ASTM F1581-08(2012)
(Specification)Standard Specification for Composition of Anorganic Bone for Surgical Implants
Standard Specification for Composition of Anorganic Bone for Surgical Implants
ABSTRACT
This specification covers material requirements for chemical composition of anorganic xenogeneic or allogeneic bone (apatite) intended for surgical implants. This specification specifically excludes synthetic hydroxylapatite, hydroxylapatite coatings, ceramic glasses, tribasic calcium phosphate, whitlockite, and alpha- and betatricalcium phosphate. Elemental analysis for calcium and phosphorus shall be consistent with the expected composition of the source of the biologically-derived bone mineral. X-ray diffraction analysis of the material shall be consistent with that specified for hydroxyapatite and calcium phosphate carbonate (carbonated apatite). The crystal size of the anorganic bone shall be determined from the X-ray diffraction data using the well-known Scherrer formula. The concentration of trace elements in the anorganic bone shall conform to the prescribed limit for: arsenic, cadmium, mercury, lead, and heavy metals (as lead), which may be determined by the following methods: inductively coupled plasma-mass spectroscopy (ICP-MS) or USP method and graphite furnace atomic absorption spectrophotometry. Organic content shall be measured either as total carbon or nitrogen or total protein by amino acid analyses. The carbonate content of the anorganic bone shall be determined. Functional groups shall be identified by infrared analysis. Requirements for biocompatibility and sterilization are given as well.
SCOPE
1.1 This specification covers material requirements for anorganic xenogeneic or allogeneic bone (apatite) intended for surgical implants. For a material to be called anorganic or deorganified bone, it must conform to this specification (see Appendix X1).
1.2 The biological response to apatite in soft tissue and bone has been characterized by a history of clinical use and by laboratory studies (1, 2, 3).2 Xenogeneic bone, with organic components present, has been shown to be antigenic in the human host (4) whereas the same material that has been completely deorganified has been shown to elicit no inflammatory or foreign body reactions in human clinical use (5, 6, 7).
1.3 This specification specifically excludes synthetic hydroxylapatite, hydroxylapatite coatings, ceramic glasses, tribasic calcium phosphate, whitlockite, and alpha- and beta-tricalcium phosphate.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 Warning—Mercury has been designated by EPA and many state agencies as a hazardous material that can cause central nervous system, kidney, and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Caution should be taken when handling mercury and mercury-containing products. See the applicable product Material Safety Data Sheet (MSDS) for details and EPA’s website (http://www.epa.gov/mercury/faq.htm) for additional information. Users should be aware that selling mercury or mercury-containing products, or both, in your state may be prohibited by state law.
1.6 This standard does not purport to address all of the safety concerns, such as health concerns due to the presence of transmissible disease, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. (See Appendix X2).
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Standards Content (Sample)
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Designation:F1581 −08(Reapproved 2012)
Standard Specification for
Composition of Anorganic Bone for Surgical Implants
This standard is issued under the fixed designation F1581; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope transmissible disease, associated with its use. It is the respon-
sibility of the user of this standard to establish appropriate
1.1 This specification covers material requirements for an-
safety and health practices and determine the applicability of
organic xenogeneic or allogeneic bone (apatite) intended for
regulatory limitations prior to use. (See Appendix X2).
surgical implants. For a material to be called anorganic or
deorganified bone, it must conform to this specification (see
2. Referenced Documents
Appendix X1).
2.1 ASTM Standards:
1.2 Thebiologicalresponsetoapatiteinsofttissueandbone
D513 Test Methods forTotal and Dissolved Carbon Dioxide
has been characterized by a history of clinical use and by
in Water
laboratory studies (1, 2, 3). Xenogeneic bone, with organic
D1688 Test Methods for Copper in Water
components present, has been shown to be antigenic in the
D2972 Test Methods for Arsenic in Water
human host (4) whereas the same material that has been
D3557 Test Methods for Cadmium in Water
completely deorganified has been shown to elicit no inflam-
D3559 Test Methods for Lead in Water
matory or foreign body reactions in human clinical use (5, 6,
D3919 Practice for Measuring Trace Elements in Water by
7).
Graphite Furnace Atomic Absorption Spectrophotometry
1.3 This specification specifically excludes synthetic D4129 Test Method for Total and Organic Carbon in Water
hydroxylapatite, hydroxylapatite coatings, ceramic glasses,
by High Temperature Oxidation and by Coulometric
tribasic calcium phosphate, whitlockite, and alpha- and beta- Detection
tricalcium phosphate.
E1184 Practice for Determination of Elements by Graphite
Furnace Atomic Absorption Spectrometry
1.4 The values stated in SI units are to be regarded as
F748 PracticeforSelectingGenericBiologicalTestMethods
standard. No other units of measurement are included in this
for Materials and Devices
standard.
F1185 Specification for Composition of Hydroxylapatite for
1.5 Warning—Mercury has been designated by EPA and
Surgical Implants
many state agencies as a hazardous material that can cause
2.2 Code of Federal Regulations:
central nervous system, kidney, and liver damage. Mercury, or
Title 21, Part 820
its vapor, may be hazardous to health and corrosive to
2.3 National Formulary:
materials.Cautionshouldbetakenwhenhandlingmercuryand
Tribasic Calcium Phosphate
mercury-containing products. See the applicable product Ma-
2.4 United States Pharmocopeia:
terial Safety Data Sheet (MSDS) for details and EPA’s website
Identification Tests for Calcium and Phosphate <191>
(http://www.epa.gov/mercury/faq.htm) for additional informa-
Lead < 251>
tion. Users should be aware that selling mercury or mercury-
Mercury <261>
containingproducts,orboth,inyourstatemaybeprohibitedby
state law.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
1.6 This standard does not purport to address all of the
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
safety concerns, such as health concerns due to the presence of
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
This specification is under the jurisdiction of ASTM Committee F04 on 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
Medical and Surgical Materials and Devices and is under the direct responsibility of www.access.gpo.gov.
Subcommittee F04.13Ceramic Materials. National Formulary 25. Available from U.S. Pharmacopeia (USP), 12601
Current edition approved Oct. 1, 2012. Published October 2012. Originally Twinbrook Pkwy., Rockville, MD 20852-1790, http://www.usp.org. Succeeding
ε1
approved in 1995. Last previous edition approved in 2008 as F1581 – 08 . DOI: USP editions may alternatively be referenced.
10.1520/F1581-08R12. United States Pharmacopeia 30. Available from U.S. Pharmacopeia (USP),
The boldface numbers in parentheses refer to the list of references at the end of 12601TwinbrookPkwy.,Rockville,MD20852-1790,http://www.usp.org.Succeed-
this specification. ing USP editions may alternatively be referenced.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F1581−08 (2012)
Cadmium <461> atomic absorption spectrophotometry may also be used for
Arsenic <211> analysis of trace elements using for arsenic (Test Methods
Heavy Metals <231> Method 1
D2972), copper (Test Methods D1688), cadmium (Test Meth-
Nitrogen Determination <4617>
ods D3557), lead (Test Methods D3559) with 1 g anorganic
2.5 U.S. Geological Survey Method:
bone/100mLwater samples. General guides for the application
Cadmium
of the graphite furnace are given in Practices D3919 and
E1184.
3. Terminology
4.5 The maximum allowable limit of all heavy metals
3.1 Definitions:
determined as lead shall be 50 ppm as described in 2.4 or
3.1.1 allogeneic, adj—derived from different individuals of
equivalent. Sample preparation shall be identical to that for
the same species.
tribasic calcium phosphate as specified in the National Formu-
3.1.2 anorganic, adj—denoting tissue (for example, bone)
lary (see 2.3), except that approximately1gof material shall
from which the organic material has been totally removed.
be dissolved in approximately 30 mL of 5 % HCl and boiled.
Also referred to as deorganified, deproteinized or deprotein-
ated.
4.6 It is recommended that all minor constituents such as
metals or oxides not detected as lead and present in concen-
3.1.3 apatite, n—the mineral substance having the molecu-
trations equal to or greater than 0.1 % be identified and
lar formula Ca (X) (PO ) where X = OH (hydroxyapatite or
10 2 4 6
quantified.
hydroxylapatite), CO (carbonated apatite), F (fluorine), or Cl
(chlorine) (8).
4.7 Organic content shall be measured either as total carbon
3.1.4 xenogeneic, adj—derived from individuals of a
or nitrogen (see Note 1) or total protein by amino acid
different, specified species. For example, bovine bone, when
analyses(13). For all methods, a synthetic hydroxylapatite
used as an implant material in humans, is xenogeneic.
control that conforms to Specification F1185 or an established
National Institute of Standards and Technology (NIST) stan-
4. Chemical Requirements
dard shall be used. The maximum allowable limit of either
4.1 Elemental analysis for calcium and phosphorus shall be
nitrogen, carbon, or protein shall be within two standard
consistent with the expected composition of the source of the
deviations of the mean value established for the control.
biologically-derived bone mineral (9).
NOTE1—TheKjeldahlprocessfornitrogendetermination(USP<461>)
4.2 An X-ray diffraction analysis of the material shall be
is set forth by the Association of Official Analytical Chemists (14) as an
consistent with PDF card #9-432 for hydroxyapatite (10) or
appropriate measure of proteins. Alternatively, organic material (carbon)
PDF card #35-180 for calcium phosphate carbonate (carbon-
can be measured by the coulometric method (Test Method D4129).
Subtract from this value the carbonate content, which can be determined
ated apatite). Analysis of relative peak intensities shall be
by Test Methods D513.
consistent with published data.
4.8 The carbonate content of the anorganic bone shall be
4.3 The crystal size of the anorganic bone shall be deter-
determined. Carbonate content is typically 5 to6%in bone
mined from the X-ray diffraction data using the well-known
Scherrer formula (11). mineral prior to removal of the organic phase. Residual
carbonate content remaining after processing is one means of
4.4 The concentration of trace elements in the anorganic
distinguishingbetweenthevariousprocessingmethodsutilized
bone shall be limited as follows:
to process bone powder into anorganic bone. Carbonate con-
Element ppm, max
tent is linked to dissolution and resorbability characteristics of
arsenic 3
cadmium 5 anorganic bone products and should be kept within1%of
mercury 5
previous lots in order to assure consistent performance. Low
lead 30
carbonate content anorganic bone mineral (2 % or less) is
total heavy metals (as lead) 50
barely soluble in dilute acids as compared to anorganic bone
For referee purposes, use either inductively coupled plasma/
containing 5 to 6 % carbonate.
mass spectroscopy (ICP/MS) (12) or th
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