毛细管气相色谱测定27种常用有机溶剂  

Determination of 27 residual solvents in ICH by capillary GC column

作　　者：魏京京[1] 张启明[1] 朱维华[1] 

机构地区：[1]中国药品生物制品检定所,北京100050

出　　处：《药物分析杂志》2006年第8期1171-1174,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立一种常用的气相色谱法分离测定 ICH 中规定必须检查的一类溶剂、二类溶剂及常用的三类溶剂。方法:以DB-624弹性石英毛细管柱为色谱柱(75m×0.53 mm,3.0μm),载气为氮气,采用氢火焰离子化检测器(FID),进样口温度为200℃,检测器温度为300℃,柱温采用程序升温(35℃保持18min,以5℃min^(-1)升至45℃,保持8min,以5℃·min^(-1)升至80℃,保持3min,以5℃·min^(-1)升至150℃,保持2min,再以30℃·min^(-1)升至250℃,并保持5min),以 N-甲基吡咯烷酮为溶剂,顶空进样。结果:27种有机溶剂均能得到很好的分离,分离度绝大多数均大于1.5。峰面积与浓度呈良好的线性关系,精密度良好。结论:本文气相色谱条件可用于常用的27种溶剂的分离与测定,方法简单准确。Objective：This paper reports a GC method for determination of about 30 solvents in ICH, like methanol,ethanol,ether and ect.. Method：Using a DB -624 column,the column length was 75 m ×0.53 mm;Flame ionization detector（FID） ;The injector temperature was 200 ℃ ;The detector temperature was 300 ℃ ;The column temperature was programmed raised;Nitrogen was used as carrier gas, the flow rate was 3 mL · min^-1 ;Using headspace injector. Results：The calibration curves of each solvent had good linear relationship, and those solvents could be completely separated. Conclusion：The established method is accuracy, sensitive, simple and can be used in detection of residual solvents.

关 键 词：毛细管气相色谱 顶空进样 残留溶剂 

分 类 号：R917[医药卫生—药物分析学]