顶空气相色谱法测定托拉塞米原料药中残留溶剂

摘要

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 Jim) 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.%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,lμm),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.