Abdallah Nora A, Fathy Mona E, Tolba Manar M, El-Brashy Amina M, Ibrahim Fawzia A
Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Mansoura University, Mansoura 35516, Egypt.
Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Mansoura University, Mansoura 35516, Egypt.
Spectrochim Acta A Mol Biomol Spectrosc. 2023 Aug 5;296:122670. doi: 10.1016/j.saa.2023.122670. Epub 2023 Mar 28.
Recently, Chemometric calibration methods in spectrophotometric analysis are achieving significant attention in the quality control of resolving drug mixtures and pharmaceutical formulations containing two or more drugs with overlapping spectra. The simple univariate methods have been used over the last few decades and has proven to be highly efficient and easy to apply. In this study, a comparative study was performed between some univariate and multivariate methods to determine if chemometric methods can substitute univariate methods in pharmaceutical analysis. In this study, three chemometric techniques were compared to seven univariate techniques to resolve a mixture of mefenamic acid and febuxostat in their raw materials, dosage forms and spiked human plasma. Mefenamic acid and febuxostat were used together for treatment of gout. The applied chemometric methods are partial least squares (PLS), artificial neural network (ANN) and genetic algorithm partial least squares (GA-PLS), while the used univariate methods include first derivative, second derivative, ratio spectra, derivative ratio spectra, ratio subtraction, Q-Absorbance ratio and mean centering spectrophotometric methods. The ten proposed methods were found to be green, sensitive, and rapid. They are simple and did not require any pre-separation steps. The results of both univariate and multivariate approaches were statistically compared with the reported spectrophotometric methods using student's t test and ratio variance F-test. They were also compared with each other, using one-way analysis of variance (ANOVA). These methods were assessed and validated according to ICH guidelines. The studied drugs were analyzed in their pharmaceutical dosage forms and spiked human plasma with good recoveries using the developed methods, which qualify them for routine quality control of the studied drugs.
最近，分光光度分析中的化学计量校准方法在解决药物混合物以及含有两种或更多种光谱重叠药物的药物制剂的质量控制方面受到了极大关注。在过去几十年中一直使用简单的单变量方法，并且已证明其高效且易于应用。在本研究中，对一些单变量和多变量方法进行了比较研究，以确定化学计量方法是否可以在药物分析中替代单变量方法。在本研究中，将三种化学计量技术与七种单变量技术进行比较，以解析甲芬那酸和非布司他在其原料、剂型和加标人血浆中的混合物。甲芬那酸和非布司他一起用于治疗痛风。应用的化学计量方法有偏最小二乘法（PLS）、人工神经网络（ANN）和遗传算法偏最小二乘法（GA-PLS），而使用的单变量方法包括一阶导数、二阶导数、比率光谱、导数比率光谱、比率减法、Q-吸光度比率和平均中心化分光光度法。发现所提出的十种方法环保、灵敏且快速。它们简单且不需要任何预分离步骤。使用学生t检验和比率方差F检验，将单变量和多变量方法的结果与已报道的分光光度法进行统计学比较。还使用单向方差分析（ANOVA）将它们相互比较。这些方法根据国际协调会议（ICH）指南进行了评估和验证。使用所开发的方法对所研究药物的剂型和加标人血浆进行分析，回收率良好，这使它们有资格用于所研究药物的常规质量控制。
