气相色谱法测定西格列汀原料药中6种残留溶剂

Determination of 6 Residual Solvents in Sitagliptin API by Gas Chromatography

采用气相色谱法检测西格列汀原料药中四氢呋喃、乙酸乙酯、丁酮、二氯甲烷、甲苯、N,N-二甲基甲酰胺。色谱条件为DB-WAX(30m×0.32mm×0.5μm)毛细管色谱柱;载气采用高纯氮气,流速为1mL/min;检测器为氢火焰离子化检测器,检测器温度为250℃,进样口温度为200℃;程序升温,分流比10∶1,进样量1μL。该方法操作简便、稳定、重复性好,可用于西格列汀原料药中上述6种残留溶剂的测定。

Gas chromatography was used to detect tetrahydrofuran,ethyl acetate,methyl ethyl ketone,dichloromethane, toluene and N,N-dimethylformamide in the drug substance of sitagliptin.The chromatographic conditions were DB-WAX (30m×0.32mm×0.5um)capillary column;the carrier gas was high purity nitrogen with a flow rate of 1ml/min;the detector was a hydrogen flame ionization detector with a detector temperature of 250 ℃.The sample temperature was 200 ℃;the temperature was programmed,the split ratio was 10 ∶ 1,and the injection volume was 1 ul.The method is simple,stable and reproducible,and can be used for the determination of the above six residual solvents in the sitagliptin bulk drug.