螺内酯片有关物质检测方法的优化

Improvement of Determination Method for Related Substance in Spironolactone Tablets

目的优化螺内酯片有关物质的测定方法和供试品溶液制备方法。方法采用Welch Materials Eclipse XB-C18色谱柱(4.6 mm×250 mm,5μm),以乙腈-水(54∶46)为流动相,流速1.0 mL·min^(–1),检测波长254 nm和283 nm,柱温35℃。样品以流动相为提取溶剂,超声提取。结果主峰与各杂质峰均能良好分离。螺内酯、坎利酮分别在1.00~100.38,1.03~102.53μg·mL^(–1)内线性关系良好(r均为1.000),回收率分别为99.52%和99.23%。结论本方法结果准确、重复性好、专属性强,比中国药典方法操作更简便,可为螺内酯片有关物质检测方法的优化提供参考依据。

OBJECTIVE To improve the method for related substance determination and sample preparation of spironolactone tablets.METHODS The detection method was performed on the column of Welch Materials Eclipse XB-C18column(4.6 mm×250 mm,5μm)with mobile phase of acetonitrile-water(54∶46)at flow rate of 1.0 mL·min^(–1),detection wavelengths was 254 nm and 283 nm,column temperature was 35℃.The samples were extracted by flow phase ultrasonic method.RESULTS Related substances were completely separated from the principal component.The linear range of spironolactone and canrenone were 1.00–100.38μg·mL^(–1) and 1.03–102.53μg·mL–1(r=1.000),respectively.The average recovery rates were 99.52%and 99.23%,respectively.CONCLUSION The method is simple,accurate,reproducible and more convenient than the Chinese Pharmacopoeia method,which can provide reference for the optimization of the determination method of spironolactone tablets in the future.