Powdered Goldenseal Extract
DEFINITION
Powdered Goldenseal Extract is prepared from the pulverized dried roots and rhizomes of Hydrastis canadensis L. (Fam. Ranunculaceae), using suitable solvents. It contains NLT 5% of hydrastine (C21H21NO6) and NLT 10% of the sum of berberine (C20H18NO4) and hydrastine, calculated on the dried basis. The ratio of starting crude plant material to Powdered Extract is 2:1.
IDENTIFICATION
• 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:
10 mg/mL of Powdered Extract in a mixture of methanol and water (1:1). Sonicate for 20 min, cool to room temperature, and filter.
Adsorbent:
0.25-mm layer of chromatographic silica gel mixture, typically 20 cm long (TLC plates)
Application volume:
10–20 µL, as bands
Developing solvent system:
Ethyl acetate, butyl alcohol, formic acid, and water (5:3:1:1)
Analysis
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.
COMPOSITION
• 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.
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:
2 mg/mL of Powdered Extract in a mixture of methanol and water (1:1). Sonicate for 20 min, cool to room temperature, and filter. [Note—The sample to be used in this test should not be subjected to the conditions specified in the test for Loss on Drying. A separate sample is used to determine the content on the dried basis. ]
Chromatographic system
Mode:
LC
Detector:
UV 235 nm
Column:
4.6-mm × 150-mm; packing L1
Flow rate:
1.8 mL/min
Injection size:
10 µL
System suitability
Samples:
Standard solution and System suitability solution
Suitability requirements
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
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentages of hydrastine and berberine in the portion of Powdered Extract taken:
Result = (rU/rS) × (CS/CU) × 100
| rU | = | = peak area of berberine or hydrastine from the Sample solution |
| rS | = | = peak area of berberine or hydrastine from the Standard solution |
| CS | = | = concentration of berberine or hydrastine in the Standard solution (mg/mL) |
| CU | = | = concentration of Powdered Extract in the Sample solution (mg/mL) |
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 5% of hydrastine and NLT 10% of the sum of hydrastine and berberine, 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.
CONTAMINANTS
• Heavy Metals, Method II 
231
:
NMT 20 ppm
231:
NMT 20 ppm
• Articles of Botanical Origin, General Method for Pesticide Residues Analysis 561:
Meets the requirements
561:
Meets the requirements
• Microbial Enumeration Tests 2021:
The total aerobic microbial count does not exceed 104 cfu/g, and the total combined molds and yeasts count does not exceed 1000 cfu/g.
2021:
The total aerobic microbial count does not exceed 104 cfu/g, and the total combined molds and yeasts count does not exceed 1000 cfu/g.
• Microbiological Procedures for Absence of Specified Microorganisms 2022:
It meets the requirements of the tests for absence of Salmonella species and Escherichia coli.
2022:
It meets the requirements of the tests for absence of Salmonella species and Escherichia coli.
SPECIFIC TESTS
• Loss on Drying 731:
Dry 1.0 g of Powdered Extract at 105
for 2 h: it loses NMT 5.0% of its weight.
731:
Dry 1.0 g of Powdered Extract at 105 for 2 h: it loses NMT 5.0% of its weight.
ADDITIONAL REQUIREMENTS
• 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 part of the plant from which the article was prepared. Label to indicate the content of hydrastine and berberine, the extracting solvent used for preparation, and the ratio of the starting crude plant material to the Powdered Extract.
Auxiliary Information—
Please check for your question in the FAQs before contacting USP.
| Topic/Question | Contact | Expert Committee |
|---|---|---|
| Monograph | Maged H. Sharaf, Ph.D.
Principal Scientific Liaison 1-301-816-8318 |
(DS2010) Monographs - Dietary Supplements |
| 2021 |
Radhakrishna S Tirumalai, Ph.D.
Principal Scientific Liaison 1-301-816-8339 |
(GCM2010) General Chapters - Microbiology |
| 2022 |
Radhakrishna S Tirumalai, Ph.D.
Principal Scientific Liaison 1-301-816-8339 |
(GCM2010) General Chapters - Microbiology |
| Reference Standards | RS Technical Services 1-301-816-8129 rstech@usp.org |
USP35–NF30 Page 1346
Pharmacopeial Forum: Volume No. 30(3) Page 954