阿司匹林双嘧达莫片溶出度及含量测定方法研究

A Research of Dissolution and Content Determination Method of Aspirin and Dipyridamole Tablets

建立了阿司匹林双嘧达莫片溶出度和含量的测定方法。采用Amethyst C18-H色谱柱(4.6 mm×250 mm,5μm),以磷酸盐缓冲液-甲醇-乙腈为流动相,梯度洗脱,流速1.0 mL/min,检测波长235 nm。溶出度实验采用篮法,以0.1 mol/L盐酸溶液和磷酸盐缓冲液(pH 6.8)为溶出介质。结果表明:溶出度实验中双嘧达莫、阿司匹林和水杨酸质量浓度分别在0.5508~49.57、1.668~150.1和0.2004~18.04μg/mL范围内线性关系良好(r^(2)≥0.9998),回收率在97.7%~102.0%之间(RSD≤1.0%,n=6)。含量测定实验中阿司匹林和双嘧达莫质量浓度分别在29.71~267.4μg/mL和10.42~93.78μg/mL范围内线性关系良好(r2≥0.9999),回收率在98.1%~101.0%之间(RSD<1.0%,n=9)。本方法准确性好、精密度高、操作简单,适用于阿司匹林双嘧达莫片溶出度和含量测定。

A method was established for the determination of the dissolution and content of aspirin and dipyridamole in the tablets.The separation was performed on an Amethyst C18-H(4.6 mm×250 mm,5μm)column with flow rate of 1.0 mL/min.Phosphate buffer,methanol and acetonitrile were used as the mobile phase in gradient elution and the detection wavelength was set at 235 nm.The basket method was adopted in the dissolution test,and the dissolution amount of dipyridamole and aspirin was determined with the dissolution medium of 0.1 mol/L hydrochloric acid solution then phosphate buffer(pH 6.8).In the dissolution test,the concentrations of dipyridamole,aspirin and salicylic acid were 0.5508-49.57,1.668-150.1 and 0.2004-18.04μg/mL,respectively.And the corresponding linear correlation coefficients were no less than 0.9998.The recovery rates were between 97.7%and 102.0%and the relative standard deviations were not exceeded 1.0%(n=6).In the content determination test,the concentrations of aspirin and dipyridamole were 29.71-267.4 and 10.42-93.78μg/mL respectively,and the corresponding linear correlation coefficients were no less than 0.9999.The recovery rates were between 98.1%and 101.0%and the relative standard deviations were less than 1.0%(n=9).This simple and precise method was applied successfully to the determination of dissolution and content of aspirin and dipyridamole tablets.