顶空气相色谱法测定海克素I中残留溶剂的含量。
Determination of the content of residual solvents in Haikesu I by head-space gas chromatography.
作者信息
Xiao Xuan, Liu Dong, Wang Ke-Min, Chen Jia-Zhi, Zhang Shu
机构信息
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.
出版信息
Zhongguo Yi Xue Ke Xue Yuan Xue Bao. 2014 Dec;36(6):599-601. doi: 10.3881/j.issn.1000-503X.2014.06.006.
OBJECTIVE
To explore the usefulness of head-space gas chromatography for the determination 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 simple,rapid,and precise technique for the measurement of residual solvents in Haikesu I.
目的
探讨顶空气相色谱法测定人工麝香原料海克苏I中甲醇和乙醇的含量。
方法
采用HP-5（30 m×0.53 mm，5μm）毛细管柱，氢火焰离子化检测器。以二甲基亚砜为溶剂，丙酮为内标。进样口温度和检测器温度分别控制在180℃和250℃。载气为氮气。顶空进样器的容器在90℃预热15分钟。柱温程序升温，实现了各组分的基线分离。
结果
甲醇和乙醇在其线性范围内呈良好的线性关系；检测限分别为0.8和1.0μg/ml。精密度和平均回收率均令人满意。
结论
顶空气相色谱法是测定海克苏I中残留溶剂的简便、快速、准确的技术。
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