ASTM F1581-1999 Standard Specification for Composition of Anorganic Bone for Surgical Implants《外科植入用无机骨料成分标准规范》.pdf

1、Designation: F 1581 99Standard Specification forComposition of Anorganic Bone for Surgical Implants1This standard is issued under the fixed designation F 1581; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisi

2、on. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This specification covers material requirements for an-organic xenogeneic or allogeneic bone (apatite) intended forsurgical impl

3、ants. For a material to be called anorganic ordeorganified bone, it must conform to this specification (seeAppendix X1).1.2 The biological response to apatite in soft tissue and bonehas been characterized by a history of clinical use2and bylaboratory studies (1,2,3). Xenogeneic bone, with organiccom

4、ponents present, has been shown to be antigenic in thehuman host (4) whereas the same material that has beencompletely deorganified has been shown to elicit no inflam-matory or foreign body reactions in human clinical use (5, 6,7).1.3 This specification specifically excludes synthetic hy-droxylapati

5、te, hydroxylapatite coatings, ceramic glasses, triba-sic calcium phosphate, whitlockite, and alpha- and beta-tricalcium phosphate.1.4 This standard does not pruport to address all of thesafety concerns, such as health concerns due to the presence oftransmissible disease, associated with its use. It

6、is the respon-sibility of the user of this standard to establish appropriatesafety and health practices and determine the applicability ofregulatory limitations prior to use.(See Appendix X2).2. Referenced Documents2.1 ASTM Standards:D 513 Test Methods for Total and Dissolved Carbon Diox-ide in Wate

7、r3D 1688 Test Methods for Copper in Water3D 2972 Test Methods for Arsenic in Water3D 3557 Test Methods for Cadmium in Water3D 3559 Test Methods for Lead in Water3D 3919 Practice for Measuring Trace Elements in Water byGraphite Furnace Atomic Absorption Spectrophotometry3D 4129 Test Method for Total

8、and Organic Carbon in WaterHigh Temperature Oxidation and Coulometric Detection4E 1184 Practice for Electrothermal (Graphite Furnace)Atomic Absorption Analysis5F 748 Practice For Selecting Generic Biological Test Meth-ods for Materials and Devices6F 1185 Specification for Composition of Ceramic Hydr

9、oxy-lapatite for Surgical Implants62.2 Code of Federal Regulations:7Title 21, Part 8202.3 National Formulary:8Tribasic Calcium Phosphate2.4 United States Pharmocopeia:9Identification Tests for Calcium and Phosphate Lead Mercury Cadmium Arnsenic Heavy Metals Method 1Nitrogen Determination 2.5 U.S. Ge

10、ological Survey Method:10Cadmium3. Terminology3.1 Definitions:3.1.1 allogeneic, adjderived from different individuals ofthe same species.3.1.2 anorganic, adjdenoting tissue (for example, bone)from which the organic material has been totally removed.Also referred to as deorganified, deproteinized or

11、deprotein-ated.3.1.3 apatite, nthe mineral substance having the molecu-lar formula Ca10(X)2(PO4)6where X=OH (hydroxyapatite orhydroxylapatite), CO3(carbonated apatite), F or C1 (8).1This specification is under the jurisdiction of ASTM Committee F04 onMedical and Surgical Materials and Devices and is

12、 under the direct responsibility ofSubcommittee F04.13 .Current edition approved Feb. 10, 1999. Published June 1999. Originallypublished as F 1581 95. Last previous edition F 1581 96.2The boldface numbers in parentheses refer to the list of references at the end ofthis specification.3Annual Book of

13、ASTM Standards, Vol. 11.01.4Annual Book of ASTM Standards, Vol. 11.02.5Annual Book of ASTM Standards, Vol. 03.06.6Annual Book of ASTM Standards, Vol. 13.01.7Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.8National For

14、mulary XVI. Available from U.S. Pharmacopeia Convention, Inc.,12601 Twinbrook Parkway, Rockville, MD 20852.9United States Pharmacopeia XXI. Available from U.S. Pharmacopeia Conven-tion, Inc., 12601 Twinbrook Parkway, Rockville, MD 20852.10Crock, J. G., Felichte, F. E., and Briggs, P. H., “Determinat

15、ion of Elements inNational Bureau of Standards Geological Reference Materials SRM 278 Obsidianand SRM 688 Basalt by Inductively Coupled Argon PlasmaAtomic EmissionSpectrometry.” Geostandards Newsletter, Vol 7, 1983, pp. 335340.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West C

16、onshohocken, PA 19428-2959, United States.3.1.4 xenogeneic, adjderived from individuals of a differ-ent, specified species. For example, bovine bone, when used asan implant material in humans, is xenogeneic.4. Chemical Requirements4.1 Elemental analysis for calcium and phosphorus will beconsistent w

17、ith the expected composition of the source of thebiologically derived bone mineral (9).4.2 An X-ray diffraction analysis of the material shall beconsistent with PDF card #9-432 for hydroxyapatite (10) orPDF card #35180 for calcium phosphate carbonate (carbon-ated apatite). Analysis of relative peak

18、intensities shall beconsistent with published data.114.3 The concentration of trace elements in the anorganicbone shall be limited as follows:Element ppm, maxAs 3Cd 5Hg 5Pb 30total heavy metals (as lead) 50For referee purposes, use either inductively coupled plasma/mass spectroscopy (ICP/MS) (11) or

19、 the United States Phar-mocopeia (USP) methods , , , ,Method 1, and for cadmium either orthe U.S. Geological Survey Method on Cadmium. (See 2.4 and2.5). Graphite furnace atomic absorption spectrophotometrymay also be used for ananlysis of trace elements using (TestMethods D 2972), Cd (Test Method D

20、1688), Pb (Test MethodsD 3559) with 1 g anorganic bone/100mL H2O samples. General guides for the application of the graphite furnace aregiven in Practices D 3919 and E 1184.4.4 The maximum allowable limit of all heavy metalsdetermined as lead will be 50 ppm as described in 2.4 orequivalent. Sample p

21、reparation will be identical to that fortribasic calcium phosphate as specified in the National Formu-lary (see 2.3), except that approximately1gofmaterial will bedissolved in approximately 30 mL of 5 % HCl and boiled.4.5 It is recommended that all minor constituents such asmetals or oxides not dete

22、cted as lead present in concentrationsequal to or greater than 0.1 % be identified and quantified.4.6 Organic content shall be measured either as total carbonor nitrogen (see Note 1) or total protein by amino acid analyses(13). For all methods, a synthetic hydroxylapatite control thatconforms to Spe

23、cification F 1185 or an established NISTstandard must be used. The maximum allowable limit of eithernitrogen, carbon, or protein will be within two standarddeviations of the mean value established for the control.NOTE 1The Kjeldahl process for nitrogen determination (USP) is set forth by the Associa

24、tion of Official Analytical Chemists (12)as an appropriate measure of proteins. Alternatively, organic material(carbon) can be measured by the coulometric method (Test MethodD 4129). Subtract from this value the carbonate content, which can bedetermined by Test Methods D 513.4.7 Functional groups wi

25、ll be identified by infrared analysis.Typical functional groups of apatites have been described byElliott (8), LeGeros et al (14), and Rey (15,16,17).4.8 Analysis of additional elements or ionic species associ-ated with the source or with processing conditions should bespecified for this material.5.

26、 Test Specimen Fabrication5.1 Prepare test specimens from the same batch of materialand by the same processes as those employed in fabricating theimplant device.6. Quality Program Requirements6.1 The manufacturer shall conform to Good ManufacturingPractices (see Title 21, Part 820, of the Code of Fe

27、deralRegulations7) or its equivalent.7. Biocompatibility7.1 The biocompatibility of anorganic bone may dependupon processing conditions or source material history, or both,which may not be identified by the compositional requirementsof this specification. The biocompatibility of these productsshould

28、 be ensured by a combination of preclinical testing andprocess controls. Material derived under the desired processconditions should be tested in accordance with the recommen-dations of Practice F 748 and manufacturing controls put inplace to ensure that process variations outside of acceptabletoler

29、ances do not occur. Substantial changes in process condi-tions or source control parameters will necessitate additionalbiocompatibility testing to ensure maintenance of an accept-able tissue response.8. Sterilization8.1 Anorganic bone may be supplied presterilized in accor-dance with current procedu

30、res set forth by the Association forthe Advancement of Medical Instrumentation (AAMI) andGood Manufacturing Practices (GMP) established by the Foodand Drug Administration (FDA).128.2 If user sterilization or resterilization is intended, vali-dated instructions for sterilization shall be supplied wit

31、h thepackage insert.9. Keywords9.1 allogeneic; anorganic; apatite; bone; hydroxyapatite;hydroxylapatite; implant; xenogeneic11The Joint Committee on Powdered Diffraction Standards has established aPowder Diffraction File. The Committee operates on an international basis andcooperates closely with th

32、e Data Commission of the International Union ofCrystallography and ASTM. Hydroxylapatite data can be found on file card number9-432 and is available from the Joint Committee on Powder Diffraction Standards,1600 Park Lane, Swarthmore, PA 19801.12Federal Register, Vol. 43, No. 141, Friday, July 21, 19

33、78.F1581992APPENDIXES(Nonmandatory Information)X1. RATIONALEX1.1 Xenogeneic and allograft bone is commercially avail-able as grafting material. To eliminate concerns about possibleimmunogenicity effects or partially purified bone, anorganic ordeorganified bone has been developed. To achieve reliable

34、biocompatibility as an implant material, this material must becharacterized for its hydroxylapatite mineral component andtrace element content as well as for the absence of organicmaterial. At the current time, sufficient data do not exist toprovide specific limits for carbon and nitrogen values. In

35、di-vidual laboratories must apply statistical analysis to showequivalence with the negative control. Test results that mightprovide data to assign specific limits for carbon and nitrogenare hereby solicited.X2. BIOCOMPATIBILITYX2.1 No known surgical implant material has ever beenshown to be complete

36、ly free of adverse reactions in the humanbody. However, long term clinical experience of the use of thematerial referred to in this standard has shown that anacceptable level of biological response can be expected, if thematerial is used in appropriate applications.REFERENCES(1) Hench, L.L., Wilson,

37、 J., An Introduction to Bioceramics, WorldScientific, 1993, pp. 139238.(2) Damien, C. J., and Parsons, J. R., “Bone Graft and Bone GraftSubstitutes: A Review of Current Technology and Applications,”Journal of Applied Biomaterials, Vol 2, 1991, pp. 187208.(3) Jarcho, M., Kay, J. F., Gumaer, K. I., Do

38、remus, R. H., and Drobeck,H. P., “Tissue, Cellular and Subcellular Events at a Bone-CeramicHydroxylapatite Interface,” Journal of Bioengineering, Vol. 1, 1977,pp. 7992.(4) Salama, R., and Gazit, E., “The Antigenicity of Kiel Bone in theHuman Host,” The Journal of Bone and Joint Surgery, Vol. 60-B No

39、.2, 1978, pp. 262265.(5) Urist, M.R., OConnor, B.T., Burwell, R.G., Bone Grafts, Derivativesand Substitutes, Butterworth-Heineman Ltd., 1994, pp 4142.(6) Begley, C.T., Doherty, M.J., Mollan, R.A., Wilson, D.J., “ComparativeStudy of the Osteoinductive Properties of Bioceramic, Coral andProcessed Bone

40、 Graft Substitutes”, Biomaterials, Vol 16. 1995, pp.11811185.(7) Callan, D.P., “Use of Bovine-Derived Hydroxyapatite in the Treatmentof Endentulous Ridge Defects: A Human Clinical and Histologic CaseReport”, Journal of Periodontology, Vol. 64, 1993, pp. 575582.(8) Elliott, J.C., Structure and Chemis

41、try of the Apatites and OtherCalcium Orthophosphates, Elsevier Science B.V., 1994, p.4(9) LeGeros, R.Z., LeGeros, J.P., Daculsi, G., Kijkowska, R., “CalciumPhosphate Biomaterials: Preparation, Properties, and Biodegradation”,Encylopedic Handbook of Biomaterials and Bioengineering, Part A:Materials,

42、Vol. 2, Marcel Dekker, 1995, pp. 14291463(10) Balmain, N., Legeros, R., and Bonel, G., “X-Ray Diffraction ofCalcified Bone Tissue: A Reliable Method for the Determination ofBone Ca/P Molar Ratio,” Calcified Tissue International, Vol 34,1982, pp. 593594.(11) Northington, D.J., “Inductively Couples Pl

43、asma-Mass Spectrometryfor the Analysis of Metals on Membrane Filters”, Am. Ind. Hyg.Assoc. J., Vol 48, 1987, pp. 977979.(12) Horwitz, W., Ed, Offcial Methods of Analysis of the Association ofAnalytical Chemists, Association of Official Analytical Chemists,Washington, DC, 1980, pp. 15, 214.(13) Ozols

44、, J., “Amino Acid Analysis”, in Guide to Protein Purification,Methods in Enzymology, Vol. 182, Editor M.P. Deutscher, 1990, pp.587601.(14) LeGeros, R.Z., Calcium Phosphates in Oral Biology and Medicine,Karger, 1991(15) Rey, C., Miquel, J.L., Facchini, L., Legrand, A.P., Glimcher, M.J.,“Hydroxyl Grou

45、ps in Bone Mineral”, Bone, Vol 16, 1995, pp.583586.(16) Rey, C., Collins, B., Goehl, T., Dickson, I.R., Glimcher, M.J., “TheCarbonate Environment in Bone Mineral: A Resolution-EnhancedFourier Transform Infrared Spectroscopy Study”, Calcified TissueInternational, Vol 45, 1989, pp. 157164.(17) Rey, C.

46、, Shimizu, M., Collins, B., Glimcher, M.J., “Resolution-Enhanced Fourier Transform Infrared Spectroscopy Study of theEnvironment of Phosphate Ions in the Early Deposits of a Solid Phaseof Calcium-Phosphate in Bone and Enamel, and their Evolution withAge. I: Investigations in the y4PO4Domain” Calcifi

47、ed TissueInternational, Vol 46, 1990, pp. 384394F1581993ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent

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