydro-dibenzo[b,f]azepine-5-yl)-ethznone, 3-chloro-5H-dibenz[b,f]azepine and 3,7-dichloro-10,11-dihydro-5H-dibenz[b,f]azepine. |
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| Keywords: | gas chromatography-mass spectrometry 3-chloro-10,11-dihydro-5H-dibenz[b,f]azepine mass spectrum analyzing |
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