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BCIT Citations Collection

Determination of hydrastine and berberine in goldenseal raw materials, extracts, and dietary supplements by high-performance liquid chromatography with UV
A multilaboratory collaborative study was conducted on a high-performance liquid chromatographic (HPLC) method utilizing UV detection, previously validated using AOAC single-laboratory validation guidelines for determination of hydrastine and berberine in goldenseal (Hydrastis canadensis L.) raw materials, extracts, and dietary supplements at levels ranging from 0.4 to 6% (w/w). Nine collaborating laboratories determined the hydrastine and berberine content in 8 blind samples. Sample materials included powdered botanical raw materials, whole root material, and 4 finished product dietary supplements containing either goldenseal powdered root material or extract. The materials were extracted with an acidified water and acetonitrile solution. HPLC analyses of the extracts were performed on a C18 column using UV detection at 230 nm. Results for powdered root material and capsule products ranged from about 0.2% (w/w) for each alkaloid to about 4% (w/w) for each alkaloid. Liquid tincture results were approximately 4000-5000 microg/mL for each alkaloid. Reproducibility relative standard deviations (RSDR) for hydrastine ranged from 2.68 to 6.65%, with HorRat values ranging from 0.77 to 1.89. RSDR for berberine ranged from 5.66 to 7.68%, with HorRat values ranging from 1.32 to 2.12. All finished products containing goldenseal extract yielded HorRat values <2.0. Based on these results, the method is recommended for Official First Action for determination of hydrastine and berberine in goldenseal raw materials and dietary supplement finished products containing powdered goldenseal and goldenseal extract., Peer-reviewed article, Published.
Determination of phenolic constituents in echinacea raw materials and dietary supplements by HPLC-UV
A collaborative study was conducted to evaluate an HPLC method for determining phenolic compounds in Echinacea spp. raw materials, powdered extracts, and tinctures. Eleven collaborating laboratories received three practice samples representing each matrix type, phenolic reference standards, eight test samples as blind duplicates, the validated analytical method, and instructions. Test samples included two raw materials, four extracts (including one in combination with astragalus and reishi), one ethanolic tincture in combination with goldenseal, and one glycerite tincture. Each material was extracted with a 60% methanol aqueous solution, separated on a C18 column, and detected at 330 nm. Results reported by laboratories for total phenolics in Echinacea roots, aerial parts, and extracts ranged from 9.5 to 62.9 mg/g with RSDR ranging from 3.64 and 7.95% and Horwitz ratio (HorRat) values ranging from 1.06 to 2.01. Total phenolics in the ethanolic tincture ranged from 4837 to 5962 μg/mL, with an RSDR of 6.35% and a HorRat value of 1.45. The glycerite tincture showed poor interlaboratory precision with a HorRat value of 3.32, an RSDR of 21.8%, and reported total phenolic values ranging from 257 to 539 μg/mL., Peer-reviewed article, Published. Received May 4, 2016; Accepted by AP May 25, 2016.