顶空毛细管气相色谱法测定高三尖杉酯碱中的残留溶剂

Determination of Residual Solvents in Homoharringtonine by Head-space Capillary Gas Chromatography

目的:建立气相色谱法分离测定高三尖杉酯碱中的残留溶剂:乙醚、二氯甲烷。方法:以DB-624弹性石英毛细管柱(30m×0.53mm,3.0μm),载气为氮气,氢离子火焰检测器,甲醇作为内标物质,二甲基甲酰胺为溶剂,采取顶空进样。结果:乙醚、二氯甲烷在各自时应的浓度范围内,其峰面积与浓度呈良好得线性关系,加样回收率(n=5)分别为97.05％(RSD=1.25％)、98.20％(RSD=3.47％)。结论:该气相色谱方法可用于同时测定高三尖杉酯碱中的乙醚、二氯甲烷的含量,方法简单可靠。

Objective: This paper reports a GC method for determination of ether and dichloromethane in Homoharringtonine by GC. Method:The analytical column is DB-624(30m×0. 53mm,3. 0μm). The injector temperature is 180℃ ,and the detector temperature is 250℃. Column temperature rises by Programming,and the carrier gas is nitrogen. The solvent was dimethyfor-mamide. Results:The standard curves are linear for dichloromethane and ether in the range of each consistency. The average recoveries(n=5) are 97. 05% (RSD=1. 25%) for ether,98. 20% (RSD=3.47%) for dichloromethane respectively. Conclusion: This method is simple,rapid and precise.