Powdered Echinacea angustifolia Extract, chemical structure, molecular formula, Reference Standards

Powdered Echinacea angustifolia Extract

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»PowderedEchinacea angustifolia Extract is prepared from Echinacea angustifolia roots by extraction with hydroalcoholic mixtures or other suitable solvents.The ratio of the starting crude plant material to Powdered Extract is between 2:1and 8:1.It contains not less than 4.0percent and not more than 5.0percent of total phenols,calculated on the dried basis as the sum of caftaric acid (C13H12O9),chicoric acid (C22H18O12),chlorogenic acid (C16H18O9),dicaffeoylquinic acids (C25H24O12),and echinacoside (C35H46O20).It contains not less than

0.1

USP28percent of dodecatetraenoic acid isobutylamides (C16H25NO)

on the dried basis.

USP28

Packaging and storage— Preserve in tight,light-resistant containers,in a cool place.

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Labeling— The label states the Latin binomial and,following the official name,the part of the plant from which the article was prepared.

If standardized by the content of alkamides,label it to indicate the targeted content of dodecatraenoic acid isobutylamides.The label bears a statement indicating that Echinacea angustifolia may cause rare allergic reactions,rashes,or aggravate asthma.

USP28It meets the requirements forLabelingunderBotanical Extracts á565ñ.

USP Reference standards á11ñ— USP Chlorogenic Acid RS.USP Powdered Echinacea angustifolia Extract RS.USP2E,4E-Hexadienoic Acid Isobutylamide RS.

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Identification—

A:Thin-Layer Chromatographic Identification Test á201ñ—

Standard solution 1,Standard solution 2,Developing solvent system,Spray reagent,and Procedure— Proceed as directed forIdentification test Bunder Echinacea angustifolia.

Test solution— Dissolve

1.0g

USP28of Powdered Extract in 10mLof methanol.Allow to stand for 15minutes before use.

B: The retention time for the major peak in the chromatogram of theTest solution corresponds to that for the echinacoside peak in the chromatogram ofStandard solution 1,as obtained in the test for Content of total phenols.

Microbial enumeration á2021ñ— The total bacterial count does not exceed 104cfu per g and the total combined molds and yeasts count does not exceed 1000cfu per g.It meets the requirements of the tests for absence of Salmonella species and Escherichia coli.

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Loss on drying á731ñ:

Dry 1g at 105

for 2hours:It loses

USP28not more than 5.0%.

Heavy metals,Method IIá231ñ: 0.002%.

Organic volatile impurities,Method Iá467ñ: meets the requirements.

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Content of total phenols—

Solvent,Solution A,Solution B,Mobile phase,Standard solution 1,Standard solution 2,and Chromatographic system— Proceed as directed for Content of total phenols under Echinacea angustifolia.

Test solution— Transfer about 60mg of Powdered Extract,accurately weighed,to

an appropriate round bottom flask equipped with a condenser.

USP28Add 25.0mLofSolvent,

and heat under reflux while shaking

USP28by mechanical means for 15minutes.Centrifuge,or pass through a membrane filter having a 0.45-µm or finer porosity.

Procedure— Proceed as directed forContent of total phenols under Echinacea angustifolia.Calculate the percentage of each relevant component of total phenols in the portion of Powdered Extract taken by the formula:

2500F(C/W)(ri/rS),

in whichFis the response factor and is equal to 0.695for chicoric acid,0.729for dicaffeoylquinic acids,0.881for caftaric acid,1.000for chlorogenic acid,and 2.220for echinacoside;Cis the concentration,in mg per mL,of USP Chlorogenic Acid RSinStandard solution 2;Wis the weight,in mg,of the portion of Powdered Extract taken;andriandrSare the peak responses for the relevant analyte obtained from theTest solution andStandard solution 2,respectively.Calculate the percentage of total phenols in the portion of Powdered Extract taken by adding the individual percentages.

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Content of dodecatetraenoic acid isobutylamides—

Mobile phase and Standard solution 2— Proceed as directed forContent of dodecatetraenoic acid isobutylamides under Echinacea angustifolia.

Standard solution 1— Dissolve an accurately weighed quantity of USP PowderedEchinacea angustifolia Extract RSin methanol,shaking for 1minute,and dilute with methanol to volume to obtain a solution having a known concentration of about 1mg per mL.Pass through a membrane filter having a 0.45-µm or finer porosity.

Test solution— Transfer about 500mg of Powdered Extract,accurately weighed,to a 100-mLvolumetric flask.Add 80mLof methanol,and sonicate for 30minutes.Dilute with methanol to volume,and pass through a membrane filter having a 0.45-µm or finer porosity.

Chromatographic system— Prepare as directed forContent of dodecatetraenoic acid isobutylamides underEchinacea angustifolia.Chromatograph Standard solution 1,and record the peak responses as directed forProcedure:the chromatogram obtained is similar to the Reference Chromatogram for alkamides provided with the USP Powdered Echinacea angustifolia Extract RS,

and the resolution,R,between the two isomers of dodecatetraenoic acid isobutylamides is not less than 1.0.

USP28ChromatographStandard solution 2,and record the peak responses as directed forProcedure:the capacity factor,k¢,is not less than 3.5;the tailing factor is not more than 2.0;and the relative standard deviation for replicate injections is not more than 2.5%.

Procedure— Proceed as directed forContent of dodecatetraenoic acid isobutylamides under Echinacea angustifolia.Calculate the percentage of dodecatetraenoic acid isobutylamides in the portion of Powdered Extract taken by the formula:

10,000(1.353)(C/W)(ri/rS),

in which 1.353is the response factor for 2E,4E-hexadienoic acid isobutylamide;Cis the concentration,in mg per mL,of USP2E,4E-Hexadienoic Acid Isobutylamide RSinStandard solution 2;Wis the weight,in mg,in the portion of Powdered Extract taken;riis the sum of the peak responses of the relevant analytes obtained from theTest solution;and rSis the peak response obtained fromStandard solution 2.

Other requirements— It meets the requirements for Residual Solventsand Pesticide Residuesunder Botanical Extracts á565ñ.

Auxiliary Information— Staff Liaison:Gabriel I.Giancaspro,Ph.D.,Senior Scientist and Latin American Specialist

Expert Committee:(DSB)Dietary Supplements:Botanicals

USP28–NF23Page 2077

Pharmacopeial Forum:Volume No.30(2)Page 554

Phone Number:1-301-816-8343