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顶空毛细管气相色谱法测定阿托伐他汀钙原料药中残留溶剂

田洁   

  1. 大连市药品检验所
  • 收稿日期:2015-03-03 修回日期:2015-05-26 出版日期:2015-06-25 发布日期:2015-06-25

Determination of Residual Solvent in Atorvastatin Calcium Raw Material by Headspace Capillary GC Method

  1. DaLian Institute for Drug Control
  • Received:2015-03-03 Revised:2015-05-26 Online:2015-06-25 Published:2015-06-25

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5.0mL/min,柱温采用程序升温(初始温度40℃,维持3mim,15℃/min 的速率升温至150℃,维持2min,再以30℃/min 的速率降至40℃,维持8分钟),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2mL。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。

Abstract: Objective :To establish a method for the determination of 4 residual solvents including methonal, acetone,tert-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 5.0mL/min 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,maintaining for 2 min,and then descending to 40 ℃ at a rate of 30 ℃/min,maintaining for 8 min). The temperature of the injector was maintaining at 180 ℃ and that of detector at 260 ℃. The split ratio was 2:1.The equilibrium temperature was 100 ℃ and equilibrium time was 30 min. The looper temperature was 100 ℃ and the The transmission pipe temperature was 110 ℃.The volume of sample was 2 mL. Results:The measured 4 residul solvents were separated completely under given chromatogram systems. The calibration curve of ezch solvent showed a good linear relationship with precision and recovery. Conclusion:The method is specific, reliable sensitive,and suitable for the content determination of residual solvents in Atorvastatin calcium raw material.