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J Food Drug Anal. 2018 Oct;26(4):1283-1292. doi: 10.1016/j.jfda.2018.06.001. Epub 2018 Jul 3.

Development and validation of a Fast gas chromatography/mass spectrometry method for the determination of cannabinoids in Cannabis sativa L.

Author information

1
Interdepartmental Centre for Industrial Agrofood Research, Alma Mater Studiorum - University of Bologna, Cesena, 47521, Italy.
2
Interdepartmental Centre for Industrial Agrofood Research, Alma Mater Studiorum - University of Bologna, Cesena, 47521, Italy; Department of Agricultural and Food Sciences, Alma Mater Studiorum - University of Bologna, Bologna, 40127, Italy. Electronic address: tullia.gallinatoschi@unibo.it.
3
Department of Agricultural and Food Sciences, Alma Mater Studiorum - University of Bologna, Bologna, 40127, Italy.
4
Enecta B.V, Amsterdam, 1058DA, Netherlands.
5
Interdepartmental Centre for Industrial Agrofood Research, Alma Mater Studiorum - University of Bologna, Cesena, 47521, Italy; Department of Agricultural and Food Sciences, Alma Mater Studiorum - University of Bologna, Bologna, 40127, Italy.

Abstract

A routine method for determining cannabinoids in Cannabis sativa L. inflorescence, based on Fast gas chromatography coupled to mass spectrometry (Fast GC/MS), was developed and validated. To avoid the decarboxylation of carboxyl group of cannabinoids, different derivatization approaches, i.e. silylation and esterification (diazomethane-mediated), reagents and solvents (pyridine or ethyl acetate), were tested. The methylation significantly increased the signal-to-noise ratio of all carboxylic cannabinoids, except for cannabigerolic acid (CBGA). Since diazomethane is not commercially available, is considered a hazardous reactive and requires 1-day synthesis by specialized chemical staff, silylation was used along the whole validation of a routine method. The method gave a fast (total analysis time < 7.0 min) and satisfactory resolution (R > 1.1), with a good repeatability (intraday < 8.38%; interday < 11.10%) and sensitivity (LOD < 11.20 ng/mL). The Fast GC/MS method suitability for detection of cannabinoids in hemp inflorescences, was tested; a good repeatability (intraday < 9.80%; interday < 8.63%), sensitivity (LOD < 58.89 ng/mg) and robustness (<9.52%) was also obtained. In the analyzed samples, the main cannabinoid was cannabidiolic acid (CBDA, 5.19 ± 0.58 g/100 g), followed by cannabidiol (CBD, 1.56 ± 0.03 g/100 g) and CBGA (0.83 g/100 g). Δ9-tetrahydrocannabivarine (THCV) was present at trace level. Therefore, the developed routine Fast GC/MS method could be a valid alternative for a fast, robust and high sensitive determination of main cannabinoids present in hemp inflorescences.

KEYWORDS:

Cannabinoids; Cannabis; Decarboxylation; Fast gas chromatography; Methylation

PMID:
30249327
DOI:
10.1016/j.jfda.2018.06.001
[Indexed for MEDLINE]
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