Assay of valdecoxib reference substance by nuclear magnetic resonance spectroscopy
FENG Yu-fei
ZHAI Chen-fei
JIN Zhi-shang
NIU Jian-zhao
SUN Hui-min
Abstract：Objective:To establish 1H quantitative nuclear magnetic resonance(1H qNMR)method for determination of the content of valdecoxib reference substance.Methods:For 1H qNMR,a Bruker Avance Ⅲ HD 500 superconducting nuclear magnetic resonance spectrometer was used with deudimethyl sulphone as solvent and noesyigldld pulse sequence with relaxation delay time of 30 s and 32 scanning times.Results:The signals 87.84 of valdecoxib and δ6.09 of 1,3,5-trimethoybenzene were used for quantitation.The linear regression equation of response area ratio of internal standard signal and molar ratio of hydrogen atom was y=0.992 2x+0.002 3,the correlation coefficient was 0.999 7,and the RSD of repeatability experiment was 0.12％(n=5).The content of vadoxib(C16H14N2O3S)was 99.25％,which was consistent with the results by mass balance method(99.61％)and HPLC assay method(99.87％).Conclusion:The nuclear magnetic quantitative method established in this paper can be used for the determination of vadoxib content.It is accurate and rapid,providing a strong evidence for the determination of reference material by mass balance method.
Keywords：valdecoxibcontent assaychemical reference standard1H quantitative nuclear magnetic resonance
Publication Date：2024-11-30
Online Publishing Date：2026-08-14(First online date of this platform, not the publication date of the document)
Pages：4( 2400-2403 )