ASTM_D_8375_-_22.pdf

Designation:D837522Standard Test Method forDetermination of Cannabinoid Concentration in DriedCannabis and Hemp Raw Materials using LiquidChromatography Tandem Mass Spectrometry(LC-MS/MS)1This standard is issued under the fixed designation D8375;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 allows for the concentration determi-nation of the cannabinoids listed in Table 1,and shall apply toany dried raw material from a cannabis plant(Note 1,Note 2)regardless of the type of cannabis plant from which it wasderived.2For the sake of brevity,the term“cannabis”shall beused from now on to refer to any type of cannabis plantincluding those that can be classified as hemp.The procedureincludes sub-sampling a ground,homogeneous sample,extrac-tion with methanol:water(80:20,v:v),3,4dilution in methanoland analysis by liquid chromatography tandem mass spectrom-etry(LC-MS/MS).The method allows for a wide-range ofsample concentrations to be determined by using a 1000-foldcalibration range and the option to perform multiple levels ofsample dilution.The calibration curve is prepared in methanolover a range of 10 ng mL to 10 000 ng/mL for all seventeencannabinoids,or a subset of cannabinoids if desired,while thesample extracts are diluted in methanol into the calibrationrange.3,4,5For example,a 1/500 dilution of sample extractsallows concentration determination over a range of 0.5 mg g to500 mgg in cannabis.The method was validated with qualitycontrol samples prepared in methanol,a candidate certifiedreference material(CRM),and repeat analysis of cannabinoidsamples.3NOTE1For this test method,dried raw material from a cannabis plantincludes one or more of inflorescence,leaves,or stems.NOTE2Certain jurisdictions or regulations may require specific partsof the plant to be included or excluded for analysis and those regulationswill take precedence for the selection of plant parts.1.2 UnitsThe values stated in SI units are to be regardedas standard.No other units of measurement are included in thisstandard.1.3 List of Measurable AnalytesSee Table 1.1.4 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:6D1193 Specification for Reagent WaterD8245 Guide for Disposal of Resin-Containing CannabisRaw Materials and Downstream ProductsD8270 Terminology Relating to CannabisD8282 Practice for Laboratory Test Method Validation andMethod DevelopmentE203 Test Method for Water Using Volumetric Karl FischerTitration3.Terminology3.1 DefinitionsFor general terms related to cannabis,referto Terminology D8270.3.2 Definitions of Terms Specific to This Standard:1This test method is under the jurisdiction of ASTM Committee D37 onCannabis and is the direct responsibility of Subcommittee D37.03 on Laboratory.Current edition approved Aug.1,2022.Published September 2022.DOI:10.1520/D8375-22.2Health Canada,Guidance Document:Good production practices guide forcannabis Testing for Phytocannabinoids.3McRae,G.and Melanson,J.E.,Quantitative determination and validation of 17cannabinoids in cannabis and hemp using liquid chromatography-tandem massspectrometry,Anal Bioanal Chem,Vol 412,No.27,2020,pp.73817393,doi:10.1007/s00216-020-02862-8.4Mudge,E.M.,Murch,S.J.,Brown,P.N.,Leaner and greener analysis ofcannabinoids,Anal Bioanal Chem,Vol 409,No.12,2017,pp.31533163,doi:10.1007/s00216-017-0256-3.5Vaclavik,L.,Benes,F.,Fenclova,M.,Hricko,J.,Krmela,A.,Svobodova,V.,etal.Quantitation of cannabinoids in cannabis dried plant materials,concentrates,andoils using liquid chromatography-diode array detection technique with optionalmass spectrometric detection:single-laboratory validation study,first action2018.11,J AOAC Int.Vol 102,No.6,2019,pp.1822336For 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.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 th