Liu Dong, Wang Ke-Min, Xiao Xuan, Lun Li-Jun, Zhang Shu
Department of Natural Medicinal Chemistry,Institute of Materia Medica,CAMS and PUMC,Beijing 100050,China.
Department of Technology,Beijing Lianxin Pharmaceutic Co.,Ltd,Beijing 102628,China;3 Department of Technology,Hongjitang Pharmaceutical Co.,Ltd,Jinan 250012,China.
Zhongguo Yi Xue Ke Xue Yuan Xue Bao. 2014 Dec;36(6):606-9. doi: 10.3881/j.issn.1000-503X.2014.06.008.
To explore the usefulness of a head-space gas chromatography in the determination of residual solvents including methanol,ethanol,ethyl ether,and petroleum ether in muscone in artificial musk.
The head-space gas chromatography was performed on HP-5(30 m×0.53 mm,5 Μm)capillary column with a hydrogen flame ionization detector. The carrier gas was nitrogen and the solvent was dimethyl sulfoxide. The injector temperature and the detector temperature were controlled at 180 ℃ and 250 ℃,respectively. The containers of head-space injector were preheated at 80 ℃ for 15 minutes. The column temperature was programmed raised,which achieved baseline separation of the components.
The results showed a good linear relationship for methanol,ethanol,ethyl ether,and petroleum ether(60-90 ℃)in the range of each consistency; and the limit of detection was 0.8,1.0,0.1,and 0.3 Μg/ml,respectively. The precision and average recoveries were satisfactory.
The head-space gas chromatography is simple,rapid,and precise technique for measuring residual solvents in muscone.
探讨顶空气相色谱法在测定人工麝香中麝香酮内甲醇、乙醇、乙醚及石油醚等残留溶剂的应用价值。
采用HP-5（30 m×0.53 mm，5μm）毛细管柱，氢火焰离子化检测器，以氮气为载气，二甲基亚砜为溶剂，进样口温度和检测器温度分别控制在180℃和250℃，顶空进样瓶在80℃预热15分钟，柱温程序升温，各组分实现基线分离。
结果表明甲醇、乙醇、乙醚及石油醚（60 - 90℃）在各自浓度范围内线性关系良好；检测限分别为0.8、1.0、0.1及0.3μg/ml，精密度和平均回收率良好。
顶空气相色谱法是测定麝香酮中残留溶剂的简便、快速、准确的技术。
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