环孢素原料药中残留溶剂检测方法的研究  

GC Detection of Residual Solvents in Cyclosporine

作　　者：陈忠[1] 任林英[1] 郑申西[2] 唐信东[1] 

机构地区：[1]福建省微生物研究所,福建福州350007 [2]福州市疾病预防控制中心,福建福州350005

出　　处：《今日药学》2011年第11期681-683,共3页Pharmacy Today

摘　　要：目的检查环孢素原料药中的有机溶剂残留量。方法采用气相色谱法,色谱柱为弹性石英毛细管柱SE-54(聚甲基苯基乙烯基硅氧烷为固定液,30 m×0.53 mm×2.5μm),进样口温度200℃;氢火焰离子化检测器(FID)温度:250℃;柱温:程序升温,初始温度55℃,维持1 min,以10℃/min的速率升温至145℃,再以55℃/min的速率升温至200℃,维持2 min;载气:氮气,进样方式:分流进样,分流比:8∶1;流速2.3 ml/min。以二甲基乙酰胺为溶剂,外标法测定。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。结论该法可用于环孢素原料药中有机溶剂残留量检测。Objective To establish a method for detection of the residual solvents in cyclosporine substances.Methods The residual solvents in cyclosporine substances were determined by GC using capillary column SE-54（30 m×0.53 mm×2.5 μm） with FID detector and nitrogen as the carries gas.The injector temperature was 200 ℃,the detector temperature was 250 ℃,the column temperature rose by program,the initial temperature was 55 ℃ and maintained for 1 min,then raised to 145 ℃ with a rate of 10 ℃/min and raised to 200 ℃ with a rate of 55 ℃/min and maintained for 2 min.Split injection was use and the split ratio was 8∶1,the flow rate was 2.3 ml/min.External standard method was used with dimethylacetylamide as solvent.Results The solvents could be completely separated,and the calibration curves of each solvent had good linear relationship within a certain range.Conclusion The method is accurate and reliable.It can be applied in detection of residual solvents in cyclosporine substances.

关 键 词：环孢素 残留溶剂 气相色谱 

分 类 号：R927.2[医药卫生—药学]