顶空毛细管气相色谱法测定米格列醇中有机溶剂残留量

目的：建立米格列醇中4种有机溶剂（甲醇、乙醇、丙酮、乙腈）残留量的分离定量方法。方法：采用内标法顶空进样毛细管气相色谱法,测定米格列醇原料中有机溶剂残留量。色谱柱为DB-624毛细管柱（30m×0.53mm×3.0μm）,载气为氮气,FID检测器;程序升温,在40℃下保留3min,然后以15℃/min的速率升温至150℃,保持2min;进样口温度200℃,检测器温度250℃,分流比为10︰1。结果：4种有机溶剂完全分离,样品中潜在杂质不干扰4种有机溶剂测定,线性关系良好,加样回收率结果理想。结论：本法灵敏、准确、快捷,适用于米格列醇中有机溶剂残留量的检测。

Headspace-capillary gas chromatographic determination of four organic residual solvents in miglitol

Objective： To establish a method to separate and quantitatively determine organic residual solvents（methanol,ethanol,acetone and acetonitrile） in miglito.Methods： The headspace-capillary gas chromatography with internal standard method was used.The separation was performed on a DB-624 capillary column（30m×0.53mm,3.0μm） with nitrogen as carrier gas and FID.The column temperature was initially maintained at 40℃ for 3min,then increased to 150℃（15℃/min） and maintained for 2 min.The injection port temperature was 200℃ and the detector temperature was 250℃.The split ratio was 10︰1.Results： Four organic residual solvents were separated completely.The linearities were excellent and recoveries were satisfactory.Conclusion： The method is sensitive,accurate,rapid and suitable for the determination of four residual solvents in miglitol.