Determination of the content of residual solvents in Haikesu 2 by head-space gas chromatography

Zhongguo Yi Xue Ke Xue Yuan Xue Bao. 2014 Dec;36(6):602-5. doi: 10.3881/j.issn.1000-503X.2014.06.007.

Abstract

Objective: To determine ethylacetate and petroleum ether(60-90 ℃)in Haikesu 2,which is one of the raw materials of artificial musk,using the head-space gas chromatography.

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 methanol. 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 ethylacetate and petroleum ether(60-90 ℃)in their linearity range;and the limit of detection was 0.7 and 0.3 Μg/ml,respectively. The good precision and good average recoveries were satisfactory.

Conclusion: The head-space gas chromatography is simple,rapid,and precise technique for the measurement of residual solvents in Haikesu 2.

MeSH terms

  • Acetates / analysis
  • Chromatography, Gas*
  • Drugs, Chinese Herbal / chemistry*
  • Fatty Acids, Monounsaturated / chemistry
  • Flame Ionization
  • Solvents / analysis*

Substances

  • Acetates
  • Drugs, Chinese Herbal
  • Fatty Acids, Monounsaturated
  • Solvents
  • musk
  • ethyl acetate