Objective To establish a headspace gas chromatography method for the determination of methanol,ethanol,isopropanol,dichloromethane,tetrahydrofuran,2-methyltetrahydrofuran,isopropylace-tate and N,N-dimethylformamide.Methods A headspace gas chromatography method was used to separate the residual solvents on a CP-Volamine capillary column(30 m×0.32 mm).The carrier gas was nitrogen.The initial temperature of the column was 40 ℃ for 5 min and was raised to 220 ℃ at the rate of 20 ℃·min-1 for 5 min.The equilibrium temperature of the headspace injector was 100 ℃ that lasted for 15 min.Results The eight solvents were well separated.The linearity was good within their respective concentra-tion ranges.The recovery ranged from 99.3％to 103.6％,with an RSD of 1.7％-4.9％(n=6).There was no significant difference in the detection of formamide content between the two injection methods.Conclusion The established method is sensitive and accurate,and suitable for the determination of residual solvents in raw materials.
关键词
顶空气相色谱法/残留溶剂/原料药
Key words
headspace gas chromatography/residual solvents/raw materials
维普
万方数据