ASTM_F_2260_-_18.pdf

Designation:F226018Standard Test Method forDetermining Degree of Deacetylation in Chitosan Salts byProton Nuclear Magnetic Resonance(1H NMR)Spectroscopy1This standard is issued under the fixed designation F2260;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last revision.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 This test method covers the determination of the degreeof deacetylation in chitosan and chitosan salts intended for usein biomedical and pharmaceutical applications as well as inTissue Engineered Medical Products(TEMPs)by high-resolution proton NMR(1H NMR).A guide for the character-ization of chitosan salts has been published as Guide F2103.1.2 The test method is applicable for determining the degreeof deacetylation(%DDA)of chitosan chloride and chitosanglutamate salts and is valid for%DDA values from 50 up toand including 99.It is simple,rapid,and suitable for routineuse.Knowledge of the degree of deacetylation is important foran understanding of the functionality of chitosan salts in TEMPformulations and applications.This test method will assist endusers in choosing the correct chitosan for their particularapplication.Chitosan salts may have utility in drug deliveryapplications,as scaffold or matrix material,and in cell andtissue encapsulation applications.1.3 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.4 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,health,and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.5 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade(TBT)Committee.2.Referenced Documents2.1 ASTM Standards:2F386 Test Method for Thickness of Resilient Flooring Ma-terials Having Flat SurfacesF2103 Guide for Characterization and Testing of ChitosanSalts as Starting Materials Intended for Use in Biomedicaland Tissue-Engineered Medical Product Applications2.2 United States Pharmacopeia Document:USP 35-NF30 Nuclear Magnetic Resonance32.3 European Pharmacopoeia Document:European Pharmacopoeia Monograph 2008:1774 ChitosanChloride43.Terminology3.1 Definitions:3.1.1 chitosan,na linear polysaccharide consisting of(14)linked 2-acetamido-2-deoxy-D-glucopyranose(Glc-NAc)and 2-amino-2-deoxy-D-glucopyranose(GlcN).Chito-san is a polysaccharide derived by N-deacetylation of chitin.3.1.2 degradation,nchange in the chemical structure,physical properties,or appearance of a material.Degradationof polysaccharides occurs via cleavage of the glycosidic bonds.It is important to note that degradation is not synonymous withdecomposition.Degradation is often used as a synonym fordepolymerization when referring to polymers.3.1.3 degree of deacetylation,nthe fraction or percentageof glucosamine units(GlcN:deacetylated monomers)in achitosan polymer molecule.3.1.4 depolymerization,nreduction in the length of apolymer chain to form shorter polymeric units.1This test method is under the jurisdiction ofASTM Committee F04 on Medicaland Surgical Materials and Devices and is the direct responsibility of SubcommitteeF04.42 on Biomaterials and Biomolecules for TEMPs.Current edition approved June 1,2018.Published August 2018.Originallyapproved in 2003.Last previous edition approved in 2012 as F2260 03(2012)1.DOI:10.1520/F2260-18.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMStandards volume information,refer to the standards Document Summary page onthe ASTM website.3Available from U.S.Pharmacopeia(USP),12601 Twinbrook Pkwy.,Rockville,MD 20852-1790,http:/www.usp.org.4Available from European Directorate for the Quality of Medicines(EDQM),Publications and Services,European Pharmacopoeia,BP 907,F-67029 Strasbourg,France.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade(TBT)Committee.1 3.1.5 water soluble chitosan salt,nan ionic compoundbetween chitosan molecule(cation)and a negatively chargedanion(e.g.glutamate,acetate,lactate,chloride)that is solublein water.4.Significance and Use4.1 T