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Research regarding the quality control of Hydrastis canadensis (goldenseal) products

This information has been complied in order to facilitate the research efforts of health care professionals and others.  These statements have not been evaluated by the Food and Drug Administration and are not intended diagnose, treat, cure, prevent, mitigate, or prevent any disease.  The information is presented with the latest publications first.  This is an ongoing work so check back often as we will update these pages as more information becomes available.  Also see the anti-parasitic and anti-diarrhea pages. Last Updated : 08/25/2008


A New Glucosyl Feruloyl Quinic Acid as a Potential Marker for Roots and Rhizomes of Goldenseal, Hydrastis canadensis.
McNamara CE, Perry NB, Follett JM, Parmenter GA, Douglas JA.
J Nat Prod. 2004 Nov 29;67(11):1818-1822.

A new compound, 5-O-(4'-[beta-d-glucopyranosyl]-trans-feruloyl)quinic acid (GPFQ, 10), is reported from the medicinal plant goldenseal (Hydrastis canadensis). A new HPLC method is described and used to show that GPFQ is a potential marker for goldenseal roots (1.0% w/w) and rhizomes (2.3%). GPFQ was found at much lower levels in stems (<0.1%) and could not be detected in leaves. Neochlorogenic acid (9), which has not previously been reported from goldenseal, and chlorogenic acid (6) reached their highest levels in leaves (0.9% 9 and 0.5% 6). The main alkaloids, hydrastine (1) and berberine (2), were highest in rhizomes (2.8% 1 and 4.6% 2), but palmatine (5) was not found in genuine goldenseal.


Immunoquantitative analysis for berberine and its related compounds using monoclonal antibodies in herbal medicines.
Kim JS, Tanaka H, Shoyama Y.
Analyst. 2004 Jan;129(1):87-91. Epub 2003 Dec 11.

The monoclonal antibody (MAb) against berberine, a bioactive constituent of Coptis japonica M., Phellodendron amurense R. and Hydrastis canadensis L., was produced and characterized. As immunogen, the derivative of berberine, 9-O-carboxymethyl berberrubine was synthesized and conjugated to carrier protein, bovine serum albumin (BSA). In order to confirm its immunogenicity, the ratio of hapten in berberine-BSA conjugate was determined by matrix-assisted laser desorption/ionization time of flight mass spectrometry (MALDI-TOF MS). After immunization, hybridomas secreting MAbs against berberine were produced by fusing splenocytes with mouse myeloma cell line, P3-X63-Ag8-653. After the screening, anti-berberine MAb 1D5-3B-7 was obtained. Subsequently, a quantitative ELISA system for berberine and its related compounds using the MAb was established and evaluated comparing with HPLC method. The ELISA method described in this study can be available as an analytical tool for quality control and standardization of medicinal plants and its prescriptions containing berberine and its related compounds.


Chemical comparison of goldenseal (Hydrastis canadensis L.) root powder from three commercial suppliers.
Weber HA, Zart MK, Hodges AE, Molloy HM, O'Brien BM, Moody LA, Clark AP, Harris RK, Overstreet JD, Smith CS.
J Agric Food Chem. 2003 Dec 3;51(25):7352-8.


The characterization of herbal materials is a significant challenge to analytical chemists. Goldenseal (Hydrastis canadensis L.), which has been chosen for toxicity evaluation by NIEHS, is among the top 15 herbal supplements currently on the market and contains a complex mixture of indigenous components ranging from carbohydrates and amino acids to isoquinoline alkaloids. One key component of herbal supplement production is botanical authentication, which is also recommended prior to initiation of efficacy or toxicological studies. To evaluate material available to consumers, goldenseal root powder was obtained from three commercial suppliers and a strategy was developed for characterization and comparison that included Soxhlet extraction, HPLC, GC-MS, and LC-MS analyses. HPLC was used to determine the weight percentages of the goldenseal alkaloids berberine, hydrastine, and canadine in the various extract residues. Palmatine, an isoquinoline alkaloid native to Coptis spp. and other common goldenseal adulterants, was also quantitated using HPLC. GC-MS was used to identify non-alkaloid constituents in goldenseal root powder, whereas LC-MS was used to identify alkaloid components. After review of the characterization data, it was determined that alkaloid content was the best biomarker for goldenseal. A 20-min ambient extraction method for the determination of alkaloid content was also developed and used to analyze the commercial material. All three lots of purchased material contained goldenseal alkaloids hydrastinine, berberastine, tetrahydroberberastine, canadaline, berberine, hydrastine, and canadine. Material from a single supplier also contained palmatine, coptisine, and jatrorrhizine, thus indicating that the material was not pure goldenseal. Comparative data for three commercial sources of goldenseal root powder are presented.


Method validation for determination of alkaloid content in goldenseal root powder.
Weber HA, Zart MK, Hodges AE, White KD, Barnes SM, Moody LA, Clark AP, Harris RK, Overstreet JD, Smith CS.
J AOAC Int. 2003 May-Jun;86(3):476-83.

A fast, practical ambient extraction methodology followed by isocratic liquid chromatography (LC) analysis with UV detection was validated for the determination of berberine, hydrastine, and canadine in goldenseal (Hydrastis canadensis L.) root powder. The method was also validated for palmatine, a major alkaloid present in the possible bioadulterants Coptis, Oregon grape root, and barberry bark. Alkaloid standard solutions were linear over the evaluated concentration ranges. The analytical method was linear for alkaloid extraction using 0.3-2 g goldenseal root powder/100 mL extraction solvent. Precision of the method was demonstrated using 10 replicate extractions of 0.5 g goldenseal root powder, with percent relative standard deviation for all 4 alkaloids < or = 1.6. Alkaloid recovery was determined by spiking each alkaloid into triplicate aliquots of neat goldenseal root powder. Recoveries ranged from 92.3% for palmatine to 101.9% for hydrastine. Ruggedness of the method was evaluated by performing multiple analyses of goldenseal root powder from 3 suppliers over a 2-year period. The method was also used to analyze Coptis root, Oregon grape root, barberry bark, and celandine herb, which are possible goldenseal bioadulterants. The resulting chromatographic profiles of the bioadulterants were significantly different from that of goldenseal. The method was directly transferred to LC with mass spectrometry, which was used to confirm the presence of goldenseal alkaloids tetrahydroberberastine, berberastine, canadaline, berberine, hydrastine, and canadine, as well as alkaloids from the bioadulterants, including palmatine, jatrorrhizine, and coptisine.


Variations in alkaloid content of herbal products containing goldenseal.
Edwards DJ, Draper EJ.
J Am Pharm Assoc (Wash DC). 2003 May-Jun;43(3):419-23.

OBJECTIVE: To determine the concentration of hydrastine and berberine, the primary alkaloids in herbal products containing goldenseal. DESIGN: Descriptive comparison of 20 products purchased at local pharmacies or health food stores; 17 products were labeled as containing goldenseal root and 3 products contained goldenseal herb as the sole active herbal ingredient. SETTING: Laboratory assessment of alkaloid content using high-performance liquid chromatography. MAIN OUTCOME MEASURES: Comparisons of hydrastine and berberine concentration, alkaloid ratio, and total alkaloid content among products. RESULTS: Hydrastine concentration in products labeled as containing goldenseal root ranged from 0 to 2.93%, whereas berberine concentration varied from 0.82% to 5.86%. Median total alkaloid concentration was 5.30%. Only 10 of 17 products met proposed United States Pharmacopeia (USP) standards for the hydrastine and berberine content of goldenseal root. Five products contained little or no hydrastine, unusual berberine:hydrastine ratios, and additional peaks not observed with other products. Alkaloid content in goldenseal root products was about fourfold higher than in products labeled as containing goldenseal herb. CONCLUSION: Alkaloid content of goldenseal products varies widely, with many products failing to meet proposed USP standards. In addition, the chromatographic pattern and alkaloid ratio for several products were atypical for goldenseal. Given the current absence of regulation of the quality of herbal products, pharmacists should take extra care to ensure that substandard goldenseal products are not sold in their pharmacies.
 


 


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