Pharmaceutical Chemistry Department, Faculty of Pharmacy, Cairo University, Kasr El-Aini St., Cairo 11562, Egypt.
Pharmaceutical Chemistry Department, Faculty of Pharmacy, Cairo University, Kasr El-Aini St., Cairo 11562, Egypt.
Spectrochim Acta A Mol Biomol Spectrosc. 2018 Dec 5;205:235-242. doi: 10.1016/j.saa.2018.06.072. Epub 2018 Jun 20.
To maintain intensive glucose control early in the type II diabetes mellitus process, novel combinations of canagliflozin/metformin (CAG/MEF) and empagliflozin/linagliptin (EMG/LIG) offer particular treatment benefits. In this study, sensitive and precise spectrophotometric methods were developed for the determination of such hypoglycemic drug combinations in bulk powder and in pharmaceutical dosage form without prior separation. The first method was ratio difference coupled with modified isosbestic point technique where the amplitude difference between 239 and 291 nm on the ratio spectrum of CAG obtained using 4 μg/ml of MEF as divisor was used for determination of CAG. On the other hand, MEF was estimated using a modified isosbestic spectrophotometric method, where the total concentration of CAG and MEF in mixture could be calculated at 250 nm (isosbestic point) after multiplication by a correction factor. Then concentration of MEF could be calculated by subtraction. The second method was ratio subtraction coupled with extended ratio subtraction, where EMG was determined at 225 nm by subtraction of plateau values from the ratio spectrum followed by multiplication with the spectrum of 6.5 μg/ml of LIG (divisor). Then, an extension of the normal ratio subtraction method was performed in order to determine LIG at 226 nm. Linearity was obtained over 5-30, 2.5-16, 2.5-16 and 1.25-8 μg/ml for CAG, MEF, EMG and LIG, respectively. The developed methods were successfully applied for the determination of studied drugs in tablets. Validation parameters were found to be within acceptance limits, thus confirming methods accuracy and selectivity. The obtained results were statistically compared with the reported one showing no significant difference in terms of accuracy and precision. The methods could be applied for routine analysis of the cited drugs in quality control laboratories.
为了在 2 型糖尿病早期维持强化血糖控制，坎格列净/二甲双胍（CAG/MEF）和恩格列净/利格列汀（EMG/LIG）的新型组合提供了特别的治疗益处。在这项研究中，开发了灵敏和精确的分光光度法，用于在没有预先分离的情况下测定这些降血糖药物组合的散装粉末和药物剂型。第一种方法是比率差与改进的等吸收点技术相结合，其中使用 4μg/ml 的 MEF 作为除数在 CAG 的比值光谱上获得的 239 和 291nm 之间的振幅差用于测定 CAG。另一方面，MEF 是使用改进的等吸收分光光度法测定的，其中混合物中 CAG 和 MEF 的总浓度可以在 250nm（等吸收点）处计算（乘以校正因子）。然后通过减法计算 MEF 的浓度。第二种方法是比率减法与扩展比率减法相结合，其中 EMG 在 225nm 处通过从比值光谱中减去平台值来测定，然后乘以 6.5μg/ml 的 LIG（除数）的光谱。然后，进行正常比率减法的扩展，以便在 226nm 处测定 LIG。对于 CAG、MEF、EMG 和 LIG，线性分别在 5-30、2.5-16、2.5-16 和 1.25-8μg/ml 范围内获得。所开发的方法成功地应用于片剂中研究药物的测定。验证参数均在可接受范围内，从而证实了方法的准确性和选择性。所获得的结果与报道的结果在准确性和精密度方面没有显著差异，进行了统计学比较。该方法可应用于质量控制实验室中引用药物的常规分析。
