Stability-Indicating Spectrofluorimetric and RP-HPLC Methods for the Determination of Aspirin and Dipyridamole in their Combination

H. Hammud, Fawzy A. El Yazbib, M. E. Mahrous, G. Sonji, N. Sonji
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引用次数: 18

Abstract

Spectrofluorimetric and high performance liquid chromatographic methods have been developed for the accu- rate and sensitive determination of Aspirin in mixture with Dipyridamole and in presence of its degradation product (Sali- cylic acid). The spectrofluorimetric method was based on the use of the first and second derivatives of the ratio of the emission spectra with a zero-crossing technique. The ratio spectra were obtained by dividing the emission spectrum of the ternary mixture by that of one of the components. The other components were quantified from their respective calibration graphs treated similarly. The proposed RP-HPLC method utilized an Adsorbosil C8, 10 � m, 250mmx4.6mm i.d. column, at ambient temperature, optimum mobile phase consisted of water-acetonitrile-ortho-phosphoric acid (65:35:2 v/v/v), with flow rate monitored at 1.5 ml/min, and UV detection at 250 nm. The total chromatographic time per sample was about 6 min with dipyridamole, aspirin and salicylic acid eluting at retention times 2.2, 3.8 and 4.6 min, respectively. Evaluation of linearity, accuracy, precision, selectivity and sensitivity of the methods produced satisfactory results. The objective of this work was to introduce new analytical methods for this ternary mixture, as the literature reveals only one method of analysis. The proposed methods were able to quantify Aspirin, Dipyridamole and Salicylic acid, irrespec- tive of the percentage of the latter in sample; and have been successfully applied to the commercial pharmaceutical formu- lations without any interference of excipients.
稳定性指示荧光光谱法和反相高效液相色谱法测定阿司匹林与双嘧达莫联用中的含量
采用荧光光谱法和高效液相色谱法对阿司匹林与双嘧达莫的混合物及其降解产物(沙利环酸)进行了准确、灵敏的测定。荧光光谱法是基于利用零交叉技术的发射光谱比值的一阶导数和二阶导数。比值光谱由三元混合物的发射光谱除以其中一种组分的发射光谱得到。其他成分从各自的校准图中进行定量处理。反相高效液相色谱(RP-HPLC)色谱柱为C8, 10 μ m, 250mmx4.6mm,室温下,最佳流动相为水-乙腈-正磷酸(65:35:2 v/v/v),流速为1.5 ml/min,检测波长为250 nm。每个样品的总色谱时间约为6 min,双嘧达莫、阿司匹林和水杨酸的洗脱时间分别为2.2、3.8和4.6 min。对方法的线性度、准确度、精密度、选择性和灵敏度进行了满意的评价。这项工作的目的是为这种三元混合物介绍新的分析方法,因为文献显示只有一种分析方法。所提出的方法能够定量测定阿司匹林、双嘧达莫和水杨酸,而不考虑后者在样品中的百分比;并已成功应用于商业制剂中,不受辅料的干扰。
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