Quantitative Determination of Empagliflozin by Nuclear Magnetic Resonance

KeyWord:empagliflozin  quantitative NMR  gemcitabine hydrochloride  zidovudine

Abstract:

      A method was established to determine the content of empagliflozin by 1H nuclear magnetic resonance spectroscopy£¨1H-NMR£©£¬using gemcitabine hydrochloride and zidovudine as the internal standard£¬repectively.NMR spectra were recorded using a standard 1D pulse sequence at a 30¡ã flip angle and with DMSO-d6-D2O as the solvent.Thirty two scans of 32 K data points were acquired at a temperature of 303 K£¬a relaxation delay of 20 s and a line broad of 0ª±3 Hz.Under the optimal conditions£¬method validation indicated specificity£¬robustness and stability up to 24 h.A good linear relationship was obtained between peak area ratio and molar ratio of empagliflozin to the internal standard.For gemcitabine£¬the regression equation was y=0.009x-0.003£¨r2=0.999 9£© with a molar ratio range of 0.512 5-1.953 8.For zidovudine£¬the regression equation was y=0.576x-0.026£¨r2=0.999 9£© with a molar ratio range of 0.494 7-1.966 0.The contents of empagliflozin were 99.83%£¨n=3£¬RSD=0.06%£©and 99.77%£¨n=3£¬RSD=0.19%£©corresponding to the internal standards gemcitabine hydrochloride and zidovudine£¬respectively.The results were consistent with each other£¬indicating that the method had the advantages of accuracy£¬high sensitivity and good repeatability£¬and could be used for the quantification of new drugs.