Content Determination of Celecoxib by ¹H and ¹⁹F Quantitative Nuclear Magnetic Resonance

OBJECTIVE To determine the content of celecoxib by ¹H quantitative nuclear magnetic resonance and ¹⁹F quantitative nuclear magnetic resonance, and compare the results of the two methods of quantitative nuclear magnetic resonance with mass balance method. METHODS CD₃OD was employed as solvent, proton signal peaks of celecoxib at δ 6.92 and δ 6.33 of maleic acid were served as quantitative peaks and inner peak, respectively. The spectra of the mixture were collected at 10 s relaxation delay, 4.01 s acquisition time and 32 scanning times. In the ¹⁹F quantitative fluorine nuclear magnetic resonance, CD₃OD was used as solvent, 4-bromo-2-fluoroacetanilide was employed as internal standard, the spectra were obtained with spectral width of 240 ppm, transmitter frequency offset was -94.26 ppm and the scanning times was 16. The results of ¹H quantitative nuclear magnetic resonance and ¹⁹F quantitative nuclear magnetic resonance were calculated. RESULTS The results of ¹H quantitative nuclear magnetic resonance and ¹⁹F quantitative nuclear magnetic resonance were very close, which were generally consistent with that of the mass balance method. CONCLUSION Quantitative nuclear magnetic resonance can be used for the quantitative determination of celecoxib with the superiority of accurate and effective.