Goldenseal
»Goldenseal consists of the dried roots and rhizomes of Hydrastis canadensis(Linné)(Fam.Ranunculaceae).It contains not less than 2.0percent of hydrastine (C21H21NO6)and not less than 2.5percent of berberine (C20H18NO4),calculated on the dried basis.
Packaging and storage— Store in tight containers,protected from light,moisture,and heat.
Labeling— The label states the Latin binomial and,following the official name,the parts of the plant contained in the article.
USP Reference standards á11ñ— USP Berberine Chloride RS.USP Hydrastine Hydrochloride RS.
Botanic characteristics—
Macroscopic— The rhizome is knotty,subcylindrical,and occasionally has an aerial stem.It is 1to 5cm in length and 2to 10mm in diameter.Externally,the rhizome is brown to dusky yellowish orange,deeply furrowed,and marked by numerous stem and bud scale scars.Numerous brittle roots arise roughly from the same side of the main axis.Fractures are short and resinous with a dark yellow to yellowish brown bark,greenish yellow margins,and a yellowish orange center that is waxy in appearance.An interrupted circle of small,radially elongated fibrovascular bundles are also present.The roots are filiform,up to 35cm in length and 1mm in diameter,and are either curved or twisted,tangled together,or broken.Fractures are short and brittle,and show an internal color of yellowish orange to greenish yellow.
Histology—
Transverse section of rhizomeand root— The rhizome has polygonal,yellowish brown,thin to slightly thick-walled cork cells.Wedge-shaped vascular bundles are separated by wide medullary rays.Tracheary elements are lignified and have slit-shaped pits.Afew large vessels with reticulate thickenings are also present.The parenchyma tissue is composed of polygonal cells with abundant simple or compound starch grains up to 8µm in diameter.Afew irregularly shaped resin cells are present in the cortex and the pith.Masses of granular,orange-brown matter are also present in the parenchyma tissues.The roots have a single layer of irregularly elongated cork cells.The tracheary elements are associated with lignified fibers.Fragments of the epidermis are sometimes present near the base of the rhizome and are composed of cells with thick,lignified,beaded walls.
Thin-layer chromatographic identification test á201ñ—
Test solution— Finely powder the rhizome and the root,transfer 0.5g of the powder to a suitable glass vial,add 0.5mLof 10%sodium carbonate,and mix.Add 5mLof methanol,and heat for 10minutes in a water bath at 60.Cool to room temperature,filter,and dry under a stream of nitrogen.Add 0.5mLof methanol to dissolve the residue.
Standard solution— Dissolve accurately weighed quantities of USP Berberine Chloride RSand USP Hydrastine Hydrochloride RSin methanol to obtain a solution having a concentration of 0.5mg of each USP Reference Standard per mL.
Application volume: 10µLto 20µL,as bands.
Developing solvent system: a mixture of ethyl acetate,butyl alcohol,formic acid,and water (50:30:10:10).
Procedure— Proceed as directed in the chapter,except to air-dry the plates,and examine them under UVlight at about 365nm.The chromatograms show zones having a lemon yellow fluorescence due to berberine at an RFvalue of about 0.53and a blue-white fluorescence due to hydrastine at an RFvalue of about 0.42.
Loss on drying á731ñ— Dry 2g of finely powdered Goldenseal at 100for 5hours:it loses not more than 12.0%.
Foreign organic matter á561ñ: not more than 2.0%.
Total ash á561ñ: not more than 9%.
Acid-insoluble ash á561ñ: not more than 5%.
Pesticide residues á561ñ: meets the requirements.
Content of berberine and hydrastine—
Mobile phase— Dissolve 9.93g of monobasic potassium phosphate in 730mLof distilled water.Add 270mLof acetonitrile,mix,filter,and degas.Make other adjustments if necessary (see System Suitabilityunder Chromatography á621ñ).
Standard solution— Dissolve accurately weighed quantities of USP Berberine Chloride RSand USP Hydrastine Hydrochloride RSin a mixture of water and methanol (1:1)to obtain a solution containing about 0.2mg of each USP Reference Standard per mL.[NOTE—Concentrations of berberine and hydrastine in this solution are calculated by multiplying the concentration of each of the USP Reference Standards with correction factors of 0.905and 0.913,respectively.]
Test solution— Finely powder an amount of Goldenseal,and transfer 1.0g,accurately weighed,to a continuous-extraction apparatus with a 500-mLround-bottom flask.Treat the Goldenseal with 150mLof methanol,and extract for 6hours,or until the solvent is clear.The volume of the thimble should be at least one-half that of the volume of methanol.Cool to room temperature,and transfer the methanol extract to a 200-mLvolumetric flask.Rinse the extraction unit with methanol,quantitatively transfer the contents to the volumetric flask,and dilute with methanol to volume.
Chromatographic system (see Chromatography á621ñ)— The liquid chromatograph is equipped with a 235-nm detector and a 4.6-mm ×150-mm column that contains packing L1.The flow rate is about 1.8mLper minute.Chromatograph the Standard solution,and record the peak responses as directed for Procedure:the capacity factor,k¢,determined from the hydrastine and berberine peaks is not less than 3.0;the column efficiency is not less than 5000theoretical plates;the tailing factor is not more than 2.0;and the relative standard deviation for replicate injections is not more than 2.5%.[NOTE—The total run time is 10minutes.]
Procedure— Separately inject equal volumes (about 10µL)of the Standard solutionand the Test solutioninto the chromatograph,record the chromatograms,and measure the areas for the major peaks.Calculate the percentages of berberine and hydrastine in the portion of Goldenseal taken by the formula:
100(CV/W)(rU/rS),
in which Cis the concentration,in mg per mL,of berberine or hydrastine in the respective USP Reference Standard in the Standard solutionusing the correction factors as noted above;Vis the final volume,in mL,of the Test solution;Wis the weight,in mg,of Goldenseal taken;and rUand rSare the peak areas for berberine and hydrastine obtained from the Test solutionand the Standard solution,respectively:not less than 2.0%of hydrastine is found;and not less than 2.5%of berberine is found.
Auxiliary Information— Staff Liaison:Gabriel I.Giancaspro,Ph.D.,Senior Scientist and Latin American Specialist
Expert Committee:(DSB)Dietary Supplements:Botanicals
USP28–NF23Page 2103
Pharmacopeial Forum:Volume No.30(3)Page 952
Phone Number:1-301-816-8343