气相色谱法测定盐酸阿夫唑嗪中5种有机溶剂残留量

GC-FID quantitative determination of five residual solvents in alfuzosin hydrochloride

目的:建立盐酸阿夫唑嗪中5种有机溶剂残留量的分离测定方法。方法:采用内标法分流进样毛细管气相色谱法,FID检测器,色谱柱为DB-624毛细管柱(30m×0.53mm×3.0μm),载气为氮气,程序升温:在40℃下保留5min,然后以50℃.min-1的速率升至200℃,至少保持11min。进样口温度160℃,检测器温度280℃,分流比为5∶1。测定盐酸阿夫唑嗪原料中甲醇、乙醇、丙酮、二氯甲烷、N,N-二甲基甲酰胺的残留量。结果:5种有机溶剂完全分离,样品中潜在杂质不干扰5种有机溶剂检测,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,适用于盐酸阿夫唑嗪中有机溶剂残留量的检测。

Objective：To establish a method for determination of five residual solvents in alfuzosin hydrochloride.Methods：The residual solvents in alfuzosin hydrochloride which are methanol,ethanol,acetone,dichloromethane and N,N-dimethylformamide were quantitatively determined by GC with internal standard method on DB-624 column,with FID detector,using nitrogen as the carries gas.The column temperature is initially maintained at 40 ℃ for five minutes,then increased at a rate of 50 ℃ per minute to 200 ℃,and maintained at 200 ℃ for at least 11 minutes.The injection temperature was maintained at 160 ℃.The detector temperature was maintained at 280 ℃.The split ratio was 5∶1.Results：Five residual solvents were completely separated and excellent linearity and recoveries were obtained.Conclusion：The method is sensitive,accurate,rapid and suitable for quality control.