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Quantitative determination and validation of 17 cannabinoids in cannabis and hemp using liquid chromatography-tandem mass spectrometry.

Authors
  • McRae, Garnet1
  • Melanson, Jeremy E2
  • 1 National Research Council of Canada, Metrology, 1200 Montreal Road, Ottawa, ON, K1A 0R6, Canada. , (Canada)
  • 2 National Research Council of Canada, Metrology, 1200 Montreal Road, Ottawa, ON, K1A 0R6, Canada. [email protected] , (Canada)
Type
Published Article
Journal
Analytical and Bioanalytical Chemistry
Publisher
Springer-Verlag
Publication Date
Nov 01, 2020
Volume
412
Issue
27
Pages
7381–7393
Identifiers
DOI: 10.1007/s00216-020-02862-8
PMID: 32833075
Source
Medline
Keywords
Language
English
License
Unknown

Abstract

The increase in production of cannabis for medical and recreational purposes in recent years has led to a corresponding increase in laboratories performing cannabinoid analysis of cannabis and hemp. We have developed and validated a quantitative liquid chromatography-tandem mass spectrometry (LC-MS/MS) method that is simple, reliable, specific, and accurate for the analysis of 17 cannabinoids in cannabis and hemp. Liquid-solid sample extraction coupled with dilution into a calibration range from 10 to 10,000 ng/mL and LC-MS/MS analysis provides quantification of samples ranging from 0.002 to 200 mg/g (0.0002 to 20.0%) in matrix. Linearity of calibration curves in methanol was demonstrated with regression r2 ≥ 0.99. Within-batch precision (0.5 to 6.5%) and accuracy (91.4 to 108.0%) and between-batch precision (0.9 to 5.1%) and accuracy (91.5 to 107.5%) were demonstrated for quality control (QC) samples in methanol. Within-batch precision (0.2 to 3.6%) and accuracy (85.4 to 111.6%) and between-batch precision (1.4 to 6.1 %) and accuracy (90.2 to 110.3%) were also evaluated with a candidate cannabis certified reference material (CRM). Repeatability (1.5 to 12.4% RSD) and intermediate precision (2.2 to 12.8% RSD) were demonstrated via analysis of seven cannabis samples with HorRat values ranging from 0.3 to 3.1. The method provides enhanced detection limits coupled with a large quantitative range for 17 cannabinoids in plant material. It is suitable for a wide range of applications including routine analysis for delta-9-tetrahydrocannabinol (Δ9-THC), delta-9-tetrahydrocannabinolic acid (Δ9-THCA), cannabidiol (CBD), cannabidiolic acid (CBDA), and cannabinol (CBN) as well as more advanced interrogation of samples for both major and minor cannabinoids.

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