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[摘要]
目的 建立核磁共振氢谱法测定槲皮素原料药的绝对含量。方法 以DMSO-d6 为溶剂,马来酸为内标,采集槲皮素和马来酸混合物的核磁共振氢谱。以槲皮素中化学位移在δ7.50~7.58和马来酸化学位移在δ6.26的质子信号峰为定量峰,测定槲皮素的量,并与质量平衡法比较。结果 槲皮素与马来酸峰的面积比(As/Ar)与其质量比(ms/mr)的线性回归方程为y=2.963 x+0.134 1(r=0.999 3)。测得3批槲皮素的质量分数分别为85.20%、84.93%和85.27%,平均质量分数为85.13%,RSD为0.21%。测定结果与质量平衡法定值基本一致。结论 所建立的氢核磁共振定量法准确、快速,为质量平衡法提供有力佐证。
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[Abstract]
Objective To establish a novel method to determine the absolute content of quercetin by proton nuclear magnetic resonance (qNMR). Methods DMSO-d6 was employed as solvent, and maleic acid as an internal standard. Proton signal peaks at δ7.50-7.58 and δ6.26 of maleic acid were served as quantification peaks. The content of quercetin is determined with qNMR in comparison with the results obtained by mass balance method. Results Linear regression of quantitative peak areas ratio (As/Ar) of quercetin-maleic acid vs mass ratio (ms/mr) yielded a correlation coefficient of 0.999 3 and a regression equation of y=2.963 x+0.134 1. The contents of three batches quercetin were 85.20%, 84.93%, and 85.27%,the average was 85.13% and its RSD was 0.21%. The results were generally consistent with that of mass balance methods. Conclusion This method was easy and simple to handle, and the analysis results were accurate. It could be the complementary for the mass balance method.
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