Standard Test Method for Determination of Cannabinoid Concentration in Dried Cannabis and Hemp Raw Materials using Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS)

SIGNIFICANCE AND USE
5.1 The analysis and reporting of cannabinoid content in cannabis and hemp is required to address human health and safety concerns, satisfy testing and labeling requirements, and meet the regulatory guidelines of various jurisdictions. This test method is useful in providing quantitative results for up to seventeen cannabinoids in dried cannabis and hemp raw material samples.
SCOPE
1.1 This test method allows for the concentration determination of the cannabinoids listed in Table 1, and shall apply to any dried raw material from a cannabis plant (Note 1, Note 2) regardless of the type of cannabis plant from which it was derived.2 For the sake of brevity, the term “cannabis” shall be used from now on to refer to any type of cannabis plant including those that can be classified as hemp. The procedure includes sub-sampling a ground, homogeneous sample, extraction with methanol:water (80:20, v:v),3,4 dilution in methanol and analysis by liquid chromatography tandem mass spectrometry (LC-MS/MS). The method allows for a wide-range of sample concentrations to be determined by using a 1000-fold calibration range and the option to perform multiple levels of sample dilution. The calibration curve is prepared in methanol over a range of 10 ng/mL to 10 000 ng/mL for all seventeen cannabinoids, or a subset of cannabinoids if desired, while the sample extracts are diluted in methanol into the calibration range.3,4,5 For example, a 1/500 dilution of sample extracts allows concentration determination over a range of 0.5 mg/g to 500 mg/g in cannabis. The method was validated with quality control samples prepared in methanol, a candidate certified reference material (CRM), and repeat extraction and analysis of cannabinoid samples.3  
Note 1: For this test method, dried raw material from a cannabis plant includes one or more of inflorescence, leaves, or stems.
Note 2: Certain jurisdictions or regulations may require specific parts of the plant to be included or excluded for analysis and those regulations will take precedence for the selection of plant parts.  
1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 List of Measurable Analytes—See Table 1.  
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

Status
Published
Publication Date
28-Feb-2023
Technical Committee
Drafting Committee
Current Stage
Ref Project

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ASTM D8375-23 - Standard Test Method for Determination of Cannabinoid Concentration in Dried Cannabis and Hemp Raw Materials using Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS)
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REDLINE ASTM D8375-23 - Standard Test Method for Determination of Cannabinoid Concentration in Dried Cannabis and Hemp Raw Materials using Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS)
English language
17 pages
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Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D8375 − 23
Standard Test Method for
Determination of Cannabinoid Concentration in Dried
Cannabis and Hemp Raw Materials using Liquid
1
Chromatography Tandem Mass Spectrometry (LC-MS/MS)
This standard is issued under the fixed designation D8375; 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.
NOTE 1—For this test method, dried raw material from a cannabis plant
1. Scope
includes one or more of inflorescence, leaves, or stems.
1.1 This test method allows for the concentration determi-
NOTE 2—Certain jurisdictions or regulations may require specific parts
nation of the cannabinoids listed in Table 1, and shall apply to of the plant to be included or excluded for analysis and those regulations
will take precedence for the selection of plant parts.
any dried raw material from a cannabis plant (Note 1, Note 2)
regardless of the type of cannabis plant from which it was
1.2 Units—The values stated in SI units are to be regarded
2
derived. For the sake of brevity, the term “cannabis” shall be
as standard. No other units of measurement are included in this
used from now on to refer to any type of cannabis plant
standard.
including those that can be classified as hemp. The procedure
1.3 List of Measurable Analytes—See Table 1.
includes sub-sampling a ground, homogeneous sample, extrac-
3,4
1.4 This standard does not purport to address all of the
tion with methanol:water (80:20, v:v), dilution in methanol
safety concerns, if any, associated with its use. It is the
and analysis by liquid chromatography tandem mass spectrom-
responsibility of the user of this standard to establish appro-
etry (LC-MS/MS). The method allows for a wide-range of
priate safety, health, and environmental practices and deter-
sample concentrations to be determined by using a 1000-fold
mine the applicability of regulatory limitations prior to use.
calibration range and the option to perform multiple levels of
1.5 This international standard was developed in accor-
sample dilution. The calibration curve is prepared in methanol
dance with internationally recognized principles on standard-
over a range of 10 ng ⁄mL to 10 000 ng/mL for all seventeen
ization established in the Decision on Principles for the
cannabinoids, or a subset of cannabinoids if desired, while the
Development of International Standards, Guides and Recom-
sample extracts are diluted in methanol into the calibration
3,4,5
mendations issued by the World Trade Organization Technical
range. For example, a 1/500 dilution of sample extracts
Barriers to Trade (TBT) Committee.
allows concentration determination over a range of 0.5 mg ⁄g to
500 mg ⁄g in cannabis. The method was validated with quality
2. Referenced Documents
control samples prepared in methanol, a candidate certified
6
2.1 ASTM Standards:
reference material (CRM), and repeat extraction and analysis
3
D1193 Specification for Reagent Water
of cannabinoid samples.
D8245 Guide for Disposal of Resin-Containing Cannabis
Raw Materials and Downstream Products
1 D8270 Terminology Relating to Cannabis
This test method is under the jurisdiction of ASTM Committee D37 on
D8282 Practice for Laboratory Test Method Validation and
Cannabis and is the direct responsibility of Subcommittee D37.03 on Laboratory.
Current edition approved March 1, 2023. Published March 2023. Originally
Method Development
approved in 2022. Last previous edition approved in 2022 as D8375 – 22. DOI:
E203 Test Method for Water Using Volumetric Karl Fischer
10.1520/D8375-23.
2 Titration
Health Canada, Guidance Document: Good production practices guide for
cannabis Testing for Phytocannabinoids.
3
McRae, G. and Melanson, J. E., Quantitative determination and validation of 17
3. Terminology
cannabinoids in cannabis and hemp using liquid chromatography-tandem mass
3.1 Definitions—For general terms related to cannabis, refer
spectrometry, Anal Bioanal Chem, Vol 412, No. 27, 2020, pp. 7381–7393,
doi:10.1007/s00216-020-02862-8.
to Terminology D8270.
4
Mudge, E. M., Murch, S. J., Brown, P. N., Leaner and greener analysis of
3.2 Definitions of Terms Specific to This Standard:
cannabinoids, Anal Bioanal Chem, Vol 409, No. 12, 2017, pp. 3153–3163, doi:
10.1007/s00216-017-0256-3.
5
Vaclavik, L., Benes, F., Fenclova, M., Hricko, J., Krmela, A., Svobodova, V., et
6
al. Quantitation of cannabinoids in cannabis dried plant materials, concentrates, and For referenced ASTM standards, visit the ASTM website, www.as
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D8375 − 22 D8375 − 23
Standard Test Method for
Determination of Cannabinoid Concentration in Dried
Cannabis and Hemp Raw Materials using Liquid
1
Chromatography Tandem Mass Spectrometry (LC-MS/MS)
This standard is issued under the fixed designation D8375; 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
1.1 This test method allows for the concentration determination of the cannabinoids listed in Table 1, and shall apply to any dried
2
raw material from a cannabis plant (Note 1, Note 2) regardless of the type of cannabis plant from which it was derived. For the
sake of brevity, the term “cannabis” shall be used from now on to refer to any type of cannabis plant including those that can be
classified as hemp. The procedure includes sub-sampling a ground, homogeneous sample, extraction with methanol:water (80:20,
3,4
v:v), dilution in methanol and analysis by liquid chromatography tandem mass spectrometry (LC-MS/MS). The method allows
for a wide-range of sample concentrations to be determined by using a 1000-fold calibration range and the option to perform
multiple levels of sample dilution. The calibration curve is prepared in methanol over a range of 10 ng ⁄mL to 10 000 ng/mL for
all seventeen cannabinoids, or a subset of cannabinoids if desired, while the sample extracts are diluted in methanol into the
3,4,5
calibration range. For example, a 1/500 dilution of sample extracts allows concentration determination over a range of 0.5 mg ⁄g
to 500 mg ⁄g in cannabis. The method was validated with quality control samples prepared in methanol, a candidate certified
3
reference material (CRM), and repeat extraction and analysis of cannabinoid samples.
NOTE 1—For this test method, dried raw material from a cannabis plant includes one or more of inflorescence, leaves, or stems.
NOTE 2—Certain jurisdictions or regulations may require specific parts of the plant to be included or excluded for analysis and those regulations will take
precedence for the selection of plant parts.
1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this
standard.
1.3 List of Measurable Analytes—See Table 1.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of
regulatory limitations prior to use.
1
This test method is under the jurisdiction of ASTM Committee D37 on Cannabis and is the direct responsibility of Subcommittee D37.03 on Laboratory.
Current edition approved Aug. 1, 2022March 1, 2023. Published September 2022March 2023. Originally approved in 2022. Last previous edition approved in 2022 as
D8375 – 22. DOI: 10.1520/D8375-22.10.1520/D8375-23.
2
Health Canada, Guidance Document: Good production practices guide for cannabis Testing for Phytocannabinoids.
3
McRae, G. and Melanson, J. E., Quantitative determination and validation of 17 cannabinoids in cannabis and hemp using liquid chromatography-tandem mass
spectrometry, Anal Bioanal Chem, Vol 412, No. 27, 2020, pp. 7381–7393, doi:10.1007/s00216-020-02862-8.
4
Mudge, E. M., Murch, S. J., Brown, P. N., Leaner and greener analysis of cannabinoids, Anal Bioanal Chem, Vol 409, No. 12, 2017, pp. 3153–3163, doi:
10.1007/s00216-017-0256-3.
5
Vaclavik, L., Benes, F., Fenclova, M., Hricko, J., Krmela, A., Svobodova, V., et al. Quantitation of cannabinoids in cannabis dried plant materials, concentrates, and oils
using liquid chromatography-diode array detection technique with optional mass spectrometric detection: single-laboratory validation study, first action 2018.11, J AOAC Int.
Vol 102, No. 6, 2019, pp. 1822–33
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D8375 − 23
TABLE 1 List of Measurable Analytes
Analyte Name Analyte Abbreviation
9
delta-9-tetrahydrocannabinol Δ -THC
9
delta-9-tetrahydrocannabinolic acid Δ -THCA
cannabidiol CBD
cannabidiolic acid CBDA
cannabigerol CBG
cannabigerolic acid CBGA
cannabigerovarin CBGV
cannabigerovarinic acid CBGVA
cannabinol CBN
cannabinolic acid CBNA
canna
...

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