RESUMO
OBJECTIVE:To establish a method for the determination of residual solvent of ethanol and toluene in diphenhydr-amine hydrochloride raw material. METHODS:Headspace capillary gas charmatography and butanone as internal standard were used. The column was Agilent DB-624 capillary column,inlet temperature was 200 ℃,hydrogen flame ionization detector was 250 ℃,the carried gas was high purity nitrogen,flow rate was 3.0 ml/min with temperature programmed,the splitting-ratio was 20∶1,the containers of headspace injector were in equilibrium at 80 ℃ for 30 min,and the injection time was 1 min. RESULTS:With this chromatographic condition,ethanol,toluene and internal standard peak were well separated;there was a good linear rela-tionship of ethanol and toluene in the range of 0.02-0.8 mg/ml (r=0.999 8 and r=0.999 4);RSDs of precision and stability test were lower than 3%;recoveries were 95.50%-103.50%(RSD=2.6%,n=9) and 96.91%-103.74%(RSD=2.2%,n=9). CON-CLUSIONS:The method is simple,sensitive and accurate,and can be used for the determination of residual solvent of ethanol and toluene in diphenhydramine hydrochloride raw material.
RESUMO
OBJECTIVE: To establish headspace capillary gas chromatography for the content determination of 3 kinds of residual organic solvent (furanidine,methanol and ethanol) in betamethasone sodium phosphate raw material.METHODS: The sample was dissolved in water and n-propanol was used as internal standard.The residual solvent in betamethasone sodium phosphate was separated on HP-INNOWAX (PEG) capillary column with column temperature set at 60 ℃.The injector temperature and FID detector temperature were controlled at 180 ℃ and 250 ℃,respectively.The carried gas was nitrogen at flow rate of 1.0 mL?min-1.The splitting-ratio was 10 ∶ 1.The containers of head-space injector were in equilibrium at 80 ℃ for 30 min.Injection time was 1 min.RESULTS: With this chromatographic condition,those solvents could be separated completely.The linear range were 0.014 4～0.071 8 mg?mL-1 for furanidine,0.060～0.300 mg?mL-1 for methanol and 0.099 3～0.497 mg?mL-1 for ethanol.The average recovery were 103.7% (RSD=0.53%,n=6),95.8% (RSD=0.30%,n=6) and 95.0% (RSD=0.48%,n=6) respectively.The minimum quantitation limit were 0.057 3 ?g?mL-1,0.486 ?g?mL-1,0.145 ?g?mL-1,respectively.3 kinds of residual organic solvents were all in line with the standard stated in Chinese Pharmacopeia.CONCLUSION: The established method is simple,sensitive and accurate for the content determination of residual solvents in betamethasone sodium phosphate raw material.