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Publication Title | A Preliminary FET Headspace GC-FID Method for Comprehensive Terpene Profiling in Cannabis

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Foods, Flavors & Fragrances Applications

A Preliminary FET Headspace GC-FID Method for Comprehensive Terpene Profiling in Cannabis

By Amanda Rigdon, Corby Hilliard, and Jack Cochran

Abstract

is application note describes an FET headspace GC-FID method that was developed in hops for the analysis of terpenes in cannabis. Good chromatographic separation allowed quanti cation of critical compounds across the volatility range, including α-pinene, β-myrcene, α-humulene, β-caryophyllene, and caryophyllene oxide.

Introduction

In addition to cannabinoids, cannabis contains a suite of compounds known as terpenes. Terpenes are not only responsible for the characteristic aromas of cannabis strains, but they also are suspected to contribute to the therapeutic properties of cannabis. By themselves, terpenes have anti-in ammatory and anti-microbial properties, and they also reportedly contribute to an “entourage e ect” with cannabinoids, modulating and/or enhancing their activity [1,2].

Because terpenes may contribute to the therapeutic e ects of cannabis, there is a growing demand for analytical methods that pro le terpenes in marijuana samples. In addition to analyzing terpenes for therapeutic purposes, terpenes can also be used as di erentiators among cannabis strains and terpene pro les can be used for strain identi cation.

While relatively few terpenes have been studied for therapeutic purposes, cannabis strains can contain dozens of terpenes in varying levels. Of these, the primary compounds of interest include α-pinene, β-myrcene, α-humulene, and β-caryophyllene [2,3]. Accurately pro ling these analytes and other emerging terpenes of interest depends heavily on separating them from potentially interfering compounds. When an interfering terpene, or other compound, coelutes with a terpene of interest, quanti cation will be compromised and, since many terpenes have the same molecular weight and share fragment ions, mass spectrometry cannot be relied upon to distinguish a terpene of interest from a coeluting interference terpene. e only way to accurately identify and quantify terpenes is to ensure that the terpenes of interest are chromatographically separated from all interfering compounds. GC is an excellent technique for accomplishing this.

Here we present a headspace gas chromatography– ame ionization detection (GC-FID) method for a comprehensive set of 38 terpenes found in cannabis. Since cannabis is illegal in Pennsylvania where this work was done, we developed the method using hops as a model system since they are related to cannabis and contain a similar suite of terpenes [2,3,4]. e headspace method presented here utilizes full evaporation technique (FET) sample preparation because cannabis product matrices are extremely varied and plant material will not dissolve in solvent. FET involves the use of a very small sample amount (10–50 mg), which e ectively creates a single phase gas system in the headspace vial at equilibrium, making it ideal for this application [5,6,7]. Figure 1 illustrates the basic principle of headspace gas chromatography using FET. To achieve chromatographic separation, a 30 m x 0.25 mm x 1.4 μm Rxi®-624Sil MS column was used. is column was chosen based on several factors. First, and most importantly, the cyano-based stationary phase of the Rxi®-624Sil MS has excellent selectivity for terpenes, making it ideal to e ect a good separation for a large suite of these compounds. Second, in addition to its excellent selectivity for terpenes, the maximum temperature of this column is 320 °C, which allows for elution of some of the less volatile terpenes and matrix compounds that may be present in the headspace sample. ird, this GC column phase is also well-suited for residual solvent analysis, potentially minimizing the number of columns and instruments required by labs to test cannabis.

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