Department of pharmaceutical analytical chemistry, faculty of pharmacy, Tanta university, Tanta, Egypt.
Chemistry department, faculty of science, Zagazig university, 44519 Zagazig, Egypt.
Ann Pharm Fr. 2021 Jan;79(1):16-27. doi: 10.1016/j.pharma.2020.08.003. Epub 2020 Aug 24.
The present work aims to develop and validate a simple, rapid, cost-effective, sensitive and extractive spectrophotometric methods for the determination of phosphodiesterase type 5-inhibitor; vardenafil HCl (VARD) in pure and in dosage forms.
The developed methods are based on the formation of ion-pair complexes between vardenafil HCl and dyes, namely, bromocresol green (BCG), bromocresol purple (BCP), bromophenol blue (BPB), bromothymol blue (BTB) and eriochrom black T (EBT) in acidic buffer solutions. Different factors affecting the reactions between VARD and the dyes were studied and optimized.
The formed complexes were extracted with methylene chloride and measured at 418, 410, 415, 417 and 520nm using BCG, BCP, BPB, BTB and EBT, respectively. The beer's law was obeyed in the ranges 1.0-10, 1.0-16, 0.5-8.0, 2.0-20 and 1.0-14μgmL for BCG, BCP, BPB, BTB and EBT, respectively under the optimum conditions. The composition of the ion-pairs was found 1:1. The molar absorptivity's, Sandell's sensitivity, limits of detection and the limits of quantification were calculated. Other method validation parameters, such as accuracy, intra-day and inter-day precision, robustness, ruggedness and selectivity, have been evaluated.
The proposed methods have been applied successfully for the analysis of vardenafil HCl in pure and dosage forms. The reliability of the methods was further ascertained by performing recovery studies using the standard addition method. Statistical comparison of the results with the reported method was performed by applying student's t- and F-tests and no significant statistical differences were obtained.
本工作旨在开发和验证一种简单、快速、经济、灵敏且具有提取能力的分光光度法，用于测定磷酸二酯酶 5 抑制剂；盐酸伐地那非（VARD）的纯品和制剂。
所开发的方法基于盐酸伐地那非与染料，即溴甲酚绿（BCG）、溴甲酚紫（BCP）、溴酚蓝（BPB）、溴百里酚蓝（BTB）和铬黑 T（EBT）在酸性缓冲溶液中形成离子对复合物。研究并优化了影响 VARD 与染料反应的各种因素。
在最佳条件下，用 BCG、BCP、BPB、BTB 和 EBT 分别于 418、410、415、417 和 520nm 处用二氯甲烷萃取形成的配合物，并进行测量。在 1.0-10、1.0-16、0.5-8.0、2.0-20 和 1.0-14μgmL 范围内，BCG、BCP、BPB、BTB 和 EBT 均符合比尔定律。确定了离子对的组成是 1:1。计算了摩尔吸光系数、桑德尔灵敏度、检测限和定量限。还评估了其他方法验证参数，如准确度、日内和日间精密度、稳健性、耐用性和选择性。
所提出的方法已成功应用于纯品和制剂中盐酸伐地那非的分析。通过使用标准加入法进行回收研究，进一步确定了方法的可靠性。通过应用学生 t-检验和 F-检验对结果与已报道方法进行统计学比较，未发现显著统计学差异。
