Validated quantitative cannabis profiling for Canadian regulatory compliance - Cannabinoids, aflatoxins, and terpenes

Brown, Alistair K.; Xia, Zhe; Bulloch, Patrique; Idowu, Ifeoluwa; Francisco, Olga; Stetefeld, Jörg; Stout, Jake; Zimmer, Jeff; Märvin, Chris H.; Letcher, Robert J.; Tomy, Gregg T.

doi:10.1016/j.aca.2019.08.042

Cited by 32 publications

(19 citation statements)

References 16 publications

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“…The terpene compositions of cannabis are a seasonal variable. The alteration in the proportion of terpenoids in cannabis are in accordance with the variety of cannabis, plant part, environmental conditions, maturity, and method of analyses [72][73][74]. Different growth stages of the cannabis could give considerable variations in the terpene compositions.…”

Section: The Cannabis Chemovarsmentioning

confidence: 98%

The Cannabis Terpenes

et al. 2020

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Terpenes are the primary constituents of essential oils and are responsible for the aroma characteristics of cannabis. Together with the cannabinoids, terpenes illustrate synergic and/or entourage effect and their interactions have only been speculated in for the last few decades. Hundreds of terpenes are identified that allude to cannabis sensory attributes, contributing largely to the consumer’s experiences and market price. They also enhance many therapeutic benefits, especially as aromatherapy. To shed light on the importance of terpenes in the cannabis industry, the purpose of this review is to morphologically describe sources of cannabis terpenes and to explain the biosynthesis and diversity of terpene profiles in different cannabis chemovars.

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Section: The Cannabis Chemovarsmentioning

confidence: 98%

The Cannabis Terpenes

et al. 2020

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“…Due to the various combinations of sample matrix, solvent extraction, sample cleanup, and chromatography techniques, reported precision of analytical protocols for cannabinoids in complex matrices varies dramatically in the literature. For cannabis plant materials, protocols often only include solvent extraction and chromatographic analysis due to the high levels of cannabinoids (Brown et al, 2019; Cardenia et al, 2018; Elkins et al, 2019; Leiman et al, 2018). When GC–MS was used, analytical precision of CBD, THC, CBDA, THCA, and CBGA ranged from 6.11% to 8.86% and from 0.80% to 8.63% for intraday and interday, respectively (Brown et al, 2019; Cardenia et al, 2018; Leiman et al, 2018).…”

Section: Resultsmentioning

confidence: 99%

“…For cannabis plant materials, protocols often only include solvent extraction and chromatographic analysis due to the high levels of cannabinoids (Brown et al, 2019; Cardenia et al, 2018; Elkins et al, 2019; Leiman et al, 2018). When GC–MS was used, analytical precision of CBD, THC, CBDA, THCA, and CBGA ranged from 6.11% to 8.86% and from 0.80% to 8.63% for intraday and interday, respectively (Brown et al, 2019; Cardenia et al, 2018; Leiman et al, 2018). For biological samples, most analytical protocols include a SPE cleanup step and the use of LC–MS (Escrivá et al, 2017;Sobolesky et al, 2019; Sørensen & Hasselstrøm, 2017; Wei et al, 2016).…”

Section: Resultsmentioning

confidence: 99%

Sample preparation for the analysis of key metabolites from cannabinoids biosynthesis in phytoplankton using gas chromatography–mass spectrometry

Budge

2021

J Americ Oil Chem Soc

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Cannabinoids biosynthesis in phytoplankton has attracted much attention due to the rapid development of genetic tools and the optimization of genetic transformation methods in microalgae. To monitor the biosynthesis process, proper sample preparation and practical instrumental methods are needed to measure the various precursors, intermediates, cannabinoids, and their degradation products. The objective of this study was to develop a sample preparation procedure for the quantification of olivetolic acid (OA), cannabigerolic acid (CBGA), cannabidiolic acid (CBDA), tetrahydrocannabinolic acid (THCA), olivetol (OL), cannabidiol (CBD), and tetrahydrocannabinol (THC) using single‐quadrupole gas chromatography–mass spectrometry (GC–MS). Isochrysis galbana was used as the model matrix. After methanol extraction, samples were purified using solid phase extraction (SPE), silylated with N‐methyl‐N‐(trimethylsilyl)trifluoroacetamide, and analyzed using GC–MS in electron ionization mode. A strong anion‐exchange SPE efficiently recovered OA, CBGA, CBDA, and THCA. A graphitized carbon black SPE was necessary to purify OL, CBD, and THC. Both columns removed amino acids, sugars, polyols, and pigments from the algae extract and prepared samples that are suitable for silylation and GC–MS analysis. The total protocol, including solvent extraction, SPE, silylation, and GC–MS analysis, was validated in accordance with the ICH guidelines. Performance characteristics of our method are superior to existing protocols with similar complexity in the literature.

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“…Increased temperatures, indeed, trigger decarboxylation and other reactions prevent their detection in the acid forms [2]. On the other hand, LC-MS, where decarboxylation is avoided, has been used for the quantitative detection of THCA and CBDA along with other cannabinoids from dried cannabis [7], hemp seed batches, food and feed products [8,9], seized street cannabis samples and medicines [10], as well as hemp consumer products such as oils, plant material, creams, and cosmetics [11]. An interesting kinetic study on the thermal degradation of 14 phytocannabinoids was performed by low resolution mass spectrometry (LRMS) targeted analysis from dried plant material [12].…”

Section: Introductionmentioning

confidence: 99%

Direct In Vivo Analysis of CBD- and THC-Acid Cannabinoids and Classification of Cannabis Cultivars Using SpiderMass

et al. 2022

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In recent years, cannabis and hemp-based products have become increasingly popular for recreational use, edibles, beverages, health care products, and medicines. The rapid detection and differentiation of phytocannabinoids is, therefore, essential to assess the potency and the therapeutic and nutritional values of cannabis cultivars. Here, we implemented SpiderMass technology for in vivo detection of cannabidiolic acid (CBDA) and ∆9-tetrahydrocannabinolicacid (∆9-THCA), and other endogenous organic plant compounds, to access distribution gradients within the plants and differentiate between cultivars. The SpiderMass system is composed of an IR-laser handheld microsampling probe connected to a mass spectrometer through a transfer tube. The analysis was performed on different plant organs from freshly cultivated cannabis plants in only a few seconds. SpiderMass analysis easily discriminated the two acid phytocannabinoid isomers via MS/MS, and the built statistical models differentiated between four cannabis cultivars. Different abundancies of the two acid phytocannabinoids were found along the plant as well as between different cultivars. Overall, these results introduce direct analysis by SpiderMass as a compelling analytical alternative for rapid hemp analysis.

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Validated quantitative cannabis profiling for Canadian regulatory compliance - Cannabinoids, aflatoxins, and terpenes

Cited by 32 publications

References 16 publications

The Cannabis Terpenes

The Cannabis Terpenes

Sample preparation for the analysis of key metabolites from cannabinoids biosynthesis in phytoplankton using gas chromatography–mass spectrometry

Direct In Vivo Analysis of CBD- and THC-Acid Cannabinoids and Classification of Cannabis Cultivars Using SpiderMass

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