Determination of the content of residual solvents in Haikesu I by head-space gas chromatography / 中国医学科学院学报

<p><b>OBJECTIVE</b>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.</p><p><b>METHODS</b>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.</p><p><b>RESULTS</b>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.</p><p><b>CONCLUSION</b>The head-space gas chromatography is simple,rapid,and precise technique for the measurement of residual solvents in Haikesu I.</p>

Determination of the content of residual solvents in Haikesu 2 by head-space gas chromatography / 中国医学科学院学报

<p><b>OBJECTIVE</b>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.</p><p><b>METHODS</b>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.</p><p><b>RESULTS</b>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.</p><p><b>CONCLUSION</b>The head-space gas chromatography is simple,rapid,and precise technique for the measurement of residual solvents in Haikesu 2.</p>

Determination of the content of residual solvents in muscone by head-space gas chromatography / 中国医学科学院学报

<p><b>OBJECTIVE</b>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.</p><p><b>METHODS</b>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.</p><p><b>RESULTS</b>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.</p><p><b>CONCLUSION</b>The head-space gas chromatography is simple,rapid,and precise technique for measuring residual solvents in muscone.</p>