Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, The British University in Egypt, El-Sherouk City, Cairo 11837, Egypt.
The Center for Drug Research and Development (CDRD), Faculty of Pharmacy, The British University in Egypt, El-Sherouk City, Cairo 11837, Egypt.
J AOAC Int. 2023 May 3;106(3):794-803. doi: 10.1093/jaoacint/qsac143.
Dapagliflozin is a sodium glucose cotransporter-II inhibitor while saxagliptin is a dipeptidyl peptidase-4 inhibitor. Both are used to manage type 2 diabetes mellitus.
The aim of this work is to develop four simple, accurate, and precise UV-spectrophotometric methods, three univariate and one multivariate, for the estimation of dapagliflozin and saxagliptin in their pure and marketed dosage forms.
Method (A) is based on the ratio difference method; Method (B) is ratio subtraction with constant multiplication; while Method (C) is a second derivative method and Method (D) is a partial least-squares method.
The calibration curves for dapagliflozin and saxagliptin were linear within the concentration range of 2.50-50.0 μg/mL and 5.0-60.0 μg/mL, respectively. The specificity of the proposed methods was studied by analyzing different laboratory-prepared mixtures and their combined pharmaceutical dosage form. According to the International Council for Harmonisation guidelines, the three proposed methods were validated regarding the accuracy, precision, and specificity. Method (D), partial least-squares, was employed for the determination of the same mixture over a wavelength range of 205-300 nm. A statistical comparison was performed between the results of the proposed methods and those of a reported spectrophotometric method and no statistically significant difference was detected at 95% confidence limit regarding both precision and accuracy.
Four accurate, specific, and precise UV-spectrophotometric methods for dapagliflozin and saxagliptin testing and estimation were successfully utilized and validated.
The examined methods are simple and do not involve sophisticated and expensive instruments. They could be effectively employed in quality control laboratories for routine examination of the investigated drugs in their pure powdered or combined pharmaceutical formulations.
达格列净是一种钠-葡萄糖协同转运蛋白 2 抑制剂，而沙格列汀是一种二肽基肽酶-4 抑制剂。两者均用于治疗 2 型糖尿病。
本工作旨在开发四种简单、准确和精密的紫外分光光度法，三种单变量法和一种多变量法，用于达格列净和沙格列汀在其纯品和市售制剂中的测定。
方法（A）基于比值差法；方法（B）是带常数乘法的比值减法；而方法（C）是二阶导数法，方法（D）是偏最小二乘法。
达格列净和沙格列汀的校准曲线在 2.50-50.0μg/mL 和 5.0-60.0μg/mL 的浓度范围内均呈线性。通过分析不同的实验室制备混合物及其组合的药用制剂，研究了所提议方法的专属性。根据国际协调理事会的指南，对所提议的三种方法的准确性、精密度和专属性进行了验证。方法（D），即偏最小二乘法，用于在 205-300nm 的波长范围内测定相同的混合物。对所提议方法的结果与已报道的分光光度法的结果进行了统计学比较，在 95%置信限内，两种方法在精密度和准确性方面均无统计学差异。
成功地利用和验证了四种用于达格列净和沙格列汀检测和定量的准确、特异和精密的紫外分光光度法。
所检查的方法简单，不涉及复杂和昂贵的仪器。它们可有效地用于质量控制实验室，用于对研究药物的纯品粉末或组合药用制剂进行常规检查。
