盐酸丁咯地尔原料药中残留溶剂检测方法的研究  

GC detection of residual solvents in buflomedil hydrochloride

作　　者：陈悦[1] 冯婧[2] 

机构地区：[1]浙江省药品检验所,杭州310004 [2]嘉兴市药品检验所,嘉兴314001

出　　处：《药物分析杂志》2008年第3期486-489,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立盐酸丁咯地尔原料药残留溶剂检查的质控分析方法。方法:采用毛细管柱顶空进样气相色谱程序升温法测定。色谱柱为 HP—FFAP 弹性石英毛细管柱(以聚乙二醇为固定液,25.0 m×0.320mm×0.5μm);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45℃,保持12 min,再以12℃·min^(-1)的升温速率升至165℃,维持3min^(-1);载气:高纯度氮气;流速:1.0 mL·min^(-1)。顶空进样,平衡温度:85℃,平衡时间:30 min,进样体积:1.0 mL。以水为溶解介质;以丁酮为内标物。结果:被测各溶剂均能良好分离,各溶剂峰面积与浓度均呈良好的线性关系;方法的精密度良好;回收率较为理想。结论:该法适用于盐酸丁咯地尔原料药的残留溶剂检测。Objective：To establish a method for detection of the residual solvents in buflomedil hydrochloride. Method：The residual solvents in this material were determined by HS - GC equipped with FID detector and linked with HP- FFAP capillary column（25.0m×0.320mm×0.5μm）. The carries gas was highly purified nitrogen. The inlet temperature was 200℃ and the FID detector temperature was 250℃. The column temperature was raised by program：the initial temperature was 45℃,maintained for 12 min,raised to 165℃ with a rate of 12℃·min^-1, maintained for 3 min, then dropped to the initial temperature immediately. The flow rate of carried gas N2 was 1.0 mL·min^-1. The heated temperature of the headspaee oven was 85℃ ,the heated time lasted 30 min,and the injection volume was 1.0 mL. The dissolved medium used to prepare all of the test solutions was water, and the in- ternal standard was butanone. Results： Each solvent could be completely separated in chromatogram obtained from systemic suitability test, 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 buflomedil hydrochloride material.

关 键 词：盐酸丁咯地尔 残留溶剂 气相色谱法 顶空进样 毛细管色谱柱 

分 类 号：R917[医药卫生—药物分析学]