Cannabis Science Conference West 2022 (CSC West)

18-20 May , Long Beach, CA
Oral Presentation
Evaluation of Sample Preparation and Introduction Techniques for Terpene Analysis via GC-MS
As cannabis approaches countrywide legalization, the demands for analytical testing continue to increase. The five major chromatographic analyses conducted in cannabis testing laboratories include potency, residual solvents, terpenes, pesticides, and mycotoxins. While it is not required by testing regulations in multiple states, terpenes remain of great interest to cannabis growers and consumers. In this research, a systematic approach was taken to implement an effective workflow solution that could be conducted in a routine cannabis testing laboratory. The research presented will focus on the implementation of Accelerated Solvent Extraction (ASE) utilizing surrogate matrix matching and evaluating traditional versus more modern sample introduction techniques for analyzing terpenes via gas chromatography-mass spectrometry. Of the sample introduction techniques presented, the Liquid Injection-Syringe (LI-Syringe) approach was the most straightforward and robust method. Workflows and results will be discussed along with opportunities for future work.
- Information:
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10:00 a.m., EST - 10:30 a.m., 10:00 a.m.20 May 2022
- Authors:
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- Colton Myer (1); Jason S. Herrington (1); Paul Hamrah (2); Kelsey Anderson (2)
- Affiliations:
- 1. Restek Corporation, 2. Verity Analytics
- Presenters:
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Colton MyerRestek Corporation
Poster Presentation
The Detection of Flavonoids in Hemp Flower by LC-MS/MS
Hemp is a chemically complex matrix that contains a wide array of bioactive compounds whose synergistic interactions give hemp and cannabis their therapeutic effects. Flavonoids are a class of compounds endogenous in hemp and cannabis that are antioxidant rich and can affect the flavor profile. Routine testing in cannabis labs oftentimes does not include flavonoid testing but as the market for both cannabis analysis and products grows, industry leaders may choose to implement new tests that not only aid the advancement of the science of cannabis but also to differentiate their services or products from their competitors. In this work, a method to detect 19 flavonoids in CBD and CBG dominant hemp flower was developed using LC-MS/MS. Extraction of flavonoids was performed by weighing out 0.5 g of ground hemp flower. 80/20 methanol/water (10 mL) was added to the hemp flower and vortexed. The samples were sonicated for 15 min, centrifuged at 4200 rpm for 5 min, and diluted 50-fold. The analytical method was developed using LC-MS/MS with electrospray ionization in positive and negative ion modes. Mobile phase A consisted of 0.1 % formic acid in water and mobile phase B consisted of 0.1% formic acid in methanol. The method uses gradient conditions on a Raptor Biphenyl 100 x 2.1, 2.7 µm column equipped with a guard cartridge. The chromatographic method was able to resolve all isobars with an overall analysis time of 7 minutes. Ten flavonoids were detected in the CBG hemp flower sample and 12 flavonoids were detected in the CBD hemp flower samples. Single point recovery experiments were also performed at 100 ppb using two isotopically labeled internal standards. The results of the single point recovery ranged from 80–104%. The developed method was able to resolve isobars within a cycle time of 7 minutes, and acceptable recoveries were achieved for both hemp flower samples, indicating this is an effective procedure for the extraction of flavonoids from hemp flower.
- Information:
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May 18 - May 2018 May 2022
The Analysis of 21 Cannabinoids by LC-MS
Testing cannabis products for potency is typically performed by LC-UV/VIS. This methodology is robust, reliable, and cost-effective but it has limited capabilities, namely, the complete chromatographic separation of all compounds and reduced detection sensitivity compared to MS. As cannabis research continues to accelerate, it is likely new phytocannabinoids of interest will need to be added into potency testing methods, which can be challenging due to the limited chromatographic space. MS can offer a sensitive and selective alternative to LC-UV/VIS methods by reaching much lower detection limits while only requiring the separation of isobaric compounds. In this work, a method was developed to detect 21 cannabinoids by LC-MS using isocratic mobile phase conditions. The method was performed on an LC-MS using electrospray ionization in positive and negative ion modes. Complete resolution of isobars was achieved using isocratic mobile phase (MP) conditions at 20:80 (MPA:MPB) with mobile phases containing 0.1% formic acid and 12 mM ammonium formate in water (A) and 0.1% formic acid in acetonitrile:methanol (50:50) (B). The column used for these experiments was a Raptor ARC-18 150 mm x 2.1 mm, 2.7 µm with the column oven at a temperature of 30 °C and a flow rate of 0.5 mL/min. In these experiments, 21 cannabinoids were monitored, including two recently discovered compounds, tetrahydrocannabiphorol (THCP) and cannabidiphorol (CBDP). Compounds indistinguishable by MS were identified and isolated to five groups. Chromatographic separation was essential within these five groups of isobars, which was achieved using the outlined conditions.