顶空气相色谱法测定盐酸倍他洛尔中6种有机溶剂残留量

Determination of 6 kinds of residual organic solvents in betaxolol hydrochloride by head-space gas chromatography

目的建立气相色谱法测定盐酸倍他洛尔中丙酮、乙酸乙酯、异丙醇、乙腈、甲苯、N,N-二甲基甲酰胺6种有机溶剂残留量。方法采用气相色谱法,色谱柱为DB-WAX石英毛细管柱(30.0m×0.53mm,1.0μm),载气为氮气,进样口温度为250℃,FID检测器温度为280℃;柱温为50℃,保持5min,以15℃·min-1升温速率升至200℃,维持6min,溶剂为二甲基亚砜。结果被测物均能得到很好的分离,峰面积与质量浓度线性关系良好,精密度和回收率良好。结论该方法准确、可行,可作为盐酸倍他洛尔的质量控制与评价的一种直观、合理、有效的技术手段。

Objective To establish a gas chromatography method for the determination of residual organic solvents：acetone,ethyl acetate,iso-propanol,acetonitrile,toluene and N,N-dimethylformamide in betaxolol hydrochloride.Methods The residual solvents in betaxolol hydrochloride were separated by DB-624capillary column（30.0m×0.53mm,1.0μm）with FID detector.The carried gas was nitrogen.The injector temperature and detector temperature were controlled at 250℃and 280℃,respectively.The column temperature was maintained at 50℃for 5min,then raised at a rate of 15℃per min to 200℃and maintained for 6min.The sample was dissolved in dimethyl sulfoxide.Results The solvents were separated completely.The calibration curve of each solvent showed a good linear relationship with good precision and accuracy.Conclusion This method is accurate and reliable,and is an efficient method for the quality evaluation of betaxolol hydrochloride.