甲硝唑有关物质测定及杂质谱研究

摘要

目的 建立甲硝唑原料药有关物质的高效液相色谱测定方法和杂质谱.方法 采用Welch Ultimate(R)XB-C18色谱柱(4.6 mm×250 mm,5 μm);以甲醇-1.36 g·L-1磷酸二氢钾溶液(20∶80)为流动相;流速1 mL·min-1;检测波长:315 nm,主成分自身对照法测定有关物质.结果 甲硝唑与有关物质具有良好的分离度,对近6年生产的20批样品进行了测定,均满足质量控制标准.杂质谱的研究能有效监控甲硝唑合成工艺和杂质变化情况.结论 该方法简便、快速、灵敏,能有效控制甲硝唑原料药中有关物质,同时杂质谱研究有助于保证甲硝唑质量稳定性检测.%Objective To establish HPLC determination method and impurity profile of the related substances in metronidazole.Methods A Welch Ultimate(R)XB-C1s (4.6 mm× 250 mm,5 μm)was used with a mobile phase consisting of methanol-1.36 g· L-1 solution of potassium dihydrogen phosphate (20∶ 80).The detection wavelength was 315 nm and the flow rate was 1 mL· min-1.Its related substances were determined by principal component self-contrast method.Results Good separation of metronidazole and the impurities could be achieved.Twenty batches of samples in the past six years were determined which meet quality standards.The study of impurity profiles could effectively monitor the synthetic process and the change of impurities in metronidazole.Conclusion The method is simple,quick and sensitive,which can be used to control the related substances in metronidazole.Meanwhile,the impurity profiles ensure the quality stability of metronidazole.