Department of Occupational Health, Faculty of Public Health and Health Informatics, Umm AL-Qura University, Makkah, Saudi Arabia; Department of Chemistry, Faculty of Science, Zagazig University, 44519 Zagazig, Egypt.
Poison control and Medical Forensic Chemistry Center, Makkah, Saudi Arabia.
Ann Pharm Fr. 2021 Jul;79(4):395-408. doi: 10.1016/j.pharma.2020.11.002. Epub 2020 Nov 19.
The present study aims to develop and validate four simple, sensitive, reproducible, and low-cost spectrophotometric methods for the determination of antimigraine drug (eletriptan hydrobromide) in pure form and pharmaceutical formulations.
The methods are based on the formation of yellow colored ion-pair complex between eletriptan hydrobromide and four acid dyes, namely, bromocresol purple (BCP), bromocresol green (BCG), bromophenol blue (BPB), and bromothymol blue (BTB) with absorption maxima at 410, 420, 414 and 416nm, respectively. Several parameters such as pH, buffer type and volume, reagent volume, sequence of addition and effect of extracting solvent were optimized.
Under the optimum experimental conditions, beer's law is obeyed over the concentration ranges of 1.0-20 and 1.0-16μgmL for (BCP or BCG) and (BPB or BTB), respectively with good correlation coefficients (0.9995-0.9999). The apparent molar absorptivity and Sandell's sensitivity values are reported for all methods. The limit of detection (LOD) and the limit of quantification (LOQ) values are found to be 0.27, 0.28, 0.25, and 0.30μgmL and 0.90, 0.93, 0.83, and 1.0μgmL for BCP, BCG, BPB and BTB, respectively. The stoichiometric ratio of the formed ion-pair complexes was found to be 1:1 (drug: reagent) for all methods.
The developed methods were successfully applied for the determination of eletriptan hydrobromide in pharmaceutical formulations with good accuracy and precision. Statistical comparison of the results was performed using Student's t-test and variance ratio F-test at the 95% confidence level and there was no significant difference between the reported and proposed methods regarding accuracy and precision. Further, the validity of the proposed methods was confirmed by recovery studies via standard addition method.
本研究旨在开发和验证四种简单、灵敏、重现性好且成本低的分光光度法，用于测定纯品和药物制剂中的抗偏头痛药物（依来曲普坦氢溴酸盐）。
这些方法基于依来曲普坦氢溴酸盐与四种酸性染料（溴甲酚紫（BCP）、溴甲酚绿（BCG）、溴酚蓝（BPB）和溴百里酚蓝（BTB））形成黄色离子对配合物，其吸收最大值分别为 410、420、414 和 416nm。优化了 pH、缓冲液类型和体积、试剂体积、添加顺序以及萃取溶剂的影响等参数。
在最佳实验条件下，BCP 或 BCG 方法的浓度范围为 1.0-20μgmL 时，BPB 或 BTB 方法的浓度范围为 1.0-16μgmL 时，比尔定律均成立，相关系数良好（0.9995-0.9999）。报告了所有方法的表观摩尔吸光系数和桑德尔灵敏度值。发现所有方法的检出限（LOD）和定量限（LOQ）值分别为 0.27、0.28、0.25 和 0.30μgmL 和 0.90、0.93、0.83 和 1.0μgmL 用于 BCP、BCG、BPB 和 BTB。发现所有方法形成的离子对配合物的化学计量比均为 1:1（药物：试剂）。
所开发的方法成功应用于药物制剂中依来曲普坦氢溴酸盐的测定，具有良好的准确性和精密度。在 95%置信水平下，使用学生 t 检验和方差比 F 检验对结果进行了统计学比较，报告的方法和提出的方法在准确性和精密度方面没有显著差异。此外，通过标准加入法回收研究验证了所提出方法的有效性。
