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Application of 1H-NMR spectroscopy to validation of berberine alkaloid reagents and to chemical evaluation of Coptidis Rhizoma.
J Nat Med. 2011 Apr; 65(2):262-7.JN

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. (1)H-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 (1)H-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 (1)H-NMR method was also applicable to direct determination of protoberberine alkaloid contents in Coptidis Rhizoma.

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Publisher Full Text (DOI)

Authors+Show Affiliations

Hasada K
Graduate School of Pharmaceutical Sciences, Nagoya City University, 3-1 Tanabe-dori, Mizuho-ku, Nagoya 467-8603, Japan.
Yoshida T
No affiliation info available
Yamazaki T
No affiliation info available
Sugimoto N
No affiliation info available
Nishimura T
No affiliation info available
Nagatsu A
No affiliation info available
Mizukami H
No affiliation info available

MeSH

BerberineBerberine AlkaloidsChromatography, High Pressure LiquidCoptisMagnetic Resonance SpectroscopyMolecular StructurePlant Extracts

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

21188644

Citation

Hasada, Keiko, et al. "Application of 1H-NMR Spectroscopy to Validation of Berberine Alkaloid Reagents and to Chemical Evaluation of Coptidis Rhizoma." Journal of Natural Medicines, vol. 65, no. 2, 2011, pp. 262-7.
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. 2011;65(2):262-7.
Hasada, K., Yoshida, T., Yamazaki, T., Sugimoto, N., Nishimura, T., Nagatsu, A., & Mizukami, H. (2011). Application of 1H-NMR spectroscopy to validation of berberine alkaloid reagents and to chemical evaluation of Coptidis Rhizoma. Journal of Natural Medicines, 65(2), 262-7. https://doi.org/10.1007/s11418-010-0490-x
Hasada K, et al. Application of 1H-NMR Spectroscopy to Validation of Berberine Alkaloid Reagents and to Chemical Evaluation of Coptidis Rhizoma. J Nat Med. 2011;65(2):262-7. PubMed PMID: 21188644.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Application of 1H-NMR spectroscopy to validation of berberine alkaloid reagents and to chemical evaluation of Coptidis Rhizoma. AU - Hasada,Keiko, AU - Yoshida,Takamitsu, AU - Yamazaki,Takeshi, AU - Sugimoto,Naoki, AU - Nishimura,Tetsuji, AU - Nagatsu,Akito, AU - Mizukami,Hajime, Y1 - 2010/12/25/ PY - 2010/08/12/received PY - 2010/10/21/accepted PY - 2010/12/29/entrez PY - 2010/12/29/pubmed PY - 2011/6/24/medline SP - 262 EP - 7 JF - Journal of natural medicines JO - J Nat Med VL - 65 IS - 2 N2 - 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. (1)H-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 (1)H-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 (1)H-NMR method was also applicable to direct determination of protoberberine alkaloid contents in Coptidis Rhizoma. SN - 1861-0293 UR - https://www.unboundmedicine.com/medline/citation/21188644/Application_of_1H_NMR_spectroscopy_to_validation_of_berberine_alkaloid_reagents_and_to_chemical_evaluation_of_Coptidis_Rhizoma_ L2 - https://dx.doi.org/10.1007/s11418-010-0490-x DB - PRIME DP - Unbound Medicine ER -