ASTM D8399-23
(Test Method)Standard Test Method for Multi-residue Analysis of Pesticides in Dried Cannabis and Hemp Raw Materials Using Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS)
Standard Test Method for Multi-residue Analysis of Pesticides 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 pesticide content in all forms of cannabis raw material that is grown or processed or both, with the intent of ingestion or consumption, is required to address health and safety concerns, satisfy testing and labeling requirements, and meet the regulatory guidelines of various jurisdictions where cannabis has been legalized for ingestion or consumption for medicinal or recreational purposes, or both. This test method is useful in providing quantitative results for the analytes listed in Table 1, which is a subset of the pesticide testing requirements found in regulatory documents for cannabis, not limited to and including Canada, many U.S. states where legalization has occurred, and the European Pharmacopeia (1-4). This test method may be appropriate for additional pesticide and growth regulator analytes, which may be added to those of Table 1 provided validation is performed in accordance with Practice D8282. Analytes may be removed from Table 1 without additional validation.
SCOPE
1.1 This test method allows for the concentration determination of the pesticides 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 (1, 2).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 which can be classified as hemp. The procedure includes sub-sampling a ground, homogenous sample, liquid-solid extraction with acetonitrile:acetic acid (100:1, v:v), solid phase extraction with C18 SPE media, dilution in 3 mM ammonium formate in water with 0.1 % formic acid and 3 mM ammonium formate in methanol with 0.02 % formic acid in a 20:80 ratio (v:v) and analysis by LC-MS/MS. This procedure encompasses the entire process from sample preparation to analyte quantitation encompassing a range of 0.005 µg/g to 0.500 µg/g.
Pyrethrins = Pyrethrin I and II
Spinetoram = Spinetoram J and L
Spinosad = Spinosyn A and D
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 Table 1 lists the analytes measured by this test method.
1.4 No recommendations found within this test method shall preclude observance of federal, state, or local regulations, which may be more restrictive or have different requirements.
1.5 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.
1.6 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
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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: D8399 − 23
Standard Test Method for
Multi-residue Analysis of Pesticides in Dried Cannabis and
Hemp Raw Materials Using Liquid Chromatography-Tandem
1
Mass Spectrometry (LC-MS/MS)
This standard is issued under the fixed designation D8399; 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 1.6 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1.1 This test method allows for the concentration determi-
ization established in the Decision on Principles for the
nation of the pesticides listed in Table 1 and shall apply to any
Development of International Standards, Guides and Recom-
dried raw material from a cannabis plant (Note 1, Note 2)
mendations issued by the World Trade Organization Technical
regardless of the type of cannabis plant from which it was
2 Barriers to Trade (TBT) Committee.
derived (1, 2). For the sake of brevity, the term “cannabis”
shall be used from now on to refer to any type of cannabis plant
2. Referenced Documents
including those which can be classified as hemp. The proce-
3
2.1 ASTM Standards:
dure includes sub-sampling a ground, homogenous sample,
liquid-solid extraction with acetonitrile:acetic acid (100:1, v:v), D1193 Specification for Reagent Water
D8245 Guide for Disposal of Resin-Containing Cannabis
solid phase extraction with C18 SPE media, dilution in 3 mM
ammonium formate in water with 0.1 % formic acid and 3 mM Raw Materials and Downstream Products
D8270 Terminology Relating to Cannabis
ammonium formate in methanol with 0.02 % formic acid in a
20:80 ratio (v:v) and analysis by LC-MS/MS. This procedure D8282 Practice for Laboratory Test Method Validation and
Method Development
encompasses the entire process from sample preparation to
analyte quantitation encompassing a range of 0.005 μg ⁄g to
3. Terminology
0.500 μg ⁄g.
NOTE 1—For this test method, dried raw material from a cannabis plant
3.1 Definitions—For general terms related to cannabis, refer
includes one or more of inflorescence, leaves, or stems.
to Terminology D8270.
NOTE 2—Certain jurisdictions or regulations may require specific parts
of the plant to be included or excluded for analysis and those regulations
3.2 Definitions of Terms Specific to This Standard:
will take precedence for the selection of plant parts.
3.2.1 blank, n—a cannabis-only sample prepared from the
1.2 Units—The values stated in SI units are to be regarded
same homogenous cannabis blend used to prepare the calibra-
as standard. No other units of measurement are included in this
tion curve, without the addition of internal standard working
standard.
solution (ISWS).
1.3 Table 1 lists the analytes measured by this test method.
3.2.2 blank-0, n—a cannabis-only sample prepared from the
same homogenous cannabis blend used to prepare the calibra-
1.4 No recommendations found within this test method shall
tion curve, with the addition of ISWS.
preclude observance of federal, state, or local regulations,
which may be more restrictive or have different requirements. 3.2.3 blank-S, n—a solvent blank prepared from only the
mobile phases, without cannabis or analytes.
1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 3.2.4 growth regulator, n—a class of chemical compounds
used to modulate the growth and development of a crop.
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
3.2.5 pesticide, n—a product or substance used as a means
mine the applicability of regulatory limitations prior to use.
to reduce or mitigate pests such as insects, fungus, bacteria,
and weeds.
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 March 1, 2023. Published March 2023. Originally
3
approved in 2022. Last previous edition approved in 2022 as D8399 – 22. DOI: For referenced ASTM standards, visit the ASTM website, www.astm.org, or
10.1520/D8399-23. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
2
The boldface numbers in parentheses refer to the list of references at the end of Standards volume information, refer to the standard’s Document Summary page on
this standard. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C70
...
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: D8399 − 22 D8399 − 23
Standard Test Method for
Multi-residue Analysis of Pesticides in Dried Cannabis and
Hemp Raw Materials Using Liquid Chromatography-Tandem
1
Mass Spectrometry (LC-MS/MS)
This standard is issued under the fixed designation D8399; 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 pesticides listed in Table 1 and shall apply to any dried raw
2
material from a cannabis plant (Note 1, Note 2) regardless of the type of cannabis plant from which it was derived (1, 2). For For
the sake of brevity, the term “cannabis” shall be used from now on to refer to any type of cannabis plant including those which
can be classified as hemp. The procedure includes sub-sampling a ground, homogenous sample, liquid-solid extraction with
acetonitrile:acetic acid (100:1, v:v), solid phase extraction with C18 SPE media, dilution in 3 mM ammonium formate in water
with 0.1%0.1 % formic acid and 3 mM ammonium formate in methanol with 0.02%0.02 % formic acid in a 20:80 ratio (v:v) and
analysis by LC-MS/MS. This procedure encompasses the entire process from sample preparation to analyte quantitation
encompassing a range of 0.005 μg ⁄g to 0.500 μg ⁄g.
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 Table 1 lists the analytes measured by this test method.
1.4 No recommendations found within this test method shall preclude observance of federal, state, or local regulations, which may
be more restrictive or have different requirements.
1.5 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.
1.6 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.
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 July 1, 2022March 1, 2023. Published August 2022March 2023. Originally approved in 2022. Last previous edition approved in 2022 as
D8399 – 22. DOI: 10.1520/D8399-22.10.1520/D8399-23.
2
The boldface numbers in parentheses refer to the list of references at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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D8399 − 23
TABLE 1 List of Measureable Analytes
Abamectin Daminozide Imidacloprid Pyraclostrobin
Acephate Deltamethrin Iprodione Pyrethrins
Acequinocyl Diazinon Kresoxim Methyl Pyridaben
Acetamiprid Dichlorvos Malathion Resmethrin
Aldicarb Dimethoate Metalaxyl Spinetoram
Allethrin Dimethomorph Methiocarb Spinosad
Azadirachtin Dinotefuran Methomyl Spirodiclofen
Azoxystrobin Dodemorph Methoprene Spiromesifen
Benzovindiflupyr Ethoprophos Mevinphos Spirotetramat
Bifenazate Etofenprox Myclobutanil Spiroxamine
Bifenthrin Etoxazole Naled Tebuconazole
Boscalid Fenoxycarb Novaluron Tebufenozide
Buprofezin Fenpyroximate Oxamyl Teflubenzuron
Carbaryl Fensulfothion Paclobutrazol Tetrachlorvinphos
Carbofuran Fenthion Permethrins Tetramethrin
Chlorantraniliprole Fenvalerate Phenothrin Thiacloprid
Chlorpyrifos Fipronil Phosmet Thiamethoxam
Clofentezine Flonicamid Piperonylbutoxide Thiophanate Methyl
Clothianidin Fludioxonil Pirimicarb Trifloxystrobin
Coumaphos Fluopyram Prallethrin
Cyantraniliprole Hexythiazox Propiconazole
Cyprodinil Imazalil Propoxur
Pyrethrins = Pyrethrin I and II
Spinetoram =
...
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