ASTM F619-2003(2008) Standard Practice for Extraction of Medical Plastics《医用塑料制品萃取的标准实施规程》.pdf

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1、Designation: F 619 03 (Reapproved 2008)Standard Practice forExtraction of Medical Plastics1This standard is issued under the fixed designation F 619; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A numb

2、er in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This practice covers methods of extraction of medicalplastics and may be applicable to other materials. This practiceidentifies a method fo

3、r obtaining “extract liquid” for use indetermining the biological response in preclinical testing.Further testing of the “extract liquid” is specified in otherASTM standards. The extract may undergo chemical analysisas part of the preclinical evaluation of the biological response,and the material af

4、ter extraction may also be examined.1.2 This practice may be used for, but is not limited to thefollowing areas: partial evaluation of raw materials, auditingmaterials within the manufacturing process, and testing finalproducts. This practice may also be used as a referee methodfor the measurement o

5、f extractables in plastics used in medicaldevices.1.3 The values stated in inch-pound units are to be regardedas standard. The values given in parentheses are mathematicalconversions to SI units that are provided for information onlyand are not considered standard.1.4 This standard does not purport

6、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 applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 543 P

7、ractices for Evaluating the Resistance of Plastics toChemical ReagentsD 570 Test Method for Water Absorption of PlasticsD 1193 Specification for Reagent WaterD 1239 Test Method for Resistance of Plastic Films toExtraction by ChemicalsD 1898 Practice for Sampling of Plastics3F 748 Practice for Select

8、ing Generic Biological Test Meth-ods for Materials and Devices2.2 Other Documents:USP NF 24 or current edition43. Terminology Definitions3.1 extraction vehiclea liquid specified for use in testingthe plastic. Specific extraction vehicles are to be designated bythe ASTM standard that references this

9、practice (see Section 7for a list of standard extraction vehicles).3.2 extract liquidthat liquid which, after extraction of thespecimen, is used in tests.3.3 specimen portionthe unit or units of plastic placedinto the extraction vehicle.3.4 blankthe extraction vehicle not containing the speci-men un

10、der test which is used for comparison with the extractliquid.4. Summary of Practice4.1 Standard-size specimens of the plastic, which mayclosely simulate the intended device depending upon the use,are immersed in defined volumes of selected liquids (extractionvehicles) for the time and temperature sp

11、ecified.4.2 Achoice is made, based on the end use, of the extractionvehicles (see Section 7) and one of the combinations of timeand temperature for the test (see Section 12).4.3 The resultant test liquids (extract liquids) are kept inglass containers until used for testing. The test liquids shall be

12、stored tightly stoppered at normal room temperature. Testliquids for biological testing are kept in sterile glass containers.Consideration should be given as to whether the extractionshould be done under aseptic conditions. The test liquids forbiological testing should be used within 24 h.5. Signifi

13、cance and Use5.1 These extraction procedures are the initial part ofseveral test procedures used in the biocompatibility screeningof plastics used in medical devices.5.2 The limitations of the results obtained from this practiceshould be recognized. The choice of extraction vehicle, dura-tion of imm

14、ersion, and temperature of the test is necessarilyarbitrary. The specification of these conditions provides a basis1This practice is under the jurisdiction ofASTM Committee F04 on Medical andSurgical Materials and Devices and is the direct responsibility of SubcommitteeF04.16 on Biocompatibility Tes

15、t Methods.Current edition approved Aug. 1, 2008. Published August 2008. Originallyapproved in 1979. Last previous edition approved in 2003 as F 619 03.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStan

16、dards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn.4Available from U.S. Pharmacopeia (USP), 12601 Twinbrook Pkwy., Rockville,MD 20852-1790, http:/www.usp.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 194

17、28-2959, United States.for standardization and serves as a guide to investigatorswishing to compare the relative resistance of various plastics toextraction vehicles.5.3 Correlation of test results with the actual performance orserviceability of materials is necessarily dependent upon thesimilarity

18、between the testing and end-use conditions (see12.1.2 and Note 4).5.4 Caution should be exercised in the understanding andintent of this practice as follows:5.4.1 No allowance or distinction is made for variables suchas end-use application and duration of use. Decisions onselection of tests to be do

19、ne should be made based on PracticeF 748.5.4.2 This practice was originally designed for use withnonporous, solid materials. Its application for other materials,such as those that are porous, or absorptive, or resorptive,should be considered with caution. Consideration should begiven to altering the

20、 specified material to liquid ratio to allowadditional liquid to fully hydrate the material and additionalliquid or other methods to fully submerge the test article.Additional procedures that fully remove the extract liquid fromthe test article, such as pressure or physically squeezing thematerial,

21、should also be considered as appropriate.Although nodefinitions are given in this practice for the following terms,such items as extraction vehicle surface tension at the specifiedextraction condition and plastic specimen physical structureshould be taken into account.5.5 Test Methods D 543, D 570,

22、and D 1239 may be usefulin providing supplemental information.6. Apparatus6.1 Autoclave, capable of maintaining a temperature of 1216 2.0C (249.8 6 3.8F) for at least 1 h and equipped with adisplay of temperature and pressure. A slow exhaust cycle isnecessary. A rack to hold the extraction container

23、s above thewater level is also necessary. Loss of fluid volume should berecorded.6.1.1 Sealed, unvented extraction vessels should not beremoved until internal temperature and pressure have reachedambient conditions and the door can be opened. It is recom-mended that the extraction vessels be left un

24、disturbed until anyrisk of boil over has passed. When the extraction vessels arecool to the touch, the lids should be sealed.6.2 Heating Equipment:6.2.1 Ovens or incubators that will maintain temperatures of37, 50, 70 6 2C (98, 122, 158 6 3F).6.2.2 Water baths capable of maintaining temperatures de-

25、scribed in 6.2.1. Those with the ability to agitate the extractionvessels are preferred.6.3 Extraction ContainersSuitable containers that protectthe extract liquid from the biological and chemical contamina-tion. They should allow expansion of the liquid, but then besealed to prevent evaporation. On

26、e suggested container is thescrew-cap culture test tube of borosilicate glass, unless a largercontainer is required for the size and shape of the material to beextracted. Screw caps, if used, shall have polytetrafluoroethyl-ene liners.6.4 Balance, accurate to 60.1 mg.6.4.1 Caution should be exercise

27、d when performing weigh-ings in glassware. Depending upon the required accuracy, therelative humidity should be the same for weighings at differenttimes.6.5 Micrometers, capable of measuring dimensions of testspecimens to 0.025 mm (0.001 in.).7. Reagents and Materials7.1 Purity of ReagentsReagent gr

28、ade, or better, chemicalsshall be used in all tests.5Other grades may be used, providedit is first ascertained that the reagent is of sufficiently highpurity to permit its use without lessening the accuracy of thedetermination.7.2 Extraction VehiclesThe following list of standardextraction vehicles

29、is intended to simulate the main constitu-ents of human body fluids. The extraction vehicles shall be:7.2.1 Sodium Chloride Injection, USP, containing by weightnot less than 0.85 % and not more than 0.95 % sodiumchloride.7.2.1.1 Other aqueous solutions shall be made with USPWFI (water for injection)

30、.7.2.2 Vegetable Oil:7.2.2.1 Sesame Oil, USP.7.2.2.2 Cottonseed Oil, USP.7.3 Other extraction vehicles as required, such as polyeth-ylene glycol, DMSO, as specified in other standards. Vehiclesshould be chosen based on biotolerance, the test protocols to beused, and the ability to extract contaminan

31、ts from the materialto be tested.NOTE 1Depending upon the material under test and the users needs,extraction vehicles other than those in 7.2 and 7.3 may be used if thereasons are justified.8. Sampling8.1 The application of this practice may be in various areas.Therefore, although some well-known qu

32、ality sampling meth-ods may be used, a statistician might be consulted to ensure astatistically valid sampling plan.8.2 Practice D 1898 may also be consulted.9. Test Specimen9.1 This practice is designed primarily for application tomaterials in the condition in which they are used. The materialshoul

33、d be exposed to all conditions and substances as during aproduction run, such as washing, packaging, and sterilization.The extraction may be done on the end-use item, specimenportions thereof, or representative molded or extruded testspecimens of the formulated compound that are preconditionedby the

34、 same processing.NOTE 2Changes to a plastic formulation, specifically additives, suchas plasticizers, stabilizers, antioxidants, pigments, and lubricants are5Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reage

35、nts notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.F 619 03 (2008)2perhaps more prone to produce differences in

36、 the extract liquid than thepolymer itself.9.2 Specimen SizeUse a specimen size as described in thefollowing sections. Suitable-size containers will allow a 20-mLextraction vehicle volume for each of the following specimensizes:9.2.1 The total surface area of a specimen (both sides) isequivalent to

37、120 cm2(18.6 in.2) when the specimen thicknessis 0.50 mm (0.020 in.) or less, or equivalent to 60 cm2(9.3 in.2)when the thickness is greater than 0.50 mm (0.020 in.).9.2.2 An alternative for specimens of intricate geometry orthose specimens with a thickness greater than 1.0 mm (0.039in.) is a specim

38、en whose weight is 0.2 g/ml.9.2.3 Specimens shall be of such dimensions as to conve-niently fit within the extraction container and their total surfacearea shall be completely covered by the extraction vehicle.9.2.3.1 To ensure full submersion of a large or bulkyspecimen, it may be necessary to cut

39、the specimen to providefor full immersion of its component pieces in the extractionvehicle. Under no circumstances shall such cutting be allowedto reduce the appropriate sample extraction ratio as determinedin 9.2.1 or 9.2.2. If the specimen cannot be cut, coupons knownto possess the same surface ch

40、aracteristics and sized to deliverthe same overall surface area as the original test specimen canalternately be utilized.9.2.4 It may be necessary to subdivide the specimen, utilizeinert and noncontaminating spacers or weights or both, orinitially agitate the extraction vehicle to ensure the entires

41、pecimen surface is contacted.9.3 Number of Specimen PortionsIn both procedures setforth in Section 12, test at least three specimen portions witheach extraction vehicle to account for variability.10. Preparation of Apparatus10.1 Clean all reusable glassware thoroughly with a chro-mic acid cleansing

42、mixture, or if necessary, with hot nitric acid,followed by prolonged rinsing with tap water and then at leasttwo rinses with distilled water.10.2 Clean cutting devices by an appropriate method, forexample, successive cleaning with suitable solvents prior touse in subdividing the sample.10.3 Clean al

43、l other equipment by thorough scrubbing witha suitable detergent and prolonged rinsing with tap water andthen at least two rinses with distilled water.10.4 Render containers and devices used for extraction andin transfer and administration of the extract liquids, sterile anddry by a suitable process

44、.NOTE 3If ethylene oxide is used as the sterilizing agent, allowadequate conditioning for complete degassing. Ethylene oxide residualsmay vary among different material formulations.11. Specimen Portion and Conditioning11.1 Biological Response ExtractionSelect and cut tosize, as in 9.2 and 9.3, at le

45、ast three specimen portions for eachextraction vehicle to be used. Aseptic precautions should beused if the extract liquid is to be used in a test requiring aseptictechnique or if the extract is to be stored for more than a fewhours before use.12. Procedure12.1 Biological Response Extraction:12.1.1

46、Prepare a set of four 20-mL portions of each extrac-tion vehicle. Place one appropriate specimen portion in each ofthree containers; the extraction vehicle in the fourth containerwill serve as a blank. Secure the cap on each container.12.1.2 Extraction ConditionsEmploy one of the follow-ing conditio

47、ns in accordance with the specified requirements.Sufficient time, in addition to that specified, should be allowedfor the liquid to reach the extraction temperature. It is recom-mended that the extraction be done at the highest temperaturethe material will withstand. If the material dissolves at 37C

48、,then the solution should be used in the tests. Mixing duringextraction is preferable. This should be done such that theextractant is mixed with the extraction vehicle, but the fluid/specimen interface is not disturbed and air bubbles should notbe formed. Mixing or agitation in the autoclave should

49、not beattempted.12.1.2.1 37 6 1C (95 6 1.8F) for 120 h. (For some testprotocols, extraction at 37C for 24 6 2hor726 2hisspecified.)12.1.2.2 50 6 2C (122 6 3.6F) for 72 h.12.1.2.3 70 6 2C (158 6 3.6F) for 24 h.12.1.2.4 121 6 2C (250 6 3.6F) for 1h.NOTE 4There may be the assumption that these conditions areequivalent to one another. The same combination of plastic and extractionvehicle, when subjected to different extraction conditions, is generallyknown to have significantly different responses when tested. The idealevaluation of a material should emplo