THC Plant Material Analysis

Introduction

The express ion^S compact mass spectrometer (CMS) is a novel high performance, easy-to-use single quadrupole mass spectrometer with enhanced scan speed and the ability for on-line polarity switching and in-source fragmentation. Priced substantially lower than other MS systems and having a small footprint to fit in space restricted laboratories, the CMS brings the analytical benefits of mass spectrometry to more laboratories than ever before.

Analysis of the active components of the cannabis sativa plant is required both for law enforcement where these compounds are illegal and also as a tool for product control and optimization in the increasing number of legal markets for cannabis plant products. Whenever simple, unequivocal and legally defensible analysis methods for the detection and quantification of plant metabolites are required, mass spectrometry is the detector of choice.

Figure 1: A Compact Mass Spectrometer (expression, Advion, NY, 1a) connected to the Plate Express (1b and 1c), a device for the extraction of samples from a TLC plate. CMS provides valuable additional information in natural product analysis workflows.

Here, we present two simple workflows for the analysis of cannabinoids such as the naturally occuring cannabinol (CBN), the psychoactive ingredient of cannabis sativa, tetrahydrocannabinol (THC) and the degradation product cannabidiol (CBD). Both TLC/FIA/CMS for qualitative detection of cannabinoids, as well as HPLC/CMS for the quantitative determination of THC demonstrate the added benefit of compact mass spectrometry in the analysis of natural products.

Method

Thin layer chromatography (TLC): Cannabinoids were separated on TLC silica gel 60 F254 (Merck, NJ) with a run solvent of 80/20 Petrolether (60-80 bp) / Dioxane (Sigma Aldrich, MO)^[1]. TLC/FIA/MS analysis: Utilizing the Plate Express™ (Advion, NY) with a solvent flow rate of 200 μL/min methanol 0.1 vol% formic acid. HPLC analysis: Samples were analyzed with a 1220 HPLC system including a UV detector (Agilent, CA) on a Supelco Titan 2.1 mm column (Sigma-Aldrich, MO) at a flow rate of 350 μL/min and a 5 min gradient from 50 % to 90 % Acetonitrile 0.1 vol% formic acid.MS analysis: A mass range of m/z 100 to m/z 1000 was scanned using both polarity switching and in-source CID. SIM scanning in negative ion mode MS was used at m/z 313.2 (THC and CBD) and m/z 309.2 (CBN) for the quantitative analysis approach. Both MS methods used the expression^S CMS mass spectrometer (Advion, NY).

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