Department of Chemistry, Faculty of Science, University of Karachi, Karachi, Pakistan/Alexander Butlerov Institute of Chemistry, Kazan Federal University, 18 Kremlevskaya Street, Kazan, Russian Federation.
H.E.J. Research Institute of Chemistry, International Center for Chemical and Biological Sciences, University of Karachi, Karachi, Pakistan.
Pak J Pharm Sci. 2024 May;37(3):491-498.
This study introduces an innovative, and rapid HPLC method using reverse phase elution for the simultaneous analysis of Sitagliptin and Metformin HCl in pharmaceutical formulations. This combination was explored in bulk and solid dosage forms using Luna Phenomenex C8 column (4.6 x 250 mm, 5 µm) at ambient temperature in isocratic elution. It was found that the mobile phase comprising of 0.1% ortho-phosphoric acid, potassium dihydrogen phosphate buffer (pH 3.0) and acetonitrile in ratios 35:35:30, showed a symmetrical peak for Sitagliptin and Metformin HCl. The detection was carried out at 210nm, using a flow rate of 1.0mL/min. The method was linear over the concentration range for Sitagliptin 2.5-7.5 ppm and Metformin HCl 25-75 ppm. The assay recoveries of Sitagliptin and Metformin were found to be 100.36% and 100.20%, respectively. The LOD and LOQ for the Sitagliptin were found to be 0.201 ppm and 0.301 ppm and for Metformin HCl 0.101 ppm and 0.303 ppm, respectively. The proposed methods can be implemented for controlling quality in bulk and solid dosage forms. The analytical methods were validated as per the guideline of ICH Q2 (R2). The developed HPLC methods were effectively employed for the determination of combined dosage forms in pharmaceutical formulations.
本研究介绍了一种创新的、快速的反相高效液相色谱法，用于同时分析药物制剂中的西他列汀和盐酸二甲双胍。在室温下，使用 Luna Phenomenex C8 柱（4.6×250mm，5μm），在等度洗脱条件下，对原料药和固体制剂中的该组合进行了研究。结果表明，流动相由 0.1%邻磷酸、磷酸二氢钾缓冲液（pH3.0）和乙腈以 35:35:30 的比例组成，对西他列汀和盐酸二甲双胍显示出对称的峰。检测波长为 210nm，流速为 1.0mL/min。西他列汀在 2.5-7.5ppm 浓度范围内，盐酸二甲双胍在 25-75ppm 浓度范围内呈线性关系。西他列汀和盐酸二甲双胍的回收率分别为 100.36%和 100.20%。西他列汀的检出限和定量限分别为 0.201ppm 和 0.301ppm，盐酸二甲双胍的检出限和定量限分别为 0.101ppm 和 0.303ppm。所提出的方法可用于控制原料药和固体制剂的质量。分析方法按照 ICH Q2（R2）指南进行了验证。所开发的 HPLC 方法有效地用于药物制剂中组合剂型的测定。
