顶空气相色谱法测定舒更葡糖钠原料药中7种有机溶剂的残留量

Determination of 7 Kinds of Organic Solvents Residualin Sugammadex Sodium Apis by Headspace Gas Chromatography

目的:建立测定舒更葡糖钠原料药中甲醇、乙醇、丙酮、丙烯腈、丙烯酸甲酯、苯和丙烯酸乙酯7种有机溶剂残留量的方法。方法:采用顶空气相色谱法,色谱柱为DB-624毛细管柱(30 m×0.32 mm,1.8μm),柱温采用程序升温,进样口温度200℃,检测器为氢火焰离子化检测器,温度250℃,载气为高纯氮气,载气流速3.0 mL/min,分流比10∶1,顶空平衡温度60℃,平衡时间30 min。结果:各有机溶剂分离度良好,7种有机溶剂在各自质量浓度范围内与相应色谱峰峰面积线性关系良好(r=0.9981~0.9999),平均回收率91.6%~104.3%。结论:该方法快捷、准确、灵敏度高,可用于舒更葡糖钠原料药中甲醇、乙醇、丙酮、丙烯腈、丙烯酸甲酯、苯和丙烯酸乙酯残留量的测定。

Objective:To establish a method for the determination of 7 kinds of organic solvents residual in Sugammadex So⁃dium raw material,including methanol,ethanol,acetone,acrylonitrile,methyl acrylate,benzene and ethyl acrylate.Meth⁃ods:The headspace gas chromatography was adopted.The samples were separated on a DB-624 capillary column(30 m×0.32 mm,1.8μm)using the temperature programming and a FID detector.The inlet temperature and the detector tempera⁃ture were set at 200℃and 250℃,respectively.Nitrogen was used as the carrier gas with a flow rate of 3.0 mL/min.The spil⁃tratio was 10∶1.The headspace equilibrium temperature was set at 60℃and the equilibrium time was 30 min.Results:Ex⁃cellent chromatographic separation was achieved.There was a good linear relationship between the mass concentrations of the seven componentsand the peak are asin the corresponding concentration range(r=0.9981~0.9999).The average recov⁃eries were all between 91.6%and 104.3%.Conclusion:The method is rapid,accurate,sensitive and can be used for the content determination of residual solvents in Sugammadex Sodium Apis.