Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Al-Azhar University, 11751 Nasr City, Cairo, Egypt.
Department of Pharmacology and Toxicology, Taif University, P.O. Box 11099, Taif 21944, Saudi Arabia; Addiction and Neuroscience Research Unit, Health Science Campus, Taif University, P.O. Box 11099, Taif 21944, Saudi Arabia.
Spectrochim Acta A Mol Biomol Spectrosc. 2025 Jan 15;325:125123. doi: 10.1016/j.saa.2024.125123. Epub 2024 Sep 10.
The fixed dose combination of Rosuvastatin and ezetimibe has recently received approval from the FDA for the treatment of elevated levels of low-density lipoprotein cholesterol in adults. Herein, an eco-friendly and highly sensitive spectrofluorimetric method was developed and validated for simultaneous determination of rosuvastatin and ezetimibe in commercial capsules. The developed method involved synchronous fluorescence spectroscopy combined with second derivative spectroscopy to resolve the overlapping fluorescence spectra of rosuvastatin and ezetimibe. The studied drugs were measured in synchronous mode at Δλ of 40 and their recorded synchronous fluorescence spectra were derivatized into second-order spectra, enabling the selective quantification of rosuvastatin and ezetimibe at 370 nm and 312 nm, respectively. Optimization studies regarding to the influence of buffer pH, incorporation of surfactant, choice of diluting solvent, and synchronous Δλ were carried out. The method was validated using the validation characteristics listed in ICH Q2(R1). The calibration curves displayed satisfactory linear relationships across the calibration range of 0.1-2 µg/mL for rosuvastatin and 0.05-3 µg/mL for ezetimibe. The methodology demonstrated robustness to minor modifications in the procedural parameters and selectivity in quantifying the studied drugs in synthetic mixed solutions and commercial capsules without interference. Furthermore, the level of environmental friendliness and sustainability of the suggested spectrofluorimetric approach was assessed in relation to two previously documented methodologies utilizing the AGREE metric. The findings indicated that the suggested method demonstrated a notably superior level of sustainability in comparison to the documented methods.
瑞舒伐他汀和依折麦布的固定剂量组合最近获得了 FDA 的批准，可用于治疗成年人的低密度脂蛋白胆固醇升高。在此，开发并验证了一种环保且高灵敏度的荧光分光光度法，用于同时测定商业胶囊中的瑞舒伐他汀和依折麦布。所开发的方法涉及同步荧光光谱法和二阶导数光谱法相结合，以解析瑞舒伐他汀和依折麦布重叠的荧光光谱。在同步模式下，以 Δλ 为 40 测量研究药物，并将其记录的同步荧光光谱衍生为二阶光谱，从而能够分别在 370nm 和 312nm 处选择性地定量测定瑞舒伐他汀和依折麦布。对缓冲液 pH 值、表面活性剂的加入、稀释溶剂的选择和同步 Δλ 的影响进行了优化研究。该方法使用 ICH Q2(R1) 中列出的验证特性进行了验证。校准曲线在瑞舒伐他汀的校准范围为 0.1-2μg/mL 以及依折麦布的校准范围为 0.05-3μg/mL 时呈现出令人满意的线性关系。该方法在对程序参数进行微小修改时表现出稳健性，并且在对合成混合溶液和商业胶囊中的研究药物进行定量时具有选择性，没有干扰。此外，还使用 AGREE 指标评估了所建议的荧光分光光度法相对于之前记录的两种方法在环境友好性和可持续性方面的水平。结果表明，与已记录的方法相比，所建议的方法在可持续性方面具有明显的优势。
