顶空气相色谱法测定托拉塞米原料药中残留溶剂

目的:检查托拉塞米原料药中甲醇、二氯甲烷、甲苯、二氧六环等有机溶剂残留量。方法:采用气相色谱(GC)法测定,色谱柱为HP-5弹性石英毛细管柱(5%-苯基甲基聚硅氧烷为固定液,30 m×0.53 mm,1μm),进样口温度220℃;氢火焰离子化检测器(FID)温度:240℃;柱温:程序升温,初始温度40℃,保持10 min,以40℃·min-1升温至200℃,保持3 min;载气:N2;流速:5 mL·min-1;以二甲亚砜为溶剂,丙酮为内标物。结果:被测物均能得到很好的分离,峰面积与浓度呈良好的线性关系,精密度良好。结论:该法可用于托拉塞米原料药中有机溶剂残留量检测。

Gas chromatography detection of residual solvents in torasemide

Objective: To establish a method for detection of the residual solvents in bulk torasemide,such as methanol,dichloromethane,toluene and 1,4-dioxane.Methods: The residual solvents in torasemide were determined by gas chromatography(GC) with HP-5 capillary column(30 m×0.53 mm,1 μm) with FID detector and with nitrogen as the carries gas.The injector temperature was 220 ℃;the detector temperature was 240 ℃;the column temperature rose by program,that was,the initial temperature was 40 ℃,maintained for 10 min,raise to 200 ℃ at a rate of 40 ℃·min-1,and then maintained for 3 min.The flow rate of N2 was 5 mL·min-1.Results: The solvents were completely separated,and the calibration curves of each solvent had good linear relationship within a certain range.Conclusion: This method is accurate and reliable.It can be applied in detection of residual solvents in torasemide.