| Objective To establish a headspace gas chromatography method for quantitative analysis of residual amounts of ethanol,acetone, acetonitrile, dichloromethane, and trichloroethane in amantadine hydrochloride raw materials.Methods The separation used Agilent DB-624 capillary column (30 m×0.53 mm, 3.0 μm), programmed heating, FID detector. The inlet temperature and the detectortemperature were set at 200 ℃ and 250 ℃, respectively. Carrier gas was nitrogen (N2), the flow rate was 2.5 mL/min, the split ratio was 5∶1, and the headspace equilibrium temperature was 80 ℃. Balance time was 30 min.Results There was a good linear relationshipbetween the concentration of the solvent to be tested and its peak area (correlation coefficient>0.999 3); The average sample recoveryrate is 97.78% to 101.03%, and the RSD was 1.27% to 2.26%.Conclusions This analytical method is efficient, fast, with good repeat-ability and stability, and high accuracy. It is expected to provide a solid experimental basis for the quantitative analysis and control ofresidual solvents such as ethanol,acetone,acetonitrile, dichloromethane, and trichloroethane in amantadine hydrochloride raw materials. |
