Quantification of natural products in herbal supplements: A combined NMR approach applied on goldenseal

• Published in: Journal of pharmaceutical and biomedical analysis 2019-02, Vol.165, p.155-161
• Main Authors: Le, Phuong Mai, Milande, Clément, Martineau, Estelle, Giraudeau, Patrick, Farjon, Jonathan
• Format: Article
• Language: English
• Subjects: 1D 1H; 2D Q QUIPU HSQC; Alkaloids; Chemical Sciences; Goldenseal (Hydrastine canadensis); Herbal supplements; Quantitative NMR
• ISSN: 0731-7085; 1873-264X
• DOI: 10.1016/j.jpba.2018.11.062

[Display omitted] •Combined 1D and 2D qNMR approach was developed for quantification of the alkaloids beberine, canadine and hydrastine, in goldenseal extracts.•Berberine with non-overlapped signals was quantified by 1D 1H NMR.•Overlapped and low-intensity signals of hydrastine and canadine were quantified by 2D Q QUIPU HSQC NMR.•Berberine, an unstable alkaloid, was not quantified by 2D Q QUIPU due to long durations.•NMR quantitative results are in good agreement with UV and MS. Authentication of natural products is of major relevance in the context of manufactured drugs or herbal supplements since such active products generate a lucrative market. The analytical method to identify and quantify valuable natural products is critical for quality control and product assignment of herbal supplements. In this framework, we propose to apply a recently developed quantitative 2D NMR approach called Q QUIPU (Quick QUantItative Perfected and pUre shifted) in combination with 1D 1H NMR capable to access the concentration of three major alkaloids, berberine, β-hydrastine and canadine, in the root extract of goldenseal (Hydrastis canadensis), one of the 20 most popular herbal supplements used worldwide. We highlight the complementarity of 1D and 2D quantitative NMR to accurately assess the amount of alkaloids with different range of concentrations and stability within extracts. In particular, unstable natural products having non-overlapped signals like berberine could only be quantified by sensitive and fast 1D 1H, while overlapped signals of β-hydrastine and low intense ones of canadine could only be quantified with the recent 2D Q QUIPU HSQC. Results obtained from this combined approach have led to a good accuracy (