Journal:Accelerated solvent extraction of terpenes in cannabis coupled with various injection techniques for GC-MS analysis

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Full article title Accelerated solvent extraction of terpenes in cannabis coupled with various injection techniques for GC-MS analysis
Journal Frontiers in Chemistry
Author(s) Myers, Colton; Herrington, Jason S.; Hamrah, Paul; Anderson, Kelsey
Author affiliation(s) Restek Corporation, Verity Analytics
Primary contact colton dot myers at restek dot com
Year published 2021
Volume and issue 9
Article # 619770
DOI 10.3389/fchem.2021.619770
ISSN 2296-2646
Distribution license Creative Commons Attribution 4.0 International
Website https://www.frontiersin.org/articles/10.3389/fchem.2021.619770/full
Download https://www.frontiersin.org/articles/10.3389/fchem.2021.619770/pdf (PDF)

Abstract

The cannabis market is expanding exponentially in the United States. As state-wide legalization efforts increase, so also do demands for analytical testing methodologies. One of the main tests conducted on cannabis products is the analysis for terpenes. This research focused on implementation of accelerated solvent extraction (ASE), utilizing surrogate matrix matching, and evaluation of traditional vs. more modern sample introduction techniques for analyzing terpenes via gas chromatography–mass spectrometry (GC-MS). Introduction techniques included headspace syringe (HS syringe), HS-solid-phase microextraction Arrow (HS-SPME Arrow), direct immersion-SPME Arrow (DI-SPME Arrow), and liquid injection syringe (LI syringe). The LI syringe approach was deemed the most straightforward and robust method, with terpene working ranges of 0.04–5.12 μg/mL; r2 values of 0.988–0.996 (0.993 average); limit of quantitation values of 0.017–0.129 μg/mL (0.047 average); analytical precisions of 2.58–9.64% RSD (1.56 average); overall ASE-LI-syringe-GC-MS method precisions of 1.73–14.6% RSD (4.97 average); and % recoveries of 84.6–98.9% (90.2 average) for the 23 terpenes of interest. Sample workflows and results are discussed, with an evaluation of the advantages/limitations of each approach and opportunities for future work.

Keywords: accelerated solvent extraction (ASE), terpenes, solid-phase microextraction (SPME), solid-phase microextraction Arrow (SPME Arrow), gas chromatography–mass spectrometry (GC-MS)

Introduction

The legal cannabis market is one of the fastest growing markets across the globe. In 2019, cannabis use for medicinal purposes in the United States generated $4 billion to $4.9 billion in sales, compared to the adult-use estimates between $6.6 billion and $8.1 billion.[1] As the United States and additional countries continue to legalize the use of medicinal and recreational cannabis, analytical testing demands increase. A 2020 report by Market Data Forecast valued the global cannabis testing market at $1,218.0 million in 2019 and estimated it to be growing at a compound annual growth rate (CAGR) of 12.42%.[2] The market is projected to almost double at $2,187.3 million by 2024.[2] Of the examinations conducted in cannabis testing laboratories, terpene profiling is a popular analysis, regardless of state regulations.

Terpenes are a naturally occurring set of organic compounds, which are commonly found in plants, and are typically strong in odor.[3] Terpenes are made up of isoprene units and are classified by the number of their isoprene units.[3] The two types of terpenes that are commonly analyzed in the cannabis testing industry are monoterpenes, which have two isoprene units, and sesquiterpenes, which have three isoprene units. Over 100 terpenes have been identified in different cannabis chemical varieties (chemovars).[4] Each cannabis chemovar has its own unique terpene profile, giving consumers different aromas, flavors, and experiences depending on the chemovar they use. According to Russo et al., terpenes play a major role in the entourage effect, which is the synergistic interaction between phytocannabinoids and terpenoids with respect to treating numerous ailments (e.g., depression).[5] The desire to understand and capitalize on this entourage effect is the motivation for terpene testing in the cannabis industry.


References

  1. Stelton-Holtmeier, J. (25 August 2020). "Chart: Nationwide sales of adult-use cannabis further eclipse those of medical marijuana". Marijuana Business Daily. https://mjbizdaily.com/chart-nationwide-sales-of-adult-use-cannabis-further-eclipse-those-of-medical-marijuana/. Retrieved 31 August 2020. 
  2. 2.0 2.1 "Chart: Nationwide sales of adult-use cannabis further eclipse those of medical marijuana". February 2020. https://www.marketdataforecast.com/market-reports/cannabis-testing-market. Retrieved 31 August 2020. 
  3. 3.0 3.1 Nuutinen, T. (2018). "Medicinal properties of terpenes found in Cannabis sativa and Humulus lupulus". European Journal of Medicinal Chemistry 157: 198–228. doi:10.1016/j.ejmech.2018.07.076. PMID 30096653. 
  4. Calvi, L.; Pentimalli, D.; Panseri, S. et al. (2018). "Comprehensive quality evaluation of medical Cannabis sativa L. inflorescence and macerated oils based on HS-SPME coupled to GC–MS and LC-HRMS (q-exactive orbitrap) approach". Journal of Pharmaceutical and Biomedical Analysis 150: 208–19. doi:10.1016/j.jpba.2017.11.073. 
  5. Russo, E.B. (2011). "Taming THC: Potential cannabis synergy and phytocannabinoid-terpenoid entourage effects". British Journal of Pharmacology 163 (7): 1344-64. doi:10.1111/j.1476-5381.2011.01238.x. PMC PMC3165946. PMID 21749363. http://www.pubmedcentral.nih.gov/articlerender.fcgi?tool=pmcentrez&artid=PMC3165946. 

Notes

This presentation is faithful to the original, with only a few minor changes to presentation. Some grammar and punctuation was cleaned up to improve readability. In some cases important information was missing from the references, and that information was added. The original article lists references in alphabetical order; this wiki organizes them by order of appearance, by design.