ASTM F2347-2015 Standard Guide for Characterization and Testing of Hyaluronan as Starting Materials Intended for Use in Biomedical and Tissue Engineered Medical Product Application.pdf

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1、Designation: F2347 15Standard Guide forCharacterization and Testing of Hyaluronan as StartingMaterials Intended for Use in Biomedical and TissueEngineered Medical Product Applications1This standard is issued under the fixed designation F2347; the number immediately following the designation indicate

2、s the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.INTRODUCTIONHyaluronan, which in this guide will encompass

3、 hyaluronic acid, hyaluronate, and its salt forms, isthe simplest of the glycosaminoglycans. Hyaluronan is soluble in water and forms highly viscoussolutions. Hyaluronan is found in ubiquitously in the body as part of the extracellular matrix of tissues,with high concentrations in the synovial fluid

4、, vitreous humor, and skin, as well as in cartilage.Hyaluronan has found uses in a variety of products ranging from viscosupplements (treatment ofosteoarthritis), adhesion prevention (prevention of post-surgical adhesions), viscoelastics (ocularprotection), and dermal implants (lip augmentation and

5、wrinkle removal). New applications, such asscaffolds for tissue engineering, are emerging. The aim of this guide is to identify key parametersrelevant to the characterization of hyaluronan for the development of new commercial applications ofhyaluronan for the biomedical and pharmaceutical industrie

6、s.1. Scope*1.1 This guide covers the evaluation of hyaluronan suitablefor use in biomedical or pharmaceutical applications, or both,including, but not limited to, Tissue Engineered MedicalProducts (TEMPs).1.2 This guide addresses key parameters relevant to thecharacterization and purity of hyalurona

7、n.1.3 As with any material, some characteristics of hyaluro-nan may be altered by processing techniques, such as cross-linking and sterilization, required for the production of aspecific formulation or device. Therefore, properties of fabri-cated forms of this polymer should be evaluated using testm

8、ethods that are appropriate to ensure safety and efficacy andare not addressed in this guide.1.4 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.5 This standard does not purport to address all of thesafety concerns, if any, as

9、sociated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory requirements prior to use.2. Referenced Documents2.1 ASTM Standards:2E1953 Practice for Description of Thermal Analysis and

10、Rheology ApparatusE2975 Test Method for Calibration of Concentric CylinderRotational ViscometersF619 Practice for Extraction of Medical PlasticsF748 Practice for Selecting Generic Biological Test Methodsfor Materials and DevicesF749 Practice for Evaluating Material Extracts by Intracuta-neous Inject

11、ion in the RabbitF756 Practice for Assessment of Hemolytic Properties ofMaterialsF763 Practice for Short-Term Screening of Implant Materi-alsF813 Practice for Direct Contact Cell Culture Evaluation ofMaterials for Medical DevicesF895 Test Method forAgar Diffusion Cell Culture Screeningfor Cytotoxici

12、tyF981 Practice for Assessment of Compatibility of Biomate-rials for Surgical Implants with Respect to Effect of1This guide is under the jurisdiction of ASTM Committee F04 on Medical andSurgical Materials and Devicesand is the direct responsibility of SubcommitteeF04.42 on Biomaterials and Biomolecu

13、les for TEMPs.Current edition approved Dec. 1, 2015. Published February 2016. Originallyapproved in 2003. Last previous edition approved in 2011 as F2347 11. DOI:10.1520/F2347-15.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org.

14、 For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1Mat

15、erials on Muscle and BoneF1439 Guide for Performance of Lifetime Bioassay for theTumorigenic Potential of Implant MaterialsF1903 Practice for Testing For Biological Responses toParticles In VitroF1904 Practice for Testing the Biological Responses toParticles in vivo2.2 USP Documents:3USP Microbial L

16、imit TestsUSP Sterility TestsUSP Bacterial Endotoxins TestsUSP Heavy MetalsUSP Loss on DryingUSP Sterilization and Sterility Assurance of Com-pendial Articles2.3 EP Documents:4EP Monograph 1472 Sodium HyaluronateEP 2.6.1 Sterility2.4 Other Referenced Documents:ISO 10993 Biological Evaluation of Medi

17、cal Devices5ISO 10993-1 Biological Evaluation of Medical DevicesPart 1: Evaluation and TestingISO 10993-7 Biological Evaluation of Medical DevicesPart 7: Ethylene Oxide Sterilization ResidualsISO 10993-9 Biological Evaluation of Medical DevicesPart 9: Framework for Identification and Quantification

18、ofPotential Degradation ProductsISO 10993-17 Biological Evaluation of Medical DevicesPart 17: Establishment of Allowable Limits for LeachableSubstancesISO 14160: 1998 Sterilization of Single-Use Medical De-vices Incorporating Materials of Animal OriginValidation and Routine Control of Sterilization

19、by LiquidChemical Sterilants5ISO 11737-1: 1995 Sterilization of Medical DevicesMicrobiological MethodsPart 1: Estimation of Popula-tion of Microorganisms on Products5ISO 11737-2: 1998 Sterilization of Medical DevicesMicrobiological MethodsPart 2: Tests of Sterility Per-formed in the Validation of a

20、Sterilization Process5ISO 13408-1: 1998 Aseptic Processing of Health CareProductsPart 1: General Requirements5ISO EN 12442-1 Animal Tissues and Their DerivativeUtilized in the Manufacture of Medical DevicesPart 1:Analysis and Management of Risk5ISO EN 12442-3 Animal Tissues and Their DerivativeUtili

21、zed in the Manufacture of Medical DevicesPart 3:Validation of the Elimination and/or inactivation of Virusand Transmissible Agents5ICH S2B A Standard Battery for Genotoxicity Testing ofPharmaceuticals (July 1997)6ICH Q1A Harmonized Tripartite Guidance for StabilityTesting of New Drug Substances and

22、Products (September2001, Revision 1)6FDA Guideline on Validation of the Limulus AmebocyteTest as an End-Product Endotoxin Test for Human andAnimal Parenteral Drugs, Biological Products and Health-care Products, DHHS, December 19877FDA Interim Guidance for Human and Veterinary DrugProducts and Biolog

23、icals, Kinetic LAL Techniques,DHHS, July 15, 19917AAMI TIR No. 7: 1999 Chemical Sterilants and High LevelDisinfectants: A Guide to Selection and Use8AAMI ST67/CDV2: 1999 Sterilization of MedicalDevicesRequirements for Products Labeled “Sterile”821 CFR 312 FDA Title 21, Food and Drugs, Investigationa

24、lNew Drug Applications93. Terminology3.1 Definitions:3.1.1 decomposition, nstructural changes of hyaluronandue to exposure to environmental, chemical, or thermal factors.Decomposition may occur at temperatures as low as 121Cduring autoclaving. Decomposition can result in deleteriouschanges to the hy

25、aluronan.3.1.2 degradation, nchange in the chemical structure,physical properties or appearance of a material. Degradation ofpolysaccharides occurs via cleavage of the glycosidic bonds,usually by acid catalyzed hydrolysis. Degradation can alsooccur thermally and by alkali. It is important to note th

26、atdegradation is not synonymous with decomposition. Degrada-tion is often used as a synonym for depolymerization whenreferring to polymers. Degradation (depolymerization) of hy-aluronan may also occur enzymatically by the action ofhyaluronidases.3.1.3 depolymerization, nreduction in length of a poly

27、merchain to form shorter polymeric units. Depolymerization mayreduce the polymer chain to smaller molecular weightpolymers, oligomeric, or monomeric units, or combinationthereof. In hyaluronan, acid hydrolysis of the glycosidic bondsis the primary mechanism.3.1.4 endotoxin, npyrogenic high molar mas

28、s lipopolysac-charide (LPS) complex associated with the cell wall ofgram-negative bacteria.3.1.4.1 DiscussionThough endotoxins are pyrogens, notall pyrogens are endotoxins. Endotoxins are specifically de-tected through a Limulus Amebocyte Lysate (LAL) test.3.1.5 hyaluronan, na polysaccharide with a

29、disacchariderepeating unit composed of D-glucuronic acid and N-acetyl-D-glucosamine in -(13) linkage. Each disaccharide unit isattached to the next by -(14) bonds. Hyaluronan is a linearpolymer. Other common names are hyaluronic acid and sodiumhyaluronate.3Available from U.S. Pharmacopeia (USP), 126

30、01 Twinbrook Pkwy., Rockville,MD 20852.4Available from European Directorate for the Quality of Medicines (EDQM),Council of Europe, BP 907, 67029 Strasbourg, France.5Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.6Available from International

31、 Conference on Harmonization (ICH) Secretariat,c/o IFPMA, 30 rue de St-Jean, P.O. Box 758, 1211 Geneva 13, Switzerland.7Available from U.S. Food and Drug Administration, 5600 Fishers Lane,Rockville, MD 20857-0001.8Available from Association for the Advancement of Medical Instrumentation,1110 North G

32、lebe Rd., Suite 220, Arlington, VA 22201-4795.9Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098F2347 1523.1.6 hydrocolloid, na water-soluble polymer of colloidalnature when hydrated.3.1.7 molecular mass average (molecular w

33、eight average),nthe given molecular weight (Mw) of hyaluronan will alwaysrepresent an average of all of the molecules in the population.The most common ways to express the Mw are as the numberaverage (Mn) and the weight average (Mw). The two averagesare defined by the following equations:MHn5(iNiMi(

34、iNiand MHw5(iwiMi(iwi5(iNiMi2(iNiMiwhere:Ni= number of molecules having a specific molecularweight Mi, andwi= weight of molecules having a specific molecular weightMi.In a polydisperse molecular population the relation MwMnis always valid. The coefficient Mw/Mnis referred to as thepolydispersity ind

35、ex, and will typically be in the range 1.2 to3.0 for commercial hyaluronan.3.1.8 non-animal derived, na term describing the absenceof any animal-derived tissue, proteins, or products in themanufacturing process.3.1.9 pyrogen, nany substance that produces fever whenadministered parenterally.4. Signif

36、icance and Use4.1 This guide contains a listing of those characterizationparameters that are directly related to the functionality ofhyaluronan. This guide can be used as an aid in the selectionand characterization of the appropriate hyaluronan for aparticular application. This guide is intended to

37、give guidancein the methods and types of testing necessary to properlycharacterize, assess, and ensure consistency in the performanceof a particular hyaluronan. It may have use in the regulation ofthese devices by appropriate authorities.4.2 The hyaluronan covered by this guide may be gelled,cross-l

38、inked, extruded, or otherwise formulated into biomedi-cal devices for use in tissue engineered medical products ordrug delivery devices for implantation as determined to beappropriate, based on supporting biocompatibility and physicaltest data. Recommendations in this guide should not beinterpreted

39、as a guarantee of clinical success in any tissueengineered medical product or drug delivery application.4.3 To ensure that the material supplied satisfies require-ments for use in TEMPs, several general areas of characteriza-tion should be considered. These are: identity of hyaluronan,physical and c

40、hemical characterization and testing, impuritiesprofile, and performance-related tests.5. Chemical and Physical Test Methods5.1 Identity of HyaluronanThe identity of hyaluronan canbe established by several methods including, but not limited tothe following:5.1.1 Sodium Hyaluronate Monograph EP Monog

41、raph1472.5.1.2 Fourier Transform Infrared Spectroscopy (FT-IR)Almost all organic chemical compounds absorb infrared radia-tion at frequencies characteristic for the functional groups inthe compound. A FT-IR spectrum will show absorption bandsrelating to bond stretching and bending and can therefore

42、serveas a unique fingerprint of a specific compound. Direct FT-IRanalysis of hyaluronan powder is perhaps the easiest techniqueto perform. One method utilizes a horizontal attenuated totalreflectance (HATR) accessory with a zinc-selenium (ZnSe)crystal (or equivalent) having a sample trough and a pre

43、ssureplate. Record background and sample spectra between 4000and 600 cm-1at an appropriate resolution. Label the peaks.Typical frequencies (cm-1) for hyaluronan (sodium salt) are3275-3390 (b), 1615 (s), 1405 (m), 1377 (m), 1150, 1077, 1045(s), 946 (m), 893 (w). The peak designators are: sh: sharp; s

44、:strong; m: medium; w: weak; b: broad. A typical FT-IR HATRspectrum is shown in Fig. 1. A reference spectrum can beobtained from the European Pharmacopoeia.105.2 Physical and Chemical Characterization of Hyaluro-nan:5.2.1 The composition and sequential structure of hyaluro-nan can be determined by t

45、he following method: High-resolution1H- and13C-nuclear magnetic resonance spectros-copy (NMR). Hyaluronan should be dissolved in D2O. If theresulting solution is viscous, viscosity may be reduced bychemical or enzymatic depolymerization. A typical1H-NMRspectrum of hyaluronan is shown below. Hyaluron

46、an is char-acterized by calculating parameters such as glucuronic acid:N-acetylglucosamine ratio. Some literature references to thedetermination of composition and structure of hyaluronan aregiven in the References section (1-4).115.2.2 Molecular mass (molecular weight) of hyaluronan willdefine cert

47、ain performance characteristics such as viscosity orgel strength, or both. As such and depending on the sensitivityof a particular end use to these variations, determination ofmolecular mass directly or indirectly may be necessary. Com-mercial hyaluronan is polydisperse with respect to molecularweig

48、ht (Mw). Mwmay be expressed as the number average(MN) or the weight average (MW). Molecular weights may bedetermined by methods such as, but not limited to the follow-ing:5.2.2.1 Molecular Weight Determination Based on IntrinsicViscosityThe intrinsic viscosity describes a polymers abilityto form vis

49、cous solutions in water and is directly proportionalto the average molecular weight of the polymer. The intrinsicviscosity is a characteristic of the polymer under specifiedsolvent and temperature conditions; it is independent of con-centration. The intrinsic viscosity () is directly related to themolecular weight of a polymer through the Mark-Houwink-Sakurada (MHS) equation: =KMa. For hyaluronan, K is0.00057 and the exponent (a) is 0.75 at the following condi-tions: 0.15 M NaCl in phosphate buffer, pH 7.5, 20C (5).Bymeasuring the intrinsi