【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。更多还原

【Abstract】 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 8 min,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 canrier gas,the flow rate was 3 mL·min^-1.NMP as the dissolution solvent.Injection:1 μL.Results:The calibra- tion curves of each solvent had good linear relationship,and those solvents could be completely separated.Conclu- sion:The established mathod is accuracy,sensitive,simple and can be used in detection of residual solvents.更多还原