摘要
目的:建立一种常用的气相色谱法分离检测ICH中规定的34种残留溶剂。方法:以DB-624弹性石英毛细管柱为色谱柱(75 m×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220℃,检测器温度为300℃,柱温采用程序升温(35℃保持18 min;以5℃·min^(-1)升至45℃,保持8 min;以5℃·min^(-1)升至80℃,保持3 min;以5℃·min^(-1)升至150℃,保持2 min;再以30℃·min^(-1)升至250℃,并保持5 min),流速3 mL·min^(-1)。以N-甲基吡咯烷酮为溶剂,进样体积为1μL。结果:34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34种溶剂的分离与测定,方法简单准确。
Objective：To establish a CGC method for determination of 34 residual solvents in ICH ,like methanol, ethanol, ether and ect.. Method： Using a DB - 624 column （75 m× 0.53 mm × 3.0 μm） ; Flame ionization detector （FID） ;The injector temperature was 220 ℃ ;The detector temperature was 300 ℃ ;The column temperature was programmed,the initial temperature was 35 ℃ ,maintain for 18 min,raise to 45 ℃ with a rate of 5 ℃ ·min^-1, maintain for 8min, raise to 80 ℃ with a rate of 5 ℃ · min^- 1, maintain 3 min, raise to 150 ℃ with a rate of 5 ℃ . min^ - 1, maintain for 2 min, then raise to 250 ℃ with a rate of 30 ℃ · min^ -1, maintain for 5 min ; Nitrogen was used as carrier gas, the flow rate was 3 mL · min^ - 1. NMP as the dissolution solvent. Injection ： 1 μL. Results： The calibration curves of each solvent had good linear relationship, and those solvents could be completely separated. Conclusion：The established mathod is accuracy,sensitive,simple and can be used in detection of residual solvents.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2008年第10期1767-1770,共4页
Chinese Journal of Pharmaceutical Analysis
