毛细管柱气相色谱法测定恩替卡韦中8种残留溶剂

Determination of residual organic solvents in Entecavir by capillary GC

目的:建立毛细管柱气相色谱法测定恩替卡韦中残留的有机溶剂。方法:采用HP-624毛细管色谱柱、顶空进样、氢火焰离子化检测器,进样口温度为250℃,检测器温度为300℃,柱温为80℃保持7 min,再以20℃/min升至220℃。结果:甲醇、乙醇、二氯甲烷、叔丁基甲基醚、正己烷、乙酸乙酯、四氢呋喃与甲苯相邻峰间的分离度及检测灵敏度均符合要求。结论:该法简便、快速、灵敏、结果准确可靠,可用于恩替卡韦中残留有机溶剂的测定。

Objective：To develop a new capillary GC method for determination of residual organic solvents in Entecavir.Methods： Standard solution and test solution were introduced to HP-624 silica capillary column by headspace injection.The chromatograms were recorded with FID.The temperatures of injection port and detector were 250℃ and 300℃ respectively,the initial column temperature was kept at 80℃ for 7 min,and then raised to 220℃ at the rate of 20℃/min.Results： The eight residual organic solvents（methyl alcohol,ethanol,dichloromethane,tert-butyl methyl ether,normal hexane,ethyl acetate,tetrahydrofuran and toluene） were separated completely.The resolution and sensitivity were acceptable.Conclusion： The method was proved to be simple,rapid,sensitive and reliable,which can be used for determination of residual organic solvents in Entecavir.