1、Designation: F1925 09F1925 17Standard Specification forSemi-Crystalline Poly(lactide) Polymer and CopolymerResins for Surgical Implants1This standard is issued under the fixed designation F1925; the number immediately following the designation indicates the year oforiginal adoption or, in the case o
2、f 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.1. Scope1.1 This specification covers virgin semi-crystalline poly(L-lactide) or poly(D-lactide) homopolym
3、er resins intended for use insurgical implants. This specification also covers semi-crystalline resins of L-lactide copolymerized with other bioabsorbablemonomers including, but not limited to, glycolide, D-lactide, and DL-lactide. The poly(L -lactide) or poly(D-lactide) basedhomopolymers and copoly
4、mers covered by this specification possess lactide segments of sufficient length to allow potential fortheir crystallization upon annealing.1.2 Since poly(glycolide) is commonly abbreviated as PGA for poly(glycolic acid) and poly(lactide) is commonly abbreviatedas PLA for poly(lactic acid), these po
5、lymers are commonly referred to as PGA, PLA, and PLA:PGA resins for the hydrolyticbyproducts to which they respectively degrade. PLAis a term that carries no stereoisomeric specificity and therefore encompassesboth the amorphous atactic/syndiotactic DL-lactide based polymers and copolymers as well a
6、s the isotactic D-PLA and L-PLAmoieties, each of which carries potential for crystallization. Inclusion of stereoisomeric specificity within the lactic acid basedacronyms results in the following: poly(L-lactide) as PLLA for poly(L-lactic acid), poly(D-lactide) as PDLA for poly(D-lactic acid),and po
7、ly(DL-lactide) as PDLLA for poly(DL-lactic acid).1.3 This specification is applicable to lactide-based polymers or copolymers that possess isotactic polymeric segments sufficientin size to carry potential for lactide-based crystallization. Such polymers typically possess nominal mole fractions that
8、equal orexceed 50 % L-lactide. This specification is particularly applicable to isotactic-lactide based block copolymers or to polymers orcopolymers synthesized from combinations of D-lactide and L-lactide that differ by more than 1.5 total mole percent (1.5 % of totalmoles). This specification is n
9、ot applicable to lactide-co-glycolide copolymers with glycolide mole fractions greater than or equalto 70 % (65.3 % in mass fraction), which are covered by Specification F2313. This specification is not applicable to amorphouspolymers or copolymers synthesized from combinations of D-lactide and L-la
10、ctide that differ by less than 1.5 total mole percent(1.5 % of total moles) as covered by Specification F2579.1.4 This specification covers virgin semi-crystalline poly(lactide)-based resins able to be fully solvated at 30C by eithermethylene chloride (dichloromethane) or chloroform (trichloromethan
11、e). This specification is not applicable to lactide:glycolidecopolymers that possess glycolide segments sufficient in size to deliver potential for glycolide-based crystallization, therebyrequiring fluorinated solvents for complete dissolution under room temperature conditions (see Specification F23
12、13).1.5 Within this specification, semi-crystallinity within the resin is defined by the presence of a DSC (differential scanningcalorimetry) crystalline endotherm after annealing above the glass transition temperature. While other copolymeric segments mayalso crystallize upon annealing (for example
13、, glycolide), specific characterization of crystalline structures other than those formedby lactide are outside the scope of this specification.1.6 This specification addresses material characteristics of the virgin semi-crystalline poly(lactide) based resins intended for usein surgical implants and
14、 does not apply to packaged and sterilized finished implants fabricated from these materials.1.7 As with any material, some characteristics may be altered by processing techniques (such as molding, extrusion, machining,assembly, sterilization, and so forth) required for the production of a specific
15、part or device. Therefore, properties of fabricatedforms of this resin should be evaluated independently using appropriate test methods to assure safety and efficacy.1.8 Biocompatibility testing is not a requirement since this specification is not intended to cover fabricated devices.1.9 The values
16、stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1 This specification is under the jurisdiction of ASTM Committee F04 on Medical and Surgical Materials and Devices and is the direct responsibility of SubcommitteeF04.11 on Polymeric Materi
17、als.Current edition approved June 1, 2009Dec. 15, 2017. Published August 2009January 2018. Originally approved in 1998. Last previous edition approved in 20052009 asF1925 99 (2005).F1925 09. DOI: 10.1520/F1925-09.10.1520/F1925-17.This document is not an ASTM standard and is intended only to provide
18、the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the stan
19、dard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States11.10 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the
20、responsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine theapplicability of regulatory limitations prior to use.1.11 This international standard was developed in accordance with internationally recognized principles o
21、n standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1505 Test Method for Density of Plastics
22、 by the Density-Gradient TechniqueD2857 Practice for Dilute Solution Viscosity of PolymersD3417 Test Method for Enthalpies of Fusion and Crystallization of Polymers by Differential Scanning Calorimetry (DSC)(Withdrawn 2004)3D3418 Test Method for Transition Temperatures and Enthalpies of Fusion and C
23、rystallization of Polymers by DifferentialScanning CalorimetryD3536 Test Method for Molecular Weight Averages and Molecular Weight Distribution of Polystyrene by Liquid ExclusionChromatography (Gel Permeation ChromatographyGPC) (Withdrawn 1996)3D3593 Test Method for Molecular Weight Averages/ Distri
24、bution of Certain Polymers by Liquid Size-Exclusion Chromatog-raphy (Gel Permeation Chromatography GPC) Using Universal Calibration (Withdrawn 1993)3D4603 Test Method for Determining Inherent Viscosity of Poly(Ethylene Terephthalate) (PET) by Glass Capillary ViscometerE386D5296 Practice for Data Pre
25、sentation Relating to High-Resolution Nuclear Magnetic Resonance (NMR) SpectroscopyTestMethod for Molecular Weight Averages and Molecular Weight Distribution of Polystyrene by High PerformanceSize-Exclusion Chromatography (Withdrawn 2015)E473 Terminology Relating to Thermal Analysis and RheologyE793
26、 Test Method for Enthalpies of Fusion and Crystallization by Differential Scanning CalorimetryE794 Test Method for Melting And Crystallization Temperatures By Thermal AnalysisE967 Test Method for Temperature Calibration of Differential Scanning Calorimeters and Differential Thermal AnalyzersE968 Pra
27、ctice for Heat Flow Calibration of Differential Scanning CalorimetersE1142 Terminology Relating to Thermophysical PropertiesE1252 Practice for General Techniques for Obtaining Infrared Spectra for Qualitative AnalysisE1356 Test Method for Assignment of the Glass Transition Temperatures by Differenti
28、al Scanning CalorimetryE1994 Practice for Use of Process Oriented AOQL and LTPD Sampling PlansE2977 Practice for Measuring and Reporting Performance of Fourier-Transform Nuclear Magnetic Resonance (FT-NMR)Spectrometers for Liquid SamplesF748 Practice for Selecting Generic Biological Test Methods for
29、 Materials and DevicesF2313 Specification for Poly(glycolide) and Poly(glycolide-co-lactide) Resins for Surgical Implants with Mole Fractions GreaterThan or Equal to 70 % GlycolideF2579 Specification for Amorphous Poly(lactide) and Poly(lactide-co-glycolide) Resins for Surgical Implants2.2 ANSI Stan
30、dards:4ANSI/ISO/ASQ Q9000-2000 Quality Management Systems; Systems Fundamentals and VocabularyANSI/ISO/ASQ Q9001-2000 Quality Management Systems; Systems Requirements2.3 Other Documents:ISO Standards:ICH Q3C(R3) International Conference on Harmonisation of Technical Requirements for Registration of
31、Pharmaceuticals forHuman Use, Quality Guideline: Impurities: Residual Solvents55ISO 31-8ISO 80000-9 Physical Chemistry and Molecular PhysicsPart 8: Quantities and UnitsQuantities and units Part 9:Physical chemistry and molecular physicsISO 10993 Biological Evaluation of Medical Devices4ISO 11357 Pla
32、sticsDifferential Scanning Calorimetry (DSC)42 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The last appro
33、ved version of this historical standard is referenced on www.astm.org.4 Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.5 Available from ICH Secretariat, c/o IFPMA, 30 rue de St-Jean, P.O. Box 758, 1211 Geneva 13, Switzer
34、land. Available online at http:/www.ich.org/LOB/media/MEDIA423.pdf.International Organization for Standardization (ISO), ISO Central Secretariat, BIBC II, Chemin de Blandonnet 8, CP401, 1214 Vernier, Geneva, Switzerland,http:/www.iso.org.F1925 17221 CFR 820 United States Code of Federal Regulations,
35、 Title 21Food and Drugs Services, Part 820Quality SystemRegulation6USP United States Pharmacopeia, Edition 267NIST Special Publication SP811 Guide for the Use of the International System of Units (SI)82.4 Code of Federal Regulations:621 CFR 820 United States Code of Federal Regulations, Title 21Food
36、 and Drugs Services, Part 820Quality SystemRegulation2.5 United States Pharmacopeia:7USP, 26th Edition United States Pharmacopeia:USP Elemental Impurities LimitsUSP Elemental Impurities ProcedureUSP Physical Tests Optical RotationUSP Particulate Matter in Injections2.6 NIST Publication:8NIST Special
37、 Publication SP811 Guide for the Use of the International System of Units (SI)2.7 Other Document:ICH Q3C(R5) International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals forHuman Use, Quality Guideline: Impurities: Residual Solvents93. Terminology3.1 Defini
38、tions:3.1.1 virgin polymer, nthe initially delivered form of a polymer as synthesized from its monomers and prior to any processingor fabrication into a medical device.4. Materials and Manufacture4.1 All raw monomer components and other materials contacting either the raw monomer(s) or resin product
39、 shall be of aquality suitable to allow use of such resin in the manufacture of an implantable medical product. Such quality includes adequatecontrol of particles and other potential contaminants that may affect either the toxicity of or the cell response to the as-implantedor degrading final produc
40、t.4.2 All polymer manufacturing (including monomer handling, synthesis, pelletization/grinding and all subsequent handling)shall be undertaken under conditions suitable to allow use of such resin in the manufacture of an implantable medical product.4.3 Guidance related to the use of colorants (color
41、 additives) may be found through the US -FDAwebsite: https:/www.fda.gov/ForIndustry/ColorAdditives/.5. Chemical Composition5.1 The semi-crystalline poly(lactide) polymers and copolymers covered by this specification shall be composed of eitherD-lactide or L-lactide in segments of sufficient length t
42、o allow crystallization. Copolymers covered by this specification can be ofvariable copolymer ratios and shall be composed of crystallizable lengths of D-lactide and/or L-lactide in combination withglycolide or other monomers where the glycolide mole fraction is less than 70 % (65.3 % in mass fracti
43、on). To assure suchcomposition and the attainment of the desired properties, the following tests shall be conducted.5.2 Chemical Identification:5.2.1 The identity of the virgin polymer shall be confirmed either by infrared, 1H-NMR, or 13C-NMR spectroscopy.5.2.2 Infrared Identification:5.2.2.1 Identi
44、ty of semi-crystalline poly(lactide) homopolymer or poly(lactide)-based copolymer may be confirmed through aninfrared spectrum exhibiting major absorption bands only at the wavelengths that appear in a suitable reference spectrum.Analysisshall be conducted using infrared spectroscopy practicesmethod
45、s similar to those described in Practice E1252. A typical infraredtransmission reference spectrum for an L-PLA homopolymer is shown in Fig. 1. While poly(lactide)-based copolymers will eachhave their own respective spectrum that will vary in response to copolymer ratio, this analytic method typicall
46、y lacks sensitivitysufficient for quantification of copolymer ratio as specified in 7.1.2.6 Available from U.S. Government Printing Office Superintendent of Documents, 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/www.access.gpo.gov.7 Available from U.S. Pharmacopeia, 12601 Twi
47、nbrook Pkwy., Rockville, MD 20852 or through http:/www.usp.org/products/USPNF/. The standards will be listed byappropriate USP citation number. Succeeding USP editions alternately may be referenced.8 Available from National Institute of Standards and Technology (NIST), 100 Bureau Dr., Stop 1070, Gai
48、thersburg, MD 20899-1070, at http:/physics.nist.gov/cuu/Units/bibliography.html.9 See discussion regarding Heavy Metals General Test inAvailable from ICH Secretariat, c/o IFPMA, 30 rue Reagent Chemcialsde St-Jean, (10th Edition), AmericanChemical Society,Analytical Inorganic Subcommittee, MinutesOct
49、ober 5, 2005; available online at http:/pubs.acs.org/reagents/comminfo/minutes.html.P.O. Box 758, 1211Geneva 13, Switzerland. Available online at http:/www.ich.org/LOB/media/MEDIA423.pdf.F1925 1735.2.2.2 Additional or variable spectral bands may be indicative of sample crystallinity or either known or unknown impurities,including residual monomer, solvents, and catalysts (refer to limits specified in Table 1).5.2.2.3 Since an infrared spectrum cannot distinguish between the different lactide stereoisomers that is, poly(L-lactide) versuspoly(D-la
