摘要
目的:建立阿托伐他汀钙原料药中甲醇、丙酮、叔丁醇、正丁醇4种有机溶剂残留量的测定方法。方法:采用顶空毛细管气相色谱法,DB-624石英毛细管柱,检测器为氢火焰离子化检测器,载气为氦气,流速为5.0 m L·min-1,柱温采用程序升温(初始温度40℃,维持3mim,15℃·min-1的速率升温至150℃,维持2 min,再以30℃·min-1的速率降至40℃,维持8 min),进样口温度为180℃,检测器温度为260℃,顶空温度为100℃,平衡时间为30 min,分流比为2∶1,定量环温度为100℃,传输管温度为110℃,进样体积为2 m L。结果:4种有机溶剂在该色谱条件下均能有效分离,峰面积与浓度呈现良好线性关系,精密度、回收率良好。结论:该方法准确、可靠,专属性强,灵敏度高,可用于阿托伐他汀钙原料药中残留溶剂的含量测定。
Objective： To establish a method for the determination of 4 residual solvents including methonal, acetone, ten-butanol, n-butanol in atorvastatin calcium raw material. Methods： Headspace capillary GC method was adopted. The determination was performed on DB-624 capillary column at the rate of 5.0 mL·min^-1 using helium gas as carrier gas and FID as the detector by temperature programming（ initial column temperature of 40 ℃ , maintaining for 3 min, then raising to 150 ℃ at a rate of 15 ℃ ~ min^- 1 , maintaining for 2 min, and then descending to 40 ℃ at a rate of 30 ℃ · min^- 1 , maintaining for 8 min）. The temperature of the injector was maintaining at 180 ℃ and that of detector at 260 ℃. The equilibrium temperature was 100 ℃ and equilibrium time was 30 min. The split ratio was 2： 1. The looper temperature was 100 ℃ and the transmission pipe temperature was ll0 ~C. The volume of sample was 2 mL. Results：The measured 4 residual solvents were separated completely under given chromatogram systems. The calibration curve of each solvent showed a good linear relationship with precision and recovery. Conclusion： The method is specific, reliable and sensitive, and suitable for the content determination of residual solvents in atorvastatin calcium raw material.
出处
《中国药物评价》
2015年第3期135-138,共4页
Chinese Journal of Drug Evaluation
关键词
阿托伐他汀钙
残留溶剂
顶空毛细管气相色谱法
Atorvastatin calcium
Residual solvent
Headspace capillary gas chromatography
