ASTM F2224-2003 Standard Specification for High Purity Calcium Sulfate Hemihydrate or Dihydrate for Surgical Implants《外科植入物用高纯度硫酸钙半水合物或二水合物的标准规范》.pdf

1、Designation: F 2224 03Standard Specification forHigh Purity Calcium Sulfate Hemihydrate or Dihydrate forSurgical Implants1This standard is issued under the fixed designation F 2224; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, t

2、he year of last revision. 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 un-fabricated and fabricated forms of hydrated calcium

3、 sulfateintended for surgical implants. Fabricated forms may includepressed and cast surgical implants in various geometric shapes.The calcium sulfate hemihydrate in the unfabricated form canbe converted with the addition of water or other water-containing solutions to a fabricated calcium sulfate d

4、ihydrateform.1.2 The requirements of this specification apply to calciumsulfate combined with two molecules of water or two calciumsulfate molecules sharing one water molecule.Approximate chemical formulae:Calcium Sulfate DihydrateCaSO42H2OCalcium Sulfate HemihydrateCaSO41/2H2O or CaSO4H2OCaSO41.3 T

5、his specification specifically excludes calcium sulfateanhydrite and calcium sulfate forms that contain additives suchas reinforcing phases, medicaments, biological agents, and soforth.1.4 The presence of processing aids does not exclude aproduct from the physical and mechanical requirements of this

6、specification.1.5 Some provisions of Specification C 59/C 59M and TestMethods C 472 apply. Special requirements that are detailed inthis specification are included to characterize the materialwhich will be used in surgical implants.1.6 The biological response to calcium sulfate in bone tissuehas bee

7、n well characterized by a history of clinical use (1-14)2and by laboratory studies (15-18).1.7 The following precautionary caveat pertains only to thetest method portion, Sections 4, 5, and 6, of this specification.This standard does not purport to address all of the safetyconcerns, if any, associat

8、ed with its use. It is the responsibilityof the user of this standard to establish appropriate safety andhealth practices and determine the applicability of regulatoryrequirements prior to use.2. Referenced Documents2.1 ASTM Standards:C 59/C 59M Specification for Gypsum Casting Plaster andGypsum Mol

9、ding Plaster3C 472 Test Methods for Physical Testing of Gypsum, Gyp-sum Plasters and Gypsum Concrete3F 648 Specification for Ultra-High-Molecular-Weight Poly-ethylene Powder and Fabricated Form for Surgical Im-plants4F 756 Practice for Assessment of Hemolytic Properties ofMaterials4F 763 Practice fo

10、r Short-Term Screening of Implant Mate-rials4F 813 Practice for Direct Contact Cell Culture Evaluation ofMaterials for Medical Devices4F 895 Test Method for Agar Diffusion Cell Culture Screen-ing for Cytotoxicity4F 981 Practice for Assessment of Compatibility of Bioma-terials for Surgical Implants w

11、ith Respect to Effect ofMaterials on Muscle and Bone4F 1088 Specification for Beta-Tricalcium Phosphate forSurgical Implantation4F 1635 Test Method for In Vitro Degradation Testing ofPoly(L-lactic acid) Resin and Fabricated Form for SurgicalImplants42.2 Other Documents:BS 6463-102: 2001 Quicklime, H

12、ydrated Lime and NaturalCalcium CarbonatePart 102: Methods for ChemicalAnalysis5US Pharmacopeia XXIV (USP 24) NF-1961This specification is under the jurisdiction of ASTM Committee F04 onMedical and Surgical Materials and Devicesand is the direct responsibility ofSubcommittee F04.13on Ceramic Materia

13、ls.Current edition approved Jan. 10, 2003. Published February 2003.2The boldface numbers in parentheses refer to the list of references at the end ofthis standard.3Annual Book of ASTM Standards, Vol 04.01.4Annual Book of ASTM Standards, Vol 13.01.5Available from the British Standards Institution, c/

14、o IHS Engineering/IHSInternational, 15 Inverness Way East, Englewood, CO 80112.6Available from U.S. Pharmacopeia (USP), 12601 Twinbrook Pkwy., Rockville,MD 20852.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.CFR Title 21, Part 820

15、Quality System Requirements7Food Chemical Codex (FCC)8European Pharmacopeia9ISO 10993-1 Biological Evaluation of Medical Devices103. Terminology3.1 Definitions:3.1.1 calcium sulfate anhydritea chemical substance hav-ing approximate molecular formula of CaSO4.3.1.2 calcium sulfate dihydratea chemical

16、 having theapproximate molecular formula of CaSO42H2O. This sub-stance is also known as gypsum.3.1.3 calcium sulfate hemihydratea chemical substancehaving approximate molecular formula of CaSO41/2H2OorCaSO4H2OCaSO4. The mineral name of this substance isbassanite and the substance is also known as Pl

17、aster of Paris inthe clinical literature.3.1.4 processing aidsany constituent intentionally used inthe processing of the raw material to fulfill a certain techno-logical purpose during treatment or processing, which mayresult in the unintentional but technically unavoidable presenceof residues of th

18、e substance or its derivatives in the finalproduct (5 % by weight), provided that these residues do notpresent any health risk. Some examples would be: binders,lubricants, compaction aids, disintegrants, plasticizers, defloc-culants, wetting agents, water retention agents, antistaticagents, antifoam

19、 agents, foam stabilizers, chelating or seques-tering agents, phase stabilizers, and so forth.4. Chemical Requirements4.1 Calcium sulfate for surgical implants (raw material)shall have a purity of not less than 98 % for calcium sulfate(absent of water) when measured by USP 24 NF 19. (Thispurity meas

20、urement method may not be applicable to thefabricated forms containing substantial additives.)4.2 The concentration of trace elements in the calciumsulfate raw material shall be limited to less than 10 ppm of totalheavy metals (for example, arsenic, cadmium, mercury, andlead). Other metallic element

21、s, such as iron, may also affectimplant performance and should be kept to a minimum. Forexample, for calcium sulfate to meet USP grade, iron concen-tration should not be higher than 100 ppm. Methods formeasuring these trace elements are described in SpecificationF 1088 (Coupled PlasmaAtomic Absorpti

22、on Spectrometry),the United States Pharmacopeia (USP), European Pharma-copeia, or Food Chemical Codex (FCC). A second method thatmay be used to analyze acid insoluble impurities is describedin BS 6463-102.5. Physical and Mechanical Characterization5.1 The following physical and mechanical characteri

23、zationmay be applicable to calcium sulfate for surgical implantapplications in either the fabricated form or intra-operativefabricated form. When characterization test results are reportedin labeling, the test methods associated with these results shallbe referenced. Labeling can be defined as but i

24、s not limited tothe product label, brochures, technical monographs, and otherrelated documentation.5.2 Set TimeIf set time is an applicable property, it shouldbe reported along with the method by which it was determinedin order to inform the final user. The set time is defined as thetypical time for

25、 the development of an implantable surgicalimplant. Test Methods C 472 as described in SpecificationC 59/C 59M can be used to define a typical set time. The actualmethod used for set time determination shall be described orreferenced in labeling.5.3 Compressive StrengthCalcium sulfate dihydrate in a

26、fabricated final form is intended to be used in non-load bearingapplications. If applicable to implant performance, documen-tation of typical compressive strength and the methods used todetermine it should be reported in order to inform the final user.Test Methods C 472 as described in Specification

27、 C 59/C 59Mcan be used for the typical compression strength determination.The actual method used shall be described or referenced inlabeling.5.4 In vitro DegradationFor calcium sulfate dihydrate ina fabricated final form, weight loss from dissolution may bereported. If reported, the method used shou

28、ld be described orreferenced.6. Test Specimen Fabrication6.1 Prepare test specimens from the same batch of materialand by similar processes to those employed in fabricating theimplant device.7. Quality Program Requirements7.1 The manufacturer shall conform to Good ManufacturingPractices (see Title 2

29、1, part 820, of the Code of FederalRegulations) or its equivalent.8. Keywords8.1 bone; calcium sulfate; gypsum; implant; plaster7Available from U.S. Government Printing Office Superintendent of Documents,732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401.8Available from National Academy Pr

30、ess, 500 Fifth St., NW, Lockbox 285,Washington, DC 20055.9Available from EDQM, European Pharmacopeia, Council of Europe, B.P. 907,F-67029, Strasbourg, France.10Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.F2224032APPENDIX(Nonmandatory Info

31、rmation)X1. RATIONALEX1.1 The biocompatibility of calcium sulfate may dependupon processing conditions and source material, both whichmay not be identified by the compositional requirements of thisspecification. The biocompatibility of these products should beensured by a combination of preclinical

32、testing and processcontrols. Material derived under the desired process conditionsshould be tested in accordance with the recommendations ofPractices F 756, F 763, F 813, and F 981; Test Methods F 895and F 1635; Specification F 648; and ISO 10933-1, and manu-facturing controls put in place to ensure

33、 that process variationsoutside of acceptable tolerances do not occur. Substantialchanges in process conditions or source material parameterswill necessitate additional biocompatibility or preclinical func-tional testing to ensure maintenance of an acceptable tissueresponse.X1.2 X-ray powder diffrac

34、tion (XRD) analysis of thematerial provides differentiation between calcium sulfate dihy-drate and calcium sulfate hemihydrate. The International Cen-tre for Diffraction Data (ICDD) designation of calcium sulfatehemihydrate for surgical implants is ICDD # 41-0224 (Bas-sanite, syn). A typical calcium

35、 sulfate dihydrate XRD patternwill show the peaks from ICDD #s 33-0311 (Gypsum, syn),37-1496 (Anhydrite syn), and 41-0224 (Bassanite, syn).X1.3 The setting time measurement in Section 5 is usefulfor the calcium sulfate hemihydrate since the hemihydrate mustbe hydrated to a calcium sulfate dihydrate

36、before surgical use.Likewise, the calcium sulfate hemihydrate and dihydrate rawmaterial powders do not have the compressive strength ordegradation attributes that are needed for surgical applicationswithout being converted by hydration to calcium sulfatedihydrate or with the dihydrate form pressed i

37、nto a geometricshape.REFERENCES(1) Alexander, D. I., et al, “Efficacy of Calcium Sulfate Plus Decompres-sion Bone in Lumbar and Lumbosacral Spinal Fusion: PreliminaryResults in 40 Patients,” Can. J. Surg., 44(4), 2001, pp. 262-266.(2) Kelly, C. M., et al, “The Use of a Surgical Grade Calcium Sulfate

38、 asa Bone Graft Substitute,” Clin. Orthop. Rel. Res., 382, 2001, pp.42-50.(3) Mirzayan, R., et al, “The Use of Calcium Sulfate in the Treatment ofBenign Bone Lesions,” J. Bone Joint Surg., 83A(3), 2001, pp.355-358.(4) Peltier, L. F., “The Use of Plaster of Paris to Fill Defects in Bone,”Clin. Orthop

39、. Rel. Res., 21, 1961, pp. 1-31.(5) Peltier, L. F. and Speer, D. P., “Calcium Sulfate,” Bone Grafts andBone Substitutes, Habal, M. B. and Reddi, A. H., eds., W. B. SaundersCompany, 1993, pp. 243-246.(6) Damien, et al, “Bone Grafts and Bone Graft Substitutes,” J. AppliedBiomat., 2, 1991, pp. 187-208.(7) Bahn, S., “Plaster: A Bone Substitute,” Oral Surg. Oral Med. or through the ASTM website(www.astm.org).F2224034