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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 the separation and determination of five organic solvents in alfuzosin hydrochloride. Methods: The internal standard method was used to separate the capillary gas chromatography with FID detector. The column was DB-624 capillary column (30m × 0.53mm × 3.0μm) with nitrogen gas as the carrier gas. The temperature was kept at 40 ℃ for 5min Then ramped to 200 ° C at a rate of 50 ° C .min-1 for at least 11 min. Inlet temperature 160 ° C, detector temperature 280 ° C, split ratio 5: 1. Residues of methanol, ethanol, acetone, methylene chloride and N, N-dimethylformamide in the alfuzosin hydrochloride raw material were determined. Results: The five organic solvents were completely separated. The potential impurities in the sample did not interfere with the detection of five kinds of organic solvents. The linearity was good and the recovery of sample was satisfactory. Conclusion: The method is sensitive, accurate and rapid and is suitable for the determination of residual organic solvents in alfuzosin hydrochloride.