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USP 39Dietary Supplements/Rhodiola rosea 6809 USP REFERENCE STANDARDS 11ish band with an RF below the gray bands;the mostUSP Rhodiola rosea Root and Rhizome Dry Extract RSintense gray band is the lower band due to rosavin.USP Rosavin RS B.HPLCUSP Salidroside RSAnalysis:Proceed as directed in the test for Content ofPhenylpropenoid Glycosides and Salidroside.Acceptance criteria:The chromatogram of the Samplesolution exhibits peaks at the retention times corre-.sponding to the peaks due to salidroside,tyrosol,rosarin,rosavin,rosin,and rosiridin in the chromato-Powdered Rhodiola rosea Extractgram of Standard solution C.The ratio of the contentsof rosarin,rosavin,and rosin is about 2.5:6.0:1.5,DEFINITIONrespectively.Powdered Rhodiola rosea Extract is prepared from Rhodiolarosea by extraction with hydroalcoholic mixtures.The ra-COMPOSITIONtio of plant material to extract is between 1.5:1 and 5:1.CONTENT OF PHENYLPROPENOID GLYCOSIDES AND SALIDROSIDEIt contains NLT 90.0%and NMT 110.0%of the labeledSolution A:Wateramount of phenylpropenoid glycosides calculated as theSolution B:Acetonitrilesum of rosarin,rosavin,and rosin,and NLT 90.0%andMobile phase:See Table 1.NMT 110.0%of the labeled amount of salidroside,bothcalculated on the dried basis.It may contain suitableTable 1added substances as carriers.TimeSolution ASolution BIDENTIFICATION(min)(%)(%)A.THIN-LAYER CHROMATOGRAPHY0946Standard solution A:1.0 mg/mL of USP Rosavin RS in68317methanol780.319.7Standard solution B:50 mg/mL of USP Rhodiola roseaRoot and Rhizome Dry Extract RS in methanol.Sonicate980.319.7for 10 min,centrifuge,and use the supernatant.100100Sample solution:50 mg/mL of Powdered Rhodiola12946rosea Extract in methanol.Sonicate for 10 min,centri-17946fuge,and use the supernatant.Chromatographic systemStandard solution A:1.0 mg/mL of USP Rosavin RS in(See Chromatography 621,Thin-Layer Chromato-methanolgraphy.)Standard solution B:0.3 mg/mL of USP Salidroside RSAdsorbent:Chromatographic silica gel with an aver-in methanolage particle size of 5 m(HPTLC plates)Standard solution C:4.0 mg/mL of USP Rhodiola roseaApplication volume:3 L of Standard solution A andRoot and Rhizome Dry Extract RS in methanol.Sonicate5 L each of Standard solution B and the Sample solu-to dissolve,if necessary.Before injection,pass through ation;as 8-mm bandsmembrane filter of 0.45-m or finer pore size.Relative humidity:Condition the plate to a relativeSample solution:4.0 mg/mL of Powdered Rhodiolahumidity of about 33%using a suitable device.rosea Extract in methanol.Sonicate to dissolve,if neces-Developing solvent system:A mixture of ethyl ace-sary.Before injection,pass through a membrane filtertate,methanol,water,and formic acid(77:13:10:2)of 0.45-m or finer pore size.Developing distance:6 cmChromatographic systemDerivatization reagent:Dissolve 1 g of diphenylamine(See Chromatography 621,System Suitability.)in 40 mL of acetone,add 1 mL of aniline,and mix.Mode:LCCarefully add 7.5 mL of phosphoric acid,and mix.Detector:UV 205 nmAnalysisColumn:3.0-mm 10-cm;2.5-m packing L1Samples:Standard solution A,Standard solution B,andColumn temperature:40 1Sample solutionFlow rate:1.0 mL/minApply the samples as bands to a suitable high perfor-Injection volume:1 Lmance thin-layer chromatographic plate,and dry inSystem suitabilityair.Develop the chromatograms in a saturated cham-Samples:Standard solution A and Standard solution Cber,remove the plate from the chamber,and dry inSuitability requirementsair.Derivatize the plate with Derivatization reagent,Chromatogram similarity:The chromatogram ob-heat at 120 for 5 min,and examine under visibletained from Standard solution C is similar to the refer-light.ence chromatogram provided with the lot of USPSystem suitability:The chromatogram of Standard solu-Rhodiola rosea Root and Rhizome Dry Extract RS be-tion B exhibits,in the lower half,three gray bands anding used.two brownish bands,one above and the other belowResolution:NLT 1.5 between the rosarin and rosavinthe gray bands;the most intense band in the chromat-peaks,Standard solution Cogram is the brownish band with an RF below the grayRelative standard deviation:NMT 2%determinedbands;the most intense gray band is the lower band atfrom the rosavin peak in repeated injections,Standardan RF corresponding to the band due to rosavin in thesolution Achromatogram of Standard solution A;the upper grayAnalysisband due to rosarin is less intense.Samples:Standard solution A,Standard solution B,Acceptance criteria:The chromatogram of the SampleStandard solution C,and Sample solutionsolution exhibits a gray band corresponding to the bandUsing the chromatograms of Standard solution A,Stan-due to rosavin in the chromatogram of Standard solu-dard solution B,Standard solution C,and the referencetion A,and the following bands corresponding to simi-chromatogram provided with the lot of USP Rhodiolalar bands in the chromatogram of Standard solution B:rosea Root and Rhizome Dry Extract RS being used,two additional gray bands and two brownish bands,identify the retention time of the peaks correspondingone above and the other below the gray bands;theto salidroside,tyrosol,rosarin,rosavin,rosin,andmost intense band in the chromatogram is the brown-rosiridin from the Sample solution.DS MonographsOfficial from May 1,2016Copyright(c)2016 The United States Pharmacopeial Convention.All rights reserved.Accessed from 10.6.1.1 by ebsc0sa on Tue Jan 26 04:15:59 EST 20166810 Rhodiola rosea/Dietary SupplementsUSP 39Separately calculate the percentage of rosarin,rosavin,SPECIFIC TESTSand rosin as rosavin in the portion of Powdered Rhodi-LOSS ON DRYING 731ola rosea Extract taken:Sample:2.0 g of Powdered Rhodiola rosea ExtractAnalysis:Dry at 105 for 2 h.P1=(rU/rS)(CS/CU)100Acceptance criteria:NMT 5%rU=peak area of the relevant analyte from theADDITIONAL REQUIREMENTSSample solution PACKAGING AND STORAGE:Preserve in well-closed contain-rS=peak area of rosavin from Standard solution Aers,protected from light and moisture,and store at con-CS=concentration of rosavin in Standard solution Atrolled room temperature.(mg/mL)LABELING:The label states the Latin binomial and,fol-CU=concentration of Powdered Rhodiola rosealowing the official name,the part of the plant fromExtract in the Sample solution(mg/mL)which the article was derived.It meets other labeling re-Calculate the percentage of phenylpropenoid glycosidesquirements under Botanical Extracts 565.as the sum of the percentages of rosarin,rosavin,and USP REFERENCE STANDARDS 11rosin.USP Rhodiola rosea Root and Rhizome Dry Extract RSCalculate the percentage of salidroside in the portion ofUSP Rosavin RSPowdered Rhodiola rosea Extract taken:USP Salidroside RSP2=(rU/rS)(CS/CU)100rU=peak area of salidroside from the Sample.solutionRhodiola rosea TincturerS=peak area of salidroside from Standard solutionBDEFINITIONCS=concentration of salidroside in StandardRhodiola rosea Tincture is prepared as follows.solution B(mg/mL)CU=concentration of Powdered Rhodiola roseaRhodiola rosea1 part(g)Extract in the Sample solution(mg/mL)Calculate the percentage of the labeled amount ofA mixture of Alcohol and Water(40:60),aphenylpropenoid glycosides in the portion ofsufficient quantity to make5 parts(mL)Powdered Rhodiola rosea Extract taken:Prepare the Tincture as directed for Botanical Extracts 565,Result=(P1/L)100Tinctures,Maceration Process.It contains NLT 0.06%(w/v)of phenylpropenoid glycosides calculated as the sum ofP1=content of phenylpropenoid glycosides,asrosarin,rosavin,and rosin;and NLT 0.016%of salidroside.determined above(%)IDENTIFICATIONL=labeled amount of phenylpropenoid glycosides A.THIN-LAYER CHROMATOGRAPHY(%)(See Chromatography 621,Thin-Layer Chromato-Calculate the percentage of the labeled amount ofgraphy.)salidroside in the portion of Powdered Rhodiola roseaStandard solution A:1.0 mg/mL of USP Rosavin RS inExtract taken:methanolResult=(P2/L)100Standard solution B:50 mg/mL of USP Rhodiola roseaRoot and Rhizome Dry Extract RS in methanol.SonicateP2=content of salidroside,as determined abovefor 10 min,centrifuge,and use the supernatant.(%)Sample solution:Centrifuge a portion of Tincture,andL=labeled amount of salidroside(%)use the supernatant.Acceptance criteria:NLT 90.0%and NMT 110.0%ofChromatographic systemthe labeled amount of phenylpropenoid glycosides,andAdsorbent:Chromatographic silica gel with an aver-NLT 90.0%and NMT 110.0%of the labeled amount ofage particle size of 5 m(HPTLC plates)salidroside,both calculated on the dried basis.Application volume:3 L of Standard solution A,5 Lof Standard solution B,and 10 L of Sample solution;asCONTAMINANTS8-mm bands ELEMENTAL IMPURITIESPROCEDURES 233Relative humidity:Condition the plate to a relativeAcceptance criteriahumidity of about 33%using a suitable device.Arsenic:NMT 2.0 g/gDeveloping solvent system:A mixture of ethyl ace-Cadmium:NMT 1.0 g/gtate,methanol,water,and formic acid(77:13:10:2)Lead:NMT 5.0 g/gDeveloping distance:6 cmMercury:NMT 1.0 g/gDerivatization reagent:Dissolve 1 g of diphenylamine ARTICLES OF BOTANICAL ORIGIN,General Method for Pesti-in 40 mL of acetone,add 1 mL of aniline,and mix.cide Residues Analysis 561:Meets the requirementsCarefully add 7.5 mL of phosphoric acid,and mix.MICROBIAL ENUMERATION TESTS 2021:The total aerobicAnalysisbacterial count does not exceed 104.cfu/g,and the totalSamples:Standard solution A,Standard solution B,andcombined molds and yeasts count does not exceed 103.Sample solutioncfu/g.Apply the samples as bands to a suitable high perfor-ABSENCE OF SPECIFIED MICROORGANISMS 2022:Meets themance thin-layer chromatographic plate,and dry inrequirements of the tests for absence of Salmonella spe-air.Develop the chromatograms in a saturated cham-cies and Escherichia coliber,remove the plate from the chamber,and dry in ARTICLES OF BOTANICAL ORIGIN,Test for Aflatoxins 561:air.Derivatize the plate with Derivatization reagent,Meets the requirementsheat at 120 for 5 min,and examine under visiblelight.System suitability:The chromatogram of Standard solu-tion B exhibits,in the lower half,three gray bands andtwo brownish bands,one above and the other belowDS MonographsOfficial from May 1,2016Copyright(c)2016 The United States Pharmacopeial Convention.All rights reserved.Accessed from 10.6.1.1 by ebsc0sa on Tue Jan 26 04:15:59 EST 2016