气相色谱法测定他达拉非原料药中甲胺与三乙胺的残留量

Determination of residual organic solvents of methylamine and triethylamine in tadalafil by Gas chromatography

目的采用顶空气相色谱法测定他达拉非原料药中溶剂甲胺、三乙胺的残留量。方法采用程序升温法,色谱柱为KB-5-V毛细管柱,进样口温度200℃,氢火焰离子化检测器温度260℃,氮气为载气,流速3.46 mL·min^(-1),分流比为5:1,顶空平衡温度80℃,平衡时间30 min,进样体积1.0 mL。结果色谱图中两组分的分离较好,峰型较好;在实验浓度范围内,浓度与峰面积具良好的线性关系,回收率为95%~105%,RSD<3%。结论所用方法简单、准确、灵敏,适用于他达拉非原料药中甲胺与三乙胺残留溶剂的检测。

OBJECTIVE To determine the residual organic solvents of methylamine and triethylamine in tadalafil by a head space GC method.METHODS The residual solvents were separated on KB-5-V capillary column by programmed temperature.The inlet temperature was 200℃and the FID temperature was 260℃.Nitrogen was used as carrier gas with flow rate of 3.46 mL·min-1,and the split ratio was 5∶1.Headspace oven was kept heating at 80℃for 30 min.The injection volume was 1.0 mL.RESULTS The two solvents could be separated in the chromatogram.The peak shapes of the two solvents appeared to be well and the calibration curve of each solvent was linear within certain range.The recoveries were within 95%-105%with the RSDs less than 3%.CONCLUSION This method is simple,accurate and sensitive.It can be applied to the determination of residual solvents of methylamine and triethylamine in tadalafil.