Powdered Goldenseal is Goldenseal reduced to a fine or very fine powder. It contains NLT 2.0% of hydrastine (C21H21NO6) and NLT 2.5% of berberine (C20H18NO4), calculated on the dried basis.
• A. Thin-Layer Chromatographic Identification Test
Standard solution: 0.5 mg/mL each of USP Berberine Chloride RS and USP Hydrastine RS in methanol
Sample solution: Transfer about 0.5 g of Powdered Goldenseal, accurately weighed, to a suitable glass vial, and add 0.5 mL of 10% sodium carbonate. Add 5 mL of methanol, and heat for 10 min in a water bath at 60. Cool to room temperature, filter, and dry under a stream of nitrogen. Add 0.5 mL of methanol to dissolve the residue.
Adsorbent: 0.25-mm layer of chromatographic silica gel mixture, typically 20 cm long (TLC plates)
Application volume: 1020 µL, as bands
Developing solvent system: Ethyl acetate, butyl alcohol, formic acid, and water (5:3:1:1)
Samples: Standard solution and Sample solution
Develop the chromatograms until the solvent front has moved about three-fourths of the length of the plate, in a saturated chamber. Remove the plate, air-dry, and examine under UV light at 365 nm.
Acceptance criteria: The chromatograms show zones having a lemon-yellow fluorescence due to berberine at an RF value of about 0.53 and a blue-white fluorescence due to hydrastine at an RF value of about 0.42.
• Content of Berberine and Hydrastine and Limit of Palmatine
Mobile phase: Dissolve 9.93 g of monobasic potassium phosphate in 730 mL of water, add 270 mL of acetonitrile, mix, filter, and degas.
Solvent: A mixture of 0.1 M monobasic potassium and acetonitrile (60:40)
Standard solution: 0.05 mg/mL each of USP Berberine Chloride RS and USP Hydrastine RS in a mixture of methanol and water (1:1)
System suitability solution: Prepare a solution of palmatine in a mixture of water and methanol (1:1) having a known concentration of about 0.05 mg/mL. Mix equal volumes of this solution and the Standard solution.
Sample solution: Transfer about 0.12 g of Powdered Goldenseal, accurately weighed, to a 50-mL volumetric flask. Add 40 mL of Solvent, sonicate for 5 min, and shake for 10 min. Dilute with Solvent to volume, mix, and filter.
Detector: UV 235 nm
Column: 4.6-mm × 150-mm; packing L1
Flow rate: 1.8 mL/min
Injection size: 10 µL
Samples: Standard solution and System suitability solution
Resolution: NLT 1.5 between the berberine and palmatine peaks, and NLT 1.5 between the hydrastine and palmatine peaks, System suitability solution
Capacity factor: NLT 3.0, determined from the hydrastine and berberine peaks, Standard solution
Column efficiency: NLT 5000 theoretical plates determined from the hydrastine and berberine peaks, Standard solution
Tailing factor: NMT 2.0 determined from the hydrastine and berberine peaks, Standard solution
Relative standard deviation: NMT 2.5% determined from the hydrastine and berberine peaks in repeated injections, Standard solution
Samples: Standard solution and Sample solution
Calculate the percentages of berberine and hydrastine in the portion of Powdered Goldenseal taken:
Result = (rU/rS) × CS × (V/W) × 100
Using the values from the chromatogram of the Sample solution, divide the peak area of berberine by the peak area of any peak at the locus for palmatine (if present).
Acceptance criteria: NLT 2.0% of hydrastine (C21H21NO6) and NLT 2.5% of berberine (C20H18NO4), on the dried basis. The ratio of the berberine peak area to any peak area at the locus for palmatine is more than 50:1.
• Heavy Metals, Method III 231: NMT 20 ppm
• Articles of Botanical Origin, General Method for Pesticide Residues Analysis 561: Meets the requirements
• Botanic Characteristics: The powder is dark yellow to moderately greenish yellow with an aromatic odor and bitter taste. Abundant starch granules are present and are either spherical or ovoid; the granules are simple or compounded, with an occasional slit-shaped hilum. Parenchyma cells range from polygonal to round and are filled with starch or brown resin. Tracheary elements with slit-shaped pits and a few large reticulated vessels are present, as are beaded, thick-walled elongated epidermal cells. Thin fragments of cork layer are also present.
• Loss on Drying 731: Dry 2 g of Powdered Goldenseal at 100 for 5 h: it loses NMT 12.0% of its weight.
• Packaging and Storage: Preserve in tight containers, and store protected from light and moisture.
• Labeling: The label states the Latin binomial and, following the official name, the parts of the plant contained in the article.
• USP Reference Standards 11
USP Berberine Chloride RS
USP Hydrastine RS
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USP35NF30 Page 1345Pharmacopeial Forum: Volume No. 30(3) Page 953