国产酚磺乙胺的有关物质研究

目的建立测定酚磺乙胺中有关物质的HPLC方法,并对主要未知杂质进行定性研究。方法采用Agilent ZORBAX NH2(4.6 mm×250 mm,5μm)色谱柱,以甲醇-0.2%磷酸二氢钾溶液(10:90)为流动相,检测波长220 nm,流速1.0 mL·min-1;对已知杂质进行定性、定量分析;未知杂质用制备液相色谱纯化,再采集质谱和核磁共振谱的数据,用于结构确定。结果在选定的色谱条件下,酚磺乙胺与各杂质峰均能良好地分离,方法学考察符合分析检测要求。根据质谱和核磁共振谱数据,分离提纯的未知杂质的结构得到初步确认。结论建立的方法简便、灵敏,专属性好,可同时测定酚磺乙胺中的已知杂质及其他未知杂质;未知杂质结构的确定,为酚磺乙胺的质量控制提供了理论依据。

Related substances of domestic etamsylate

Objective To establish an HPLC method to determine the related substances of etamsylate, and to determine the structure of unknown impurity. Methods The Agilent ZORBAX NH2（4.6 mm×250 mm, 5 μm） column was used, and the mobile phase was consisted of methanol-0.2% potassium dihydrogen phosphate solution（10 ：90）. The fl ow rate was 1.0 mL · min^- 1 with UV detective wavelength at 220 nm. Preparative liquid chromatograph was usedto obtain pure unknown impurity, and fi gure out its structure through LC/MS and NMR. Results Etamsylate and impurities were well separated under selected liquid chromatographic system. The methodological study conformed to the requirements for analysis. According to MS and NMR spectral data, the structure of unknown impurities was identified. Conclusion The method is simple, sensitive, specific, which can be used to determine simultaneously known and unknown impurities in etamsylate. The structure identification of unknown impurities provides a theoretical basis for the quality control of etamsylate.