Determination of parecoxib sodium mass fraction by 1H qNMR
Objective:To establish an 1H quantitative nuclear magnetic resonance(1H qNMR)method for the determination of parecoxib sodium.Methods:1H qNMR spectra were obtained in DMSO-d6 by using Bruker Ascend 600 spectrometer with zg30 pulse sequence,the relaxation delay time was 30 s,and 64 scans were recorded.Results:The signals δ7.74 of parecoxib sodium and δ6.23 of maleic acid were used for quantitation.Linear regression of areas ratio versus mass ratio yielded a correlation coefficient of 0.999 7 and regression equation of y=0.296 2x-0.001 0,the repeatability RSD was 0.15％(n=6),and the mass fraction of parecoxib(C19H17 N2O4S-)was 93.91％,which was consistent with the results by mass balance method(93.83％)and HPLC assay method(93.89％).Conclusion:The established 1H qNMR method can be used for the quantitative determination of parecoxib sodium.It is accurate and rapid and could be complementary to the mass balance method for the assay of reference substances.
1H quantitative nuclear magnetic resonancemass fraction assaychemical reference standardparecoxib sodium
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