达帕格列嗪
色谱法
化学
杂质
色谱检测器
降级(电信)
乙腈
高效液相色谱法
质谱法
分析化学(期刊)
有机化学
医学
电信
计算机科学
2型糖尿病
糖尿病
内分泌学
作者
Ali Ismail,Mohammad Haroun,Youssef Alahmad
标识
DOI:10.21123/bsj.2023.7596
摘要
Dapagliflozin is a novel sodium-glucose cotransporter type 2 inhibitor. This work aims to develop a new validated sensitive RP-HPLC coupled with a mass detector method for the determination of dapagliflozin, its alpha isomer, and starting material in the presence of dapagliflozin major degradation products and an internal standard (empagliflozin). The separation was achieved on BDS Hypersil column (length of 250mm, internal diameter of 4.6 mm and 5-μm particle size) at a temperature of 35℃. Water and acetonitrile were used as mobile phase A and B by gradient mode at a flow rate of 1 mL/min. A wavelength of 224nm was selected to perform detection using a photo diode array detector. The method met the requirement of the International Conference on Harmonisation for Registration of Pharmaceuticals for Human Use (ICH) for validation. The molecular weight of impurities and degradation products was estimated using positive ESI-MS. Fifteen impurities were detected during the analysis of dapagliflozin APIs and the brand Farxiga ® and some generic products. Three of fifteen detected impurities (H, J and K) exceeded the impurities acceptable limits 0.1%. Those impurities were isolated using new preparative chromatography then characterized using elemental analysis, FTIR and NMR.
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