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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。
Objective: To examine the residues of organic solvents such as methanol, methylene chloride, toluene and dioxane in torsemide. Methods: Gas chromatography (GC) was used. The column was HP-5 elastic quartz capillary column (5% -phenylmethyl polysiloxane as fixative solution, 30 m × 0.53 mm, 1 μm) 220 ℃; FID temperature: 240 ℃; column temperature: programmed temperature, the initial temperature was 40 ℃, maintained for 10 min, heated to 200 ℃ at 40 ℃ · min-1 for 3 min; : N2; flow rate: 5 mL · min-1; dimethyl sulfoxide as solvent and acetone as internal standard. Results: The analytes can be well separated, the peak area and concentration showed a good linear relationship, good precision. Conclusion: This method can be used for the determination of organic solvent residues in torsemide raw material.