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

Zhongguo Yi Xue Ke Xue Yuan Xue Bao. 2014 Dec;36(6):606-9. doi: 10.3881/j.issn.1000-503X.2014.06.008.

Abstract

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.

MeSH terms

  • Chromatography, Gas*
  • Cycloparaffins / chemistry*
  • Drug Contamination
  • Drugs, Chinese Herbal / chemistry*
  • Ethanol / analysis
  • Solvents / analysis*

Substances

  • Cycloparaffins
  • Drugs, Chinese Herbal
  • Solvents
  • Ethanol
  • muscone