(+)2-氨基丁醇合成工艺中残留溶剂的研究

Research on Residual Solvent in the Synthesis Process of(+)2-Aminobutanol

目的:建立GC法测定(+)2-氨基丁醇中有机溶剂的残留量。方法:色谱柱为J&W DB-SELECT624UI,以起始温度40℃程序升温8min,8℃/min的速率升温至120℃,维持7min;进样口温度为200℃,检测器温度为250℃;载气为氮气,流速2mL/min;分流比为40∶1;进样量为1μL。结果:甲醇线性范围为0.045mg/mL~3.6mg/mL(r=0.9999),定量限为15.03μg/mL,检测限为5.01μg/mL。结论:该方法灵敏度高、操作简单、可行性好,适用测定(+)2-氨基丁醇中残留溶剂。

Objective:To determine the residual amount of organic solvent in(+)2-aminobutanol by establishing a GC method.Methods:The chromatographic column was J&W DB-SELECT 624UI,with the initial temperature of 40℃,the programmed temperature of 8min,and the heating rate of 8℃/min to 120℃for 7min.Inlet temperature was 200℃and detector temperature was 250℃;The carry gas is nitrogen,and that flow rate is 2mL/min;The split ratio is 40∶1;The injection volume was 1L.Results:The linear range of methanol is 0.045 mg/mL to 3.6 mg/mL(r=0.9999),and the LOQ is 15.03μg/mL and the LOD is 5.01μg/mL.Conclusion:The method has the advantages of high sensitivity,simple operation and good feasibility,and is suitable for the determination of residual solvents in(+)2-aminobutanol.