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 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
Historical
Publication Date
31-Jul-2022
Technical Committee
Drafting Committee
Current Stage
Ref Project

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ASTM D8375-22 - 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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Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D8375 − 22
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.
includes one or more of inflorescence, leaves, or stems.
1. Scope
NOTE 2—Certain jurisdictions or regulations may require specific parts
1.1 This test method allows for the concentration determi-
of the plant to be included or excluded for analysis and those regulations
nation of the cannabinoids listed in Table 1, and shall apply to
will take precedence for the selection of plant parts.
any dried raw material from a cannabis plant (Note 1, Note 2)
1.2 Units—The values stated in SI units are to be regarded
regardless of the type of cannabis plant from which it was
as standard. No other units of measurement are included in this
2
derived. For the sake of brevity, the term “cannabis” shall be
standard.
used from now on to refer to any type of cannabis plant
1.3 List of Measurable Analytes—See Table 1.
including those that can be classified as hemp. The procedure
1.4 This standard does not purport to address all of the
includes sub-sampling a ground, homogeneous sample, extrac-
3,4
safety concerns, if any, associated with its use. It is the
tion with methanol:water (80:20, v:v), dilution in methanol
responsibility of the user of this standard to establish appro-
and analysis by liquid chromatography tandem mass spectrom-
priate safety, health, and environmental practices and deter-
etry (LC-MS/MS). The method allows for a wide-range of
mine the applicability of regulatory limitations prior to use.
sample concentrations to be determined by using a 1000-fold
1.5 This international standard was developed in accor-
calibration range and the option to perform multiple levels of
dance with internationally recognized principles on standard-
sample dilution. The calibration curve is prepared in methanol
ization established in the Decision on Principles for the
over a range of 10 ng ⁄mL to 10 000 ng/mL for all seventeen
Development of International Standards, Guides and Recom-
cannabinoids, or a subset of cannabinoids if desired, while the
mendations issued by the World Trade Organization Technical
sample extracts are diluted in methanol into the calibration
3,4,5
Barriers to Trade (TBT) Committee.
range. For example, a 1/500 dilution of sample extracts
allows concentration determination over a range of 0.5 mg ⁄g to
2. Referenced Documents
500 mg ⁄g in cannabis. The method was validated with quality
6
control samples prepared in methanol, a candidate certified
2.1 ASTM Standards:
reference material (CRM), and repeat analysis of cannabinoid
D1193 Specification for Reagent Water
3
samples.
D8245 Guide for Disposal of Resin-Containing Cannabis
NOTE 1—For this test method, dried raw material from a cannabis plant
Raw Materials and Downstream Products
D8270 Terminology Relating to Cannabis
D8282 Practice for Laboratory Test Method Validation and
1
This test method is under the jurisdiction of ASTM Committee D37 on
Method Development
Cannabis and is the direct responsibility of Subcommittee D37.03 on Laboratory.
E203 Test Method for Water Using Volumetric Karl Fischer
Current edition approved Aug. 1, 2022. Published September 2022. DOI:
Titration
10.1520/D8375-22.
2
Health Canada, Guidance Document: Good production practices guide for
cannabis Testing for Phytocannabinoids.
3. Terminology
3
McRae, G. and Melanson, J. E., Quantitative determination and validation of 17
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,
to Terminology D8270.
doi:10.1007/s00216-020-02862-8.
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.astm.org, or
oils using liquid chromatography-diode array detection technique with optional contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
mass spectrometric detection: single-laboratory validation study, first action
...

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