Abbas Noha S, Derayea Sayed M, Omar Mahmoud A, Saleh Gamal A
Ministry of Health and Population Assiut Egypt
Department of Analytical Chemistry, Faculty of Pharmacy, Minia University Egypt.
RSC Adv. 2020 Nov 9;10(67):40795-40805. doi: 10.1039/d0ra05628f.
Herein, a sensitive and reliable eco-friendly TLC-spectrodensitometric method has been established for the simultaneous determination of dapagliflozin (DAPA) and rosuvastatin (ROSV) for the first time. TLC separation was carried out on silica gel F using ethyl acetate : methanol (5 : 0.1, v/v) as a mobile phase and UV measurement at 243 nm. The method was fully validated according to ICH guidelines. Acceptable separation was achieved with values of 0.23 and 0.44 for DAPA and ROSV, respectively. Regression plots revealed linear relationships in the concentration range 20-2500 ng per band and 10-2500 ng per band with LODs of 6.60 and 3.57 ng per band for both DAPA and ROSV, respectively. The relative standard deviations (RSDs%) were found to be 1.35 and 0.53 for DAPA and ROSV, respectively. Moreover, kinetic studies were conducted for measurement of degradation rate constant () and half life time ( ) of DAPA and ROSV forced photo-degradation.
在此，首次建立了一种灵敏、可靠且环保的薄层色谱-分光密度法，用于同时测定达格列净（DAPA）和瑞舒伐他汀（ROSV）。在硅胶F板上进行薄层色谱分离，以乙酸乙酯∶甲醇（5∶0.1，v/v）作为流动相，并在243nm处进行紫外测定。该方法根据国际协调会议（ICH）指南进行了全面验证。达格列净和瑞舒伐他汀的分离度分别为0.23和0.44，实现了可接受的分离效果。回归曲线显示，在每条带20 - 2500 ng和10 - 2500 ng的浓度范围内呈线性关系，达格列净和瑞舒伐他汀的检测限分别为每条带6.60 ng和3.57 ng。达格列净和瑞舒伐他汀的相对标准偏差（RSDs%）分别为1.35和0.53。此外，还进行了动力学研究，以测定达格列净和瑞舒伐他汀强制光降解的降解速率常数（）和半衰期（）。
