ASTM F2847-2010 Standard Practice for Reporting and Assessment of Residues on Single Use Implants《报告和评定一次性植入物上残留物的标准操作规程》.pdf

1、Designation: F2847 10Standard Practice forReporting and Assessment of Residues on Single UseImplants1This standard is issued under the fixed designation F2847; 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 () indicates an editorial change since the last revision or reapproval.1. Scope1.1 The purpose of this practice is to describe how thecleanliness of single use implants as manufactured shall bereported. This prac

3、tice proposes how to approach the identifi-cation of critical compounds and suggests different analyticalmethods.1.2 The practice does not address substances which areintrinsic to the implant properties or design. In particular, itdoes not address substances released during implant resorption,implan

4、t coatings, or leachables by design.1.3 This practice does not address the cleanliness of im-plants which are re-processed, re-cleaned after unpacking forre-use in the hospital or by the manufacturer.1.4 This practice does not establish limit values for residues.1.5 This practice suggests appropriat

5、e test methods for thegeneral specification of residues and residue requirements ofimplants. This practice may also be used to characterizesemi-finished components for implants.1.6 The test methods suggested and described herein refer toestablished analytical methods and to existing standard meth-od

6、s for chemical, biochemical, or biological analysis.1.7 This practice is intended solely to provide guidanceregarding suitable test methods and reporting conventions forresidues, which may or may not affect implant biocompatibil-ity. This practice does not suggest or recommend test methodsfor biocom

7、patibility, which may be found in Practice F748 orin ISO 10993-1.1.8 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the appl

8、ica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E996 Practice for Reporting Data in Auger Electron Spec-troscopy and X-ray Photoelectron SpectroscopyE1078 Guide for Specimen Preparation and Mounting inSurface AnalysisE1504 Practice for Reporting Mass Spec

9、tral Data in Sec-ondary Ion Mass Spectrometry (SIMS)E1635 Practice for Reporting Imaging Data in SecondaryIon Mass Spectrometry (SIMS)E1829 Guide for Handling Specimens Prior to SurfaceAnalysisF561 Practice for Retrieval and Analysis of Medical De-vices, and Associated Tissues and FluidsF748 Practic

10、e for Selecting Generic Biological Test Meth-ods for Materials and DevicesF1251 Terminology Relating to Polymeric Biomaterials inMedical and Surgical DevicesF1877 Practice for Characterization of ParticlesF2459 Test Method for Extracting Residue from MetallicMedical Components and Quantifying via Gr

11、avimetricAnalysisF2809 Terminology Relating to Medical and Surgical Ma-terials and DevicesG121 Practice for Preparation of Contaminated Test Cou-pons for the Evaluation of Cleaning AgentsG131 Practice for Cleaning of Materials and Componentsby Ultrasonic TechniquesG136 Practice for Determination of

12、Soluble Residual Con-taminants in Materials by Ultrasonic Extraction2.2 ISO Standards:3ISO 10993-1 Biological Evaluation of Medical DevicesPart 1: Evaluation and Testing1This practice is under the jurisdiction ofASTM Committee F04 on Medical andSurgical Materials and Devices and is the direct respon

13、sibility of SubcommitteeF04.15 on Material Test Methods.Current edition approved Dec. 1, 2010. Published January 2011. DOI: 10.1520/F284710.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volum

14、e information, refer to the standards Document Summary page onthe ASTM website.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428

15、-2959, United States.ISO 10993-17 Biological Evaluation of Medical DevicesPart 17: Establishment of Allowable Limits for LeachableSubstancesISO 10993-18 Biological Evaluation of Medical DevicesPart 18: Chemical Characterization of MaterialsISO 11737-1 Sterilization of Medical DevicesMicrobiological

16、MethodsPart 1: Determination of aPopulation of Microorganisms on Products2.3 United States Pharmacopeia (USP) Document:4Bacterial Endotoxin Test2.4 European Pharmacopoeia (PhEUR) Documents:52.2.23 Atomic Absorption Spectrometry2.2.24 Absorption Spectrophotometry, Infrared2.2.25 Absorption Spectropho

17、tometry, Ultraviolet and Vis-ible2.2.28 Gas Chromatography2.2.29 Liquid Chromatography2.2.43 Mass Spectrometry2.2.44 Total Organic Carbon in Water for PharmaceuticalUse2.2.48 Raman Spectrometry2.2.55 Peptide Mapping2.2.57 Inductively Coupled Plasma-Atomic Emission Spec-trometry2.2.58 Inductively Cou

18、pled Plasma-Mass Spectrometry2.5 Association for the Advancement of Medical Instrumen-tation (AAMI) Document:6AAMI ST72 Bacterial EndotoxinsTest Methodologies,Routine Monitoring, and Alternatives to Batch Testing2.6 Other References:FDA Guideline on Validation of the Limulus AmebocyteLysate Test as

19、an End-Product Endotoxin Test for Humanand Animal Parenteral Drugs, Biological Products, andMedical Device, 19877200.7 EPA Methodologies for ICP88270C EPA Methodologies for GC-MS83. Terminology3.1 Unless provided otherwise in 3.2, terminology shall bein conformance with Terminology F1251 and with Te

20、rminol-ogy F2809.3.2 Definitions:3.2.1 action value, nthe amount(s) of substance(s) toler-ated at the surface of an implant by the manufacturer before itwill interfere with the manufacturing process.3.2.2 exhaustive extraction, nextraction until the cumula-tive residue change is analytically insigni

21、ficant or less than10 % of the initial extract.3.2.3 limit value, nthe maximum allowable amount(s) ofsubstance(s) at the surface of an implant not yet found to beharmful for the surrounding tissues and organs. Its value isestablished and defined by the manufacturer.3.2.4 model residue, na single sub

22、stance or a mixture ofsubstances that reflect the process materials likely to beencountered and used during the manufacturing of the device.3.2.5 residue, na substance present at the surface of animplant or embedded therein that is not explicitly recognizedand defined as part of the implant specific

23、ation (specialdefinition for residue analysis of surfaces). It includes process-based residues as well as contamination by environmentalfactors (adsorbates).3.2.6 single use implant, na medical device which in-tended use is to be implanted permanently and that is notre-cleaned or re-worked for a sec

24、ond implantation after even-tual removal.3.2.7 soiling, nprocedure of applying known amounts of asubstance onto a medical device for determination of processcapability, that is, cleaning efficiency and extraction yields.3.2.8 spiking, nprocedure of applying exact quantities ofa substance to an analy

25、te for instrumental calibration anddetermination reaction yield.3.2.9 surface area, nthe projected surface area of a part.This area does not include the internal porosity of parts withcancellous, porous, or wire structure. It does include factorsthat correct for the estimated surface roughness.4. Su

26、mmary of Practice4.1 This practice describes how to report residues on im-plant surfaces and indicates useful and typical applicableanalytical methods.4.2 Application of the test methods contained within thispractice does not guarantee clinical success of a finishedimplant, but it will help to ensur

27、e consistency in its cleanliness.5. Significance and Use5.1 The quality and consequently the clinical performanceof implants may be affected by residues. Residues may induceno tissue response, minor tissue irritations, or they may lead tolocal inflammation of tissues surrounding the implant whichmay

28、 lead to failure in short-term or long-term use. Residuesmay also cause harm at locations away from the implant.Residues may originate from manufacturing materials used inthe course of processing, or may be the result of handling andpackaging (1-3).95.2 This practice shall be used to report the resu

29、lts of testingfor residue. All residues cannot necessarily be detected. Itsuggests standard techniques that may be applied for analysis,and provides suggestions for how limit values may be set.5.3 Residues may be of inorganic, organic, or biologicalnature. They may exhibit as surface bound substance

30、, or as an4Available from U.S. Pharmacopeia (USP), 12601 Twinbrook Pkwy., Rockville,MD 20852-1790, http:/www.usp.org.5Available from European Directorate for the Quality of Medicines andHealthCare (EDQM), 7 allee Kastner, CS 30026, F67081, Strasbourg, France,http:/www.edqm.eu/en/News-and-General-Inf

31、ormation-43.html.6Available from Association for the Advancement of Medical Instrumentation(AAMI), 4301 North Fairfax Drive, Suite 301, Arlington, VA 22203, http:/www.aami.org.7Available from Food and Drug Administration (FDA), 5600 Fishers Ln.,Rockville, MD 20857, http:/www.fda.gov.8Available from

32、United States Environmental Protection Agency (EPA), ArielRios Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460, http:/www.epa.gov.9The boldface numbers in parentheses refer to the list of references at the end ofthis standard.F2847 102adsorbate (for example, electrostatically held), an efflo

33、res-cence, or a mechanically held substance. Residues may besoluble in aqueous media, soluble in organic solvents, or maybe insoluble particulates.5.4 Data generated in validation processes, that is, cleaningvalidation or sterility validation may be used as results or asbasis for setting acceptance

34、criteria in the report.6. Reporting of Residues on Implants6.1 The reporting of cleanliness of implants shall include atable that lists at least sections on (1) the chemical categories,(2) the results of validation studies or of routine analysis, (3)the acceptance criteria if applicable, (4) the det

35、ection limits ofthe methods used, and (5) the methods of analysis (see Table1).6.2 Categories of Residues:6.2.1 Residues shall be classified, as needed, according tothe common description and reported accordingly as (I) inor-ganic, (II) organic, (III) biologic, (IV) microbiological, and (V)particula

36、te residues.6.2.2 In this practice, inorganic residues are referred to assubstances of all elements with the exception of carbon-containing substances. Carbonates, graphite or graphite-likestructures (for example, diamond like coatings) are tradition-ally listed as inorganic substances.6.2.3 In this

37、 practice, organic residues are referred to assynthetic and natural carbon-based substances. It includes bothsmall molecules with low molecular mass (for example,paraffin or low viscosity oil) and high molecular mass basedsynthetic polymers. Polysilanes and -oxanes are also consid-ered organic resid

38、ues.6.2.3.1 In this practice, microbiologic residues are to belisted separately and differentiated as bioburden and endotoxin.It should be noted that for medical devices sold sterile,bioburden testing is often part of sterilization validation and ismonitored on a predetermined schedule for the purpo

39、se of doseaudits or process control.6.2.4 In this practice, particulate residues are referred to asmaterial insoluble in aqueous media or organic solvent, whichcan be removed from the surface of an implant by physical-chemical means without interfering with the integrity of theimplant surface. Even

40、though particulates shall be reportedseparately, they belong to one of the chemical classes men-tioned above.6.3 Reported Units:6.3.1 Results of inorganic and organic analysis shall bereported as mass per implant and/or mass per surface area (useSI units).6.3.2 Results of biological analysis shall b

41、e reported in thespecific units per implant, that is, enumeration methods such ascolony forming unit (CFU), or enzymatic assays such as forexample, endotoxin units (EU).6.3.3 Results of particulate analysis shall be reported inmass per implant, mass per surface area, number per device,number per sur

42、face area, or atomic-%, or fraction per surfacearea. The size range of particulates considered in the analysis(for example, based on filter pore sizes, capillaries, diffractionsettings) shall be reported.6.3.4 Results of surface analysis shall be reported asatomic-%, molecular-%, or fraction per sur

43、face area.6.4 Identification of ResiduesResidues that have beenidentified shall be listed separately in the report if they areconsidered significant by the practitioner of this practice.7. Quality Assurance7.1 The cleanliness of the implant shall be determined usingthe final product after packaging.

44、 Assessment can also beTABLE 1 Suggested Table for Reporting of ResiduesNOTE 1The reported table shall reflect the mean value of all measurements of a product and the error including the error of the method.NOTE 2The column Applied Analytical Method exemplifies methods and applicable standards. They

45、 can be replaced by any method/standardprotocol suitable for the particular residues.CategoriesResults ofAnalysisSet LimitValuesDetection LimitApplied AnalyticalMethodsInorganic mass/implantmass/surface areamass/implantmass/surface areamass/implantmass/surface areaICP-OES(PhEur 2.2.57)Organic GC-MS(

46、PhEur 2.2.28,EPA 8270C)Biological e-spray MS(PhEur 2.2.43)Bioburden CFU/implant CFU/implant CFU/implant ISO 11737-1Endotoxin EU/implant EU/implantAEU/implant USPAAMI ST72Particulate mass/implantmass/surface areaNumber/implantor cm2/cm2Atomic-%or Molecular-%mass/implantmass/surface areaNumber/ implan

47、tor cm2/cm2Atomic-%or Molecular-%mass/implantmass/surface areaNumber/implantor cm2/cm2Atomic-%or Molecular-%SEM (internal protocol)XPS (ASTM E996)Visual Inspection Optical observations Optical observations Optical observations (internal protocol)ALimit value as defined for device types listed in FDA

48、 Guidance for Industry and Guideline on Validation of the Limulus Amebocyte Lysate Test as an End-ProductEndotoxin Text for Human and Animal Parenteral Drugs, Biological Products, and Medical Devices (December 1987).F2847 103performed at various stages along the manufacturing processfor manufacturin

49、g control or validation.NOTE 1Sterilization processes can affect the chemical and biologicalnature of residues. The manufacturer may elect to assess the residuecontent before and after sterilization. In the case of bioburden, testing hasto be performed before sterilization.7.2 Each method of analysis shall be validated individuallyin the laboratory conducting the analysis.7.3 The manufacturing process for the implant being ana-lyzed shall be reviewed regarding manufacturing materialsused, for e