Abstract: We established a rapid and accurate method for the content determination of 4-(p-hydroxyphenyl)-2-butanone with quantitative nuclear magnetic resonance. We acquired 1HNMR spectra of the mixture of 4-(p-hydroxyphenyl)-2-butanone and benzoic acid at 25 ℃ with Bruker 400 MHz spectrometer scanning 32 times, DMSO as solution, and benzoic acid as internal standard. Proton signal peaks at δ 6.97 of 4-(p-hydroxyphenyl)-2-butanone and δ 7.95 of benzoic acid served as quantification peaks. Linear regression equation of y=0.197x+0.783 and correlation coefficient of 0.997 were obtained for peak areas ratio y(As/Ar) of 4-(p-hydroxyphenyl)-2-butanone andbenzoic acid and mass ratio x(ms/mr).RSD of 0.47% (n=6), RSD of stability of 0.58%, and RSD of recovery rate of 1.18% were acquired for repeatable tests of content determination.The contents of 3 batches of 4-(p-hydroxyphenyl)-2-butanone were 99.53%, 99.46% and 99.49%. Experimental results show that the concentration of quantitative nuclear magnetic resonance determined 4-(p-hydroxyphenyl)-2-butanone isslightly lower than that by HPLC without reference substance. The method therefore can be used for the content determination and quality control of 4-(p-hydroxyphenyl)-2-butanone. It can also provide references for content determination of other reference substances.

Key words: content determination, 4-(p-hydroxyphenyl)-2-butanone, QNMR