顶空气相色谱法测定雷诺嗪中5种有机溶剂残留量

Determination of residual solvents in ranolazine by headspace gas chromatography

目的采用顶空进样毛细管气相色谱法测定雷诺嗪原料药中甲醇、乙醇、甲苯、二氯甲烷及二氧六环5种有机溶剂的残留量。方法使用HP-INNOWAX毛细管色谱柱(0.32mm×30m×0.25μm),柱温45℃,FID检测器,以水为溶剂,载气为氮气,进样口温度180℃,检测器温度250℃。结果5种有机溶剂分离完全,线性范围分别为甲醇3.96～39.6μg·ml-1,乙醇7.89～78.9μg·ml-1,二氯甲烷3.34～33.4μg·ml-1,甲苯11.2～111.8μg·ml-1,二氧六环8.80～88.0μg·ml-1。在所考察的浓度范围内线性关系良好,r为0.9994～0.9988,平均回收率为89.4%～104.0%,精密度、重复性RSD均小于8%。结论本方法适用于雷诺嗪原料药中有机溶剂残留量的测定。

Objective To determine the contents of the residual solvents, methanol, ethanol, toluene, diehloromethane and dioxane in ranolazine raw material. Methods Headspace gas chromatography was used to analyze the residual solvents quantitatively. Samples were analyzed on an HP-INNOWAX column with column temperature at 45 ℃ using water as solvent. Results Five residual solvents were completely separated. The liner range and recoveries were satisfied. RSD of precision and accuracy was less than 8% with average recoveries between 87.1% and 105.6%. Conclusion The method could be used for the quality control of ranolazine raw material.