Accelerated Solvent Extraction of Terpenes in Cannabis Coupled With Various Injection Techniques for GC-MS Analysis

Colton Myers; Jason S Herrington; Paul Hamrah; Kelsey Anderson

doi:10.3389/fchem.2021.619770

Accelerated Solvent Extraction of Terpenes in Cannabis Coupled With Various Injection Techniques for GC-MS Analysis

Front Chem. 2021 Apr 1:9:619770. doi: 10.3389/fchem.2021.619770. eCollection 2021.

Authors

Colton Myers¹, Jason S Herrington¹, Paul Hamrah², Kelsey Anderson²

Affiliations

¹ Restek Corporation, Bellefonte, PA, United States.
² Verity Analytics, San Diego, CA, United States.

Abstract

The cannabis market is expanding exponentially in the United States. As state-wide legalization increases, so 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; r ² 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); gas chromatography–mass spectrometry (GC-MS); solid-phase microextraction (SPME); solid-phase microextraction Arrow (SPME Arrow); terpenes.