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

Zhongguo Yi Xue Ke Xue Yuan Xue Bao. 2014 Dec;36(6):599-601. doi: 10.3881/j.issn.1000-503X.2014.06.006.

Abstract

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.

MeSH terms

  • Acetone / analysis
  • Chromatography, Gas*
  • Drugs, Chinese Herbal / chemistry*
  • Ethanol / analysis
  • Flame Ionization
  • Methanol / analysis
  • Solvents / analysis*

Substances

  • Drugs, Chinese Herbal
  • Solvents
  • Acetone
  • Ethanol
  • Methanol