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ASTM D8399-22

(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 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
30-Jun-2022
ICS
11.120.99 - Other standards related to pharmaceutics
71.040.01 - Analytical chemistry in general
Technical Committee
D37 - Cannabis
Drafting Committee
D37.03 - Laboratory
Current Stage
Ref Project

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ASTM D8399-22 - 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)ASTM D8399-22 - 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)
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ASTM D8399-22 - 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)
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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: D8399 − 22
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 Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
1.1 This test method allows for the concentration determi-
Barriers to Trade (TBT) Committee.
nation of the pesticides listed in Table 1 and shall apply to any
dried raw material from a cannabis plant (Note 1, Note 2)
2. Referenced Documents
regardless of the type of cannabis plant from which it was
3
2.1 ASTM Standards:
2
derived (1, 2). For the sake of brevity, the term “cannabis”
D1193 Specification for Reagent Water
shall be used from now on to refer to any type of cannabis plant
D8245 Guide for Disposal of Resin-Containing Cannabis
including those which can be classified as hemp. The proce-
Raw Materials and Downstream Products
dure includes sub-sampling a ground, homogenous sample,
D8270 Terminology Relating to Cannabis
liquid-solid extraction with acetonitrile:acetic acid (100:1, v:v),
D8282 Practice for Laboratory Test Method Validation and
solid phase extraction with C18 SPE media, dilution in 3 mM
Method Development
ammonium formate in water with 0.1% formic acid and 3 mM
ammonium formate in methanol with 0.02% formic acid in a
3. Terminology
20:80 ratio (v:v) and analysis by LC-MS/MS. This procedure
3.1 Definitions—For general terms related to cannabis, refer
encompasses the entire process from sample preparation to
to Terminology D8270.
analyte quantitation encompassing a range of 0.005 µg ⁄g to
3.2 Definitions of Terms Specific to This Standard:
0.500 µg ⁄g.
3.2.1 blank, n—a cannabis-only sample prepared from the
NOTE 1—For this test method, dried raw material from a cannabis plant
includes one or more of inflorescence, leaves, or stems. same homogenous cannabis blend used to prepare the calibra-
NOTE 2—Certain jurisdictions or regulations may require specific parts
tion curve, without the addition of internal standard working
of the plant to be included or excluded for analysis and those regulations
solution (ISWS).
will take precedence for the selection of plant parts.
3.2.2 blank-0, 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, with the addition of ISWS.
standard.
3.2.3 blank-S, n—a solvent blank prepared from only the
1.3 Table 1 lists the analytes measured by this test method.
mobile phases, without cannabis or analytes.
1.4 This standard does not purport to address all of the
3.2.4 growth regulator, n—a class of chemical compounds
safety concerns, if any, associated with its use. It is the
used to modulate the growth and development of a crop.
responsibility of the user of this standard to establish appro-
3.2.5 pesticide, n—a product or substance used as a means
priate safety, health, and environmental practices and deter-
to reduce or mitigate pests such as insects, fungus, bacteria,
mine the applicability of regulatory limitations prior to use.
and weeds.
1.5 This international standard was developed in accor-
3.2.5.1 Discussion—May be used in gardens, crops, wood-
dance with internationally recognized principles on standard-
lands or recreational areas, these are fungicides, insecticides,
ization established in the Decision on Principles for the
herbicides, and biocontrols approved for use by regulatory
authorities to control pests harmful to plants, humans, or
animals.
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.
3
Current edition approved July 1, 2022. Published August 2022. DOI: 10.1520/ For referenced ASTM standards, visit the ASTM website, www.astm.org, or
D8399-22. 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 C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D8399 − 22
TABLE 1 List of Measureable Analytes
Abamecti
...

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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.
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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.  
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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.
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1.4 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.

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    5 pages
    English language
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  • Technical specification
    5 pages
    English language
    sale 15% off