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Application of 1H-NMR spectroscopy to validation of berberine alkaloid reagents and to chemical evaluation of Coptidis Rhizoma

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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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Acknowledgment

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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Authors and Affiliations

  1. Graduate School of Pharmaceutical Sciences, Nagoya City University, 3-1 Tanabe-dori, Mizuho-ku, Nagoya, 467-8603, Japan

    Keiko Hasada, Takamitsu Yoshida & Hajime Mizukami

  2. College of Pharmacy, Kinjo Gakuin University, 2-1723 Omori, Moriyama-ku, Nagoya, 463-8521, Japan

    Keiko Hasada & Akito Nagatsu

  3. National Institute of Health Sciences, 1-18-1 Kamiyoga, Setagaya-ku, Tokyo, 158-8501, Japan

    Takeshi Yamazaki, Naoki Sugimoto & Tetsuji Nishimura

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  1. Keiko Hasada
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  2. Takamitsu Yoshida
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  3. Takeshi Yamazaki
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  4. Naoki Sugimoto
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  5. Tetsuji Nishimura
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  6. Akito Nagatsu
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  7. Hajime Mizukami
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Corresponding author

Correspondence to Hajime Mizukami.

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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

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