顶空气相色谱法测定麝香酮中残留溶剂的含量  

Determination of the Content of Residual Solvents in Muscone by Head-space Gas Chromatography

作　　者：刘冬[1] 王可敏 肖宣[1] 伦立军 章菽 

机构地区：[1]中国医学科学院北京协和医学院药物研究所天然产物室,北京100050 [2]北京联馨药业有限公司技术部,北京102628 [3]山东宏济堂制药集团有限公司技术部,济南250012

出　　处：《中国医学科学院学报》2014年第6期606-609,共4页Acta Academiae Medicinae Sinicae

摘　　要：目的 建立测定麝香酮中甲醇、乙醇、乙醚及石油醚（60～ 90℃）有机溶剂含量的顶空气相色谱法.方法 采用顶空气相色谱法,氢火焰离子化检测器,以二甲基亚砜为溶媒,顶空预热温度为80℃,预热时间为15 min,进样口温度为180℃,检测器温度为250℃,以氮气为载气,使用HP-5交联毛细管柱（30m×0.53mm,5μm）,采用程序升温,实现各组分的基线分离.结果 甲醇、乙醇、乙醚及石油醚（60 ～90 ℃）在各自对应的浓度范围内,线性关系良好;最小检测限分别为0.8、1.0、0.1、0.3μg/ml;加样回收率、精密度良好.结论 经方法学考察,该方法灵敏、准确、可靠,适用于麝香酮中残留有机溶剂的测定.Objective 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.Methods 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.Results 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.Conclusion The head-space gas chromatography is simple,rapid,and precise technique for measuring residual solvents in muscone.

关 键 词：麝香酮 人工麝香 顶空气相色谱法 残留溶剂 

分 类 号：R917[医药卫生—药物分析学]