Department of Analytical Chemistry, Faculty of Pharmacy, Zagazig University, Zagazig, Egypt.
Department of Applied Chemistry, Graduate School of Engineering, Kyushu University, Fukuoka, Japan.
Drug Dev Ind Pharm. 2022 Feb;48(2):41-51. doi: 10.1080/03639045.2022.2093896. Epub 2022 Jul 8.
Two simple and validated chromatographic studies were performed for simultaneous estimation of sildenafil citrate (SIL) and alfuzosin hydrochloride (ALF) in bulk, pharmaceuticals, and in the presence of their main degradation products. Two systems of mobile phase were applied isocratically for their first chromatographic separation using conventional and micellar mobile phases. Methanol, acetonitrile, and 0.02 M potassium dihydrogen phosphate (43:14:43 ; pH 4.66) were pumped at 1.3 mL/min in method I. Meanwhile, method II was based on less hazardous micellar mobile phase of nonionic surfactant (0.005 M Brij-35 in water; pH 2.5 adjusted with 0.1% orthophosphoric acid) with a flow rate of 1 mL/min. Both methods were carried on C18 column and coupled with UV detection at 225 nm at ambient temperature. The first method was rectilinear over the concentration range of 5-62.5 μg/mL for both drugs, while the second method showed higher linearity ranges of 0.5-40, 2.5-62.5 μg/mL for ALF and (SIL), respectively. The developed methods successfully enabled the quantification of the studied binary mixture in their tablets dosage form and evaluation their stabilities. Validation of the proposed methods according to ICH guidelines and system suitability were ascertained. Moreover, the applied methods were evaluated and compared from the perspective of green analytical chemistry, employing the National Environmental Methods Index, analytical Eco-Scale score, and Green Analytical Procedure Index, as three assessment tools.
进行了两项简单且经过验证的色谱研究，旨在同时对枸橼酸西地那非（SIL）和盐酸阿夫唑嗪（ALF）原料药及其主要降解产物进行定量分析。两种流动相体系采用等度洗脱，分别使用常规和胶束流动相进行了第一次色谱分离。方法 I 中，以甲醇、乙腈和 0.02 M 磷酸二氢钾（43:14:43；pH 4.66）为流动相，流速为 1.3 mL/min。同时，方法 II 基于非离子表面活性剂（0.005 M Brij-35 水溶液；pH 2.5 用 0.1%正磷酸调）的危险性较小的胶束流动相，流速为 1 mL/min。两种方法均在 C18 柱上进行，在环境温度下于 225nm 处进行紫外检测。第一种方法对于两种药物的浓度范围在 5-62.5μg/mL 之间呈线性关系，而第二种方法的线性范围分别为 0.5-40μg/mL 和 2.5-62.5μg/mL。所开发的方法成功地实现了片剂制剂中研究的二元混合物的定量，并评估了其稳定性。根据 ICH 指南和系统适用性对提出的方法进行了验证。此外，从绿色分析化学的角度，采用国家环境方法指数、分析生态标度评分和绿色分析程序指数这三种评估工具，对所应用的方法进行了评估和比较。
