ANSI NSF 321-2016 Goldenseal Root (Hydrastis canadensis).pdf

1、NSF International Standard / American National StandardNSF/ANSI 321 - 2016Goldenseal Root (Hydrastis canadensis)NSF International, an independent, not-for-profit, non-governmental organization, is dedicated to being the leading global provider of public health and safety-based risk management soluti

2、ons while serving the interests of all stakeholders. This Standard is subject to revision. Contact NSF to confirm this revision is current. Users of this Standard may request clarifications and interpretations, or propose revisions by contacting: Chair, Joint Committee on Dietary Supplements c/o NSF

3、 International 789 North Dixboro Road, P. O. Box 130140 Ann Arbor, Michigan 48113-0140 USA Phone: (734) 769-8010 Telex: 753215 NSF INTL FAX: (734) 769-0109 E-mail: infonsf.org Web: http:/www.nsf.orgi NSF/ANSI 321-2016 NSF International Standard/ American National Standard for Botanical Dietary Suppl

4、ements Goldenseal Root (Hydrastis canadensis) Standard Developer NSF International Designated as an ANSI Standard October 6, 2016 American National Standards Institute ii Prepared by The NSF Joint Committee on Dietary Supplements Recommended for Adoption by The NSF Council of Public Health Consultan

5、ts Adopted by NSF International June 2010 Revised October 2016 Published by NSF International P. O. Box 130140, Ann Arbor, Michigan 48113-0140, USA For ordering copies or for making inquiries with regard to this Standard, please reference the designation “NSF/ANSI 321 2016.” Copyright 2017 NSF Inter

6、national Previous editions 2010 Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from NSF International. Printed in the United States of Ame

7、rica.iii Disclaimers1 NSF, in performing its functions in accordance with its objectives, does not assume or undertake to discharge any responsibility of the manufacturer or any other party. The opinions and findings of NSF represent its professional judgment. NSF shall not be responsible to anyone

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9、tation and protection of the public health. Provisions for mechanical and electrical safety have not been included in this Standard because governmental agencies or other national standards-setting organizations provide safety requirements. Participation in NSF Standards development activities by re

10、gulatory agency representatives (federal, local, state) shall not constitute their agencys endorsement of NSF or any of its Standards. Preference is given to the use of performance criteria measurable by examination or testing in NSF Standards development when such performance criteria may reasonabl

11、y be used in lieu of design, materials, or construction criteria. The illustrations, if provided, are intended to assist in understanding their adjacent standard requirements. However, the illustrations may not include all requirements for a specific product or unit, nor do they show the only method

12、 of fabricating such arrangements. Such partial drawings shall not be used to justify improper or incomplete design and construction. Unless otherwise referenced, the annexes are not considered an integral part of NSF Standards. The annexes are provided as general guidelines to the manufacturer, reg

13、ulatory agency, user, or certifying organization. 1 The information contained in this Disclaimer is not part of this American National Standard (ANS) and has not been processed in accordance with ANSIs requirements for an ANS. Therefore, this Disclaimer may contain material that has not been subject

14、ed to public review or a consensus process. In addition, it does not contain requirements necessary for conformance to the Standard. This page is intentionally left blank.v Contents 1 General . 1 1.1 Purpose 1 1.2 Scope . 1 2 Normative references . 1 3 Definitions . 2 4 Ingredient requirements 2 4.1

15、 AHP Pharmacopoeial Standard . 2 4.2 Sampling, preparation, and analysis of samples - High Performance Thin Layer Chromatography (HPTLC) for the Identification of Goldenseal Root . 4 4.3 High Performance Liquid Chromatography (HPLC) for the Quantification of Berberine and Hydrastine . 5 4.4 Limit te

16、sts . 7 4.5 Storage . 7 This page is intentionally left blank.vii Foreword2 The purpose of this Standard is to serve as an evaluation tool for analyzing the botanical dietary supplement Goldenseal Root (Hydrastis canadensis). NSF/ANSI 321 contains requirements for dietary supplements that contain go

17、ldenseal root as an ingredient. It allows for the determination that this botanical ingredient is accurately identified, that the product contains the quantity of dietary ingredients and marker constituents as determined by the American Herbal Pharmacopoeia (AHP), that the ingredient does not contai

18、n unacceptable quantities of contaminants, conforms to the compliance criteria of the AHP, and can be used to facilitate GMP compliance. Certification to this Standard serves as a communication tool between manufacturers of ingredients and finished product, retailers, healthcare practitioners, and c

19、onsumers. This Standard provides test methods and evaluation criteria to allow for the determination that a botanical dietary supplement identified as Goldenseal root contains the ingredients claimed on the label, either qualitatively or quantitatively, and that it does not contain specific undeclar

20、ed contaminants. In some instances, validated laboratory methods are not yet available for analyzing certain ingredients. In such cases, new methods will be added to this Standard as they become available. NSF offers a certification program to this Standard. Products certified by NSF carry the NSF M

21、ark, the leading mark in public health and safety certification around the world. The NSF Mark on a product gives consumers and retailers assurance that the product meets the requirements of the NSF Standard. For more information on the NSF certification program, please contact the General Manager o

22、f Dietary Supplements, P.O. Box 130140, Ann Arbor, MI 48113-0140 or at 1-800-NSF-MARK (800-673-6275). This Standard was developed by the NSF Joint Committee on Dietary Supplements using the NSF Consensus process accredited by the American National Standards Institute. Suggestions for improvement of

23、this Standard are welcome. This Standard is maintained on a Continuous Maintenance schedule and can be opened for comment at any time. Comments should be sent to Chair, Joint Committee on Dietary Supplements at standardsnsf.org, or c/o NSF International, Standards Department, P.O. Box 130140, Ann Ar

24、bor, Michigan, 48113-0140, USA. 2 The information contained in this Foreword is not part of this American National Standard (ANS) and has not been processed in accordance with ANSIs requirements for an ANS. Therefore, this Foreword may contain material that has not been subjected to public review or

25、 a consensus process. In addition, it does not contain requirements necessary for conformance to the Standard. This page is intentionally left blank.1 2017 NSF NSF/ANSI 321 2016 NSF International Standard for Botanical Dietary Supplements Goldenseal Root (Hydrastis canadensis) 1 General 1.1 Purpose

26、This Standard provides test methods for ensuring the identity, strength, purity, and composition of the dietary supplement ingredient Goldenseal root (Hydrastis canadensis) to allow for the determination that this botanical ingredient is accurately identified, that the product contains the quantity

27、of dietary ingredients and marker constituents as determined by the American Herbal Pharmacopoeia (AHP), that the ingredient does not contain unacceptable quantities of contaminants, conforms to the compliance criteria of the AHP, and can be used to facilitate GMP compliance. Other limit tests, such

28、 as for metals, microbes, and pesticides, are not included in the monograph. 1.2 Scope This Standard contains requirements for dietary supplements that contain goldenseal root as an ingredient in a dietary supplement as defined as a dietary substance for use by man to supplement the diet by increasi

29、ng the total dietary intake, or a concentrate, metabolite, constituent, extract, or combinations of these ingredients. With appropriate modifications to the testing methodology, this Standard can also apply to extracts of the ingredient. Products and ingredients deemed a hazard to public health or s

30、afety by a regulatory agency having jurisdiction shall be excluded from the scope of this document. 2 Normative references The following documents contain requirements, which by reference in this text, constitute requirements of this Standard. AHP, Goldenseal Root (Hydrastis canadensis): Standards o

31、f Analysis, Quality Control, when magnified it has the appearance of broken beeswax. The internal surface is bright yellow to orange-yellow in younger roots, changing to greenish-yellow or dark yellowish-brown in older roots. Occasionally there is a reddish hue to the central part of the root. The b

32、ark is thick and the wood is arranged in a quadrangular fashion. 4.1.2 Organoleptic characterization Aroma: Characteristic and persistent. Taste: Acrid and astringent, possessing a marked and unique bitterness stimulating salivation. Powder: Bright yellow to brownish-yellow. 4.1.3 Microscopic identi

33、fication 4.1.3.1 Rhizome: Preparation in chloral hydrate: Parenchyma tissue dominates the rhizome in cross section. The rhizome has a thin, yellowish-brown cork consisting of several thin-walled cell layers. The secondary phloem consists of parenchyma cells only; these are generally thin-walled, tho

34、ugh in the outer regions they may be somewhat thickened. The cells are rounded or polygonal in cross section and elongated in longitudinal view, and frequently contain yellow-brown, granular masses. Close to the cambium, semicircular regions of smaller cells indicate the sieve tubes and companion ce

35、lls. Interior to the cambium and associated with the phloem bundles are found narrow cuneiform groups of vessels separated by wide medullary rays. The vessels are small with numerous slit-shaped pits, bordered pits, or helical secondary walls. Many of the pitted vessels are filled with yellow, amorp

36、hous, granular masses. The thin-walled cells of the pith, as well as other parenchyma cells, contain single or compound starch granules with either a round or slit-shaped hilum. Calcium oxalate crystals, sclereids, and fibers are absent throughout. 4.1.3.2 Root: Preparation in chloral hydrate: Paren

37、chyma tissue dominates the root in cross section. The root is covered by a hypodermis of a single cell layer. The cortex consists of parenchyma cells only and is separated from the stele by a conspicuous primary endodermis, the cells of which often have sinuous walls. The stele shows the typical str

38、ucture of an oligarch radial bundle. Sclerenchymatous cells and crystals are absent. The primary diagnostic characteristics are the pervading yellow color, the minute starch grains, the absence of calcium oxalate crystals, the nature of the elements of the wood, and the absence of sclerenchymatous c

39、ells. 4.1.3.3 Powder: Goldenseal root powder contains numerous, mostly single, nearly spheroidal starch grains from 2-15 m in diameter, either free or in the parenchyma cells; fragments of the fibro-vascular bundles mostly associated with starch-bearing parenchyma; vessels with pitted (simple and bo

40、rdered) or helical secondary walls; and occasional fragments of tabular cork cells with yellowish- or reddish-brown walls and occasional granular masses attached to them. Powdered goldenseal root may be adulterated by goldenseal leaf. Goldenseal leaf powder is dark green and lacks the persistent cha

41、racteristic odor and 2016 NSF NSF/ANSI 321 2016 4 taste of the root. Pure goldenseal leaf or admixtures of root and leaf can be identified by the occurrence of leaf fragments with unicellular, thick-walled, acute trichomes (up to 600 m in length) and epidermal cells with wavy or sinuous walls. On fr

42、agments from the lower epidermis of the leaf, anomocytic stomata are often found. NOTE Goldenseal that has been improperly dried, stored, or that is old will have a greenish hue to it rather than a brilliant gold color. 4.2 Sampling, preparation, and analysis of samples - High Performance Thin Layer

43、 Chromatography (HPTLC) for the Identification of Goldenseal Root 4.2.1 Sample preparation In a test tube, 0.25 g of powdered drug is extracted in an ultrasonic bath at room temperature for 30 minutes with 4 mL of a methanol and water mixture (80:20). The suspension is filtered and the residue washe

44、d twice with 2 mL methanol. The filtrate and washings are combined and brought up to volume with methanol in a 20 mL volumetric flask. One mL of the solution is transferred into a small sample vial. This is the test solution. The solution is sensitive to light and heat and shall be stored in the ref

45、rigerator in an amber vial. Hydro alcohol extracts can be applied to the plate directly. Dried extracts can be dissolved in an appropriate solvent (e.g. methanol) and stirred and applied to the plate directly. 4.2.2 Standard preparation In a 50 mL volumetric flask, 25.0 mg (1R,9S)-b-hydrastine HCl,

46、1.0 mg hydrastinine HCl, 1.2 mg palmatine chloride, and 1.2 mg berberine chloride are dissolved in methanol. After dissolution is complete, the solution is brought up to volume with methanol. One mL of this solution is transferred into a small sample vial. This is the reference solution. NOTE Hydras

47、tine is light and heat sensitive and readily decomposes. 4.2.3 Ninhydrin reagent (optional) Ninhydrin reagent is prepared by dissolving 0.6 g Ninhydrin in 190 mL isopropanol/5 mL acetic acid. 4.2.4 Chromatographic conditions 4.2.4.1 Stationary phase: HPTLC plates 10 x 10 cm or 20 x 10 cm silica gel

48、60 F254. NOTE HPTLC plates allow for better separation, shorter development times, and less solvent. Standard TLC plates can also be used under the same conditions. 4.2.4.2 Solvent system: Ethyl acetate:methanol:formic acid:water (50:10:6:3). 4.2.4.3 Sample application: 5 L test solution and 5 L sta

49、ndard are applied each as an 8 mm band with 4 mm distance between bands. Application position should be 8 mm from lower edge of plate. 4.2.4.4 Development: 10 x 10 cm or 20 x 10 cm Twin Trough Chamber, chamber pre-saturated for 15 minutes, 5 mL or 10 mL, solvent, respectively, per trough Developing distance 60 mm from lower edge of plate. Dry plate in a 2016 NSF NSF/ANSI 321 2016 5 stream of cold air. 4.2.4.5 Detection: a) UV 254 nm. b) UV 366 nm. c) Ninhydrin reagent (optional): Immerse plate in or spray plate with reagent for 2 seconds, then dry in a stre