顶空气相色谱法测定海可素Ⅱ中残留溶剂的含量  

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

作　　者：肖宣[1] 刘冬[1] 王可敏 陈家智 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]上海杏灵科技药业有限公司技术部,上海201703

出　　处：《中国医学科学院学报》2014年第6期599-601,共3页Acta Academiae Medicinae Sinicae

摘　　要：目的 建立测定人工麝香原料之一海可素Ⅰ中甲醇、乙醇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,丙酮为内标,顶空预热温度为90℃,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×0.53 mm,5μm）,采用程序升温,实现各组分的基线分离.结果 甲醇、乙醇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、1.0μg/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,适用于海可素Ⅰ中残留有机溶剂的测定.Objective To explore the usefulness of head-space gas chromatography for the determina- tion of methanol and ethanol in Haikesu I, a raw material of artificial musk. Methods The determination was performed on HP-5 （30 m × 0. 53 mm, 5 μm） capillary column with an hydrogen flame ionization detector. The solvent was dimethyl sulfoxide and the internal standard was acetone. The injector temperature and the detector temperature were controlled at 180 ℃ and 250 ℃ , respectively. The carrier gas was nitrogen. The containers of head-space injector were preheated at 90 ℃ 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 and ethanol in their linearity range; and the limit of detection was 0.8 and 1.0 μg/ml, respectively. The precision and average recoveries were satisfactory. Conclusion The head-space gas chromatography is sim- ple, rapid, and precise technique for the measurement of residual solvents in Haikesu I.

关 键 词：海可素Ⅰ 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]