基于~1H-NMR的定坤丹指纹图谱研究

Fingerprint research of Dingkun Dan based on ~1H NMR method

目的建立定坤丹的~1H NMR指纹图谱,为其质量控制提供比较全面快速的评价方法。方法采用600 MHz NMR仪测定,建立10批次定坤丹甲醇水相和氯仿相的~1H NMR指纹图谱,利用SPSS统计分析软件计算批次间Pearson相关系数。结果建立了10批定坤丹样品的指纹图谱,可检测到糖类、有机酸类及芳香类化合物,10批供试品的指纹图谱间的相似系数均大于0. 9,与生成的对照图谱数据间相似系数均大于0. 95(P <0. 01),即呈现显著相关性,表明该复方总体质量较为稳定。结论该指纹图谱方法科学、准确且简便,可以为定坤丹的内在质量控制提供科学依据。

Objective To establish the 1H NMR fingerprint of Dingkun Dan(DKD) and conduct a comprehensive and efficient method of quality evaluation. Methods The 600 MHz 1H-NMR was employed to establish the 1H NMR fingerprint of 10 batches of DKD. DKD samples were extracted with chloroform-methanol-aqueous. The Pearson correlation coefficient between batches was calculated using SPSS statistical analysis software. Results The 1H NMR fingerprint of 10 batches of DKD were established. Carbohydrate, organic acids, aromatic compounds and other compounds were detected. The Pearson correlation coefficient values of the DKD were all above 0.9, and the coefficient compared with generated control group data were all above 0.95( P <0.01), which showed significant correlation, indicating a relatively stable quality of the formula. Conclusion The 1H-NMR analysis method established in this study is scientific, accurate, reliable, and simple, and it can also supply a solid scientific basis for the further quality control of DKD.