关键词: SHR0410, 回收率, 基质效应, 顶空气相色谱法, 溶解度

Abstract:

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 programmed 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 average 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.

Key words: SHR0410, Recovery rates, Matrix effect, Headspace gas chromatography, Solubility