Objective:Toestablish a method for the determination of methylene chloride,isopropyl ether and triisopropyl silane,three kinds of residual solvents with poor water solubility in SHR0410 API,and lay a foundation for the risk assessment of these three residual solvents in SHR0410 API.Methods:TheHeadspace gas chromatography external standard methodwas used.The capillary columnwas CP-Volamine(30 m×0.32 mm),and with nitrogen as the carriergas and an FID as the detector.The column temperature was pro-grammed raising.Results:Thechromatographic peaksofthe three residual solvents dichloromethane,isopropyl ether and triisopropyl silane can be effectively separated under this condition.The linear ranges for methylene chloride,isopropyl ether and triisopropyl silane were16.58-99.50 μg·mL-1(r=0.999),2.47-14.83 μg·mL-1(r=0.999),123.24-739.46 μg·mL-1(r=0.998)respectively.The aver-age recoverieswere 97.2%(RSD%=2.3%,n=6),95.5%(RSD%=2.0%,n=6),99.6%(RSD%=1.4%,n=6),respectively,and the LOD were 0.07 μg·mL-1,0.01 μg·mL-1,0.005 μg·mL-1 respectively.Three batches of samples were tested and noneof the above three residual solvents was detected.Conclusion:The methodestablishedcan be used for the determination of residual solvents with poor water solubility in SHR0410 API samples.
SHR0410Recovery ratesMatrix effectHeadspace gas chromatographySolubility
维普
万方数据
