Abstract
Berberine, palmatine, and coptisine are major pharmacologically active protoberberine alkaloids in Coptidis Rhizoma, and have been used as indices for chemical evaluation of the crude drug. 1H-NMR spectroscopy was applied to determination of purities of commercial reagents of protoberberine alkaloids. The purities of the alkaloids were calculated from the ratios of the intensities of the H-13 singlet signal at about δ 8.7 ppm of target protoberberine alkaloids to integration of a hexamethyldisilane (HMD) signal at 0 ppm. The concentration of HMD was corrected with SI traceability using potassium hydrogen phthalate of certified reference material (CRM) grade. The purity of the reagent estimated by the 1H-NMR was, in general, lower than that claimed by the manufacturer, leading to over-estimation of the alkaloid contents of Coptidis Rhizoma when determined by HPLC. The present quantitative 1H-NMR method was also applicable to direct determination of protoberberine alkaloid contents in Coptidis Rhizoma.
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This work is supported by Health and Labour Sciences Research Grants from the Ministry of Health, Labour and Welfare of Japan.
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Hasada, K., Yoshida, T., Yamazaki, T. et al. Application of 1H-NMR spectroscopy to validation of berberine alkaloid reagents and to chemical evaluation of Coptidis Rhizoma. J Nat Med 65, 262–267 (2011). https://doi.org/10.1007/s11418-010-0490-x
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DOI: https://doi.org/10.1007/s11418-010-0490-x