Quantitative determination and validation of 17 cannabinoids in cannabis and hemp using liquid chromatography-tandem mas
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Quantitative determination and validation of 17 cannabinoids in cannabis and hemp using liquid chromatography-tandem mass spectrometry Garnet McRae 1 & Jeremy E. Melanson 1 Received: 29 June 2020 / Revised: 29 July 2020 / Accepted: 4 August 2020 # The Author(s) 2020
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 ranges 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 (1.4 to 6.1%) 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. Keywords Cannabinoids . Cannabis . Hemp . Liquid chromatography-mass spectrometry . Validation
Introduction With the legalization of recreational cannabis in Canada and medicinal cannabis in many other jurisdictions, a large number of analytical laboratories servicing the cannabis industry have emerged to address the growing need for cannabis testing. The lack of standardization in cannabis testing has resulted in a wide
ABC Highlights: authored by Rising Stars and Top Experts. Electronic supplementary material The online version of this article (https://doi.org/10.1007/s00216-020-02862-8) contains supplementary material, which is available to authorized users. * Jeremy E. Melanson [email protected] 1
National Research Council of Canada, Metrology, 1200 Montreal Road, Ottawa, ON K1A 0R6, Canada
variety of methods being used, which has undoubtedly contributed to the high variability of results between testing laboratories [1, 2]. However, associations such as AOAC, AST
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