顶空毛细管气相色谱法测定西洛他唑中有机溶剂的残留量  

Headspace capillary GC determination of residual organic solvents in cilostazol

作　　者：张亿 朱蓉 

机构地区：[1]成都市药品检验所,成都610045

出　　处：《药物分析杂志》2006年第7期1026-1027,共2页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立了西洛他唑合成中所用丙酮、异丙醇、乙醇、氯仿有机溶剂残留量检测方法。方法:采用毛细管气相色谱法,顶空进样,氢火焰离子化检测器(FID),以水为溶剂,HP-INNOWAX(30 m×0.53 mm×1.0μm)毛细管色谱柱,进样口温度200℃,检测器温度250℃,柱温先在40℃保持5 min,然后以每分钟5℃的升温速率升至80℃,再以每分钟20℃升温速率升至150℃。结果:4种溶剂均达到了完全分离,各溶剂线性试验所得回归方程相关系数均在0.99以上,加样回收率在95.9%～102.1%之间,RSD<2.0%(n=6)。结论:方法准确、灵敏、重现性好,达到有机溶剂残留的检测要求。Objective ：To develop a headspace capillary GC method for detemaination of acetone, isopmpanol, ethanol, chloroform in cilostazol. Method：Using HP-INNWAX capillary column（30 m ×0. 53 mm × 1.0 μm） ,FID detector and programmablly increased temperature,the samples were dissolved in water. The initial temperature was kept at 40 ℃ for 5 min,the temperature was raised to 80 ℃ at the heating rate of 5 ℃ · min^-1 and then was raised to 150 ℃ at the heating rate of 20 ℃ · min ^- 1. The injection pert and detector temperature were 200 ℃ and 250 ℃ respectively. Result：Four residual organic solvents consisting of acetone, isopropanol, ethanol and chloroform in cilostazol were completely separated. The correlation coefficient of calibration curve of each content in equation was more than 0. 99. The recoveries were between 95. 9% and 102. 1% ,RSD 〈2. 0% （n =6）. Conclusion：The method is proved to be accurate and sensitive after validation. It is suitable to the determination of residual organic solvents in cilostazol.

关 键 词：顶空毛细管气相色谱法 西洛他唑 残留有机溶剂 

分 类 号：R917[医药卫生—药物分析学]