CBD oils on the Belgian market: A validated MRM GC-MS/MS method for routine quality control using QuEChERS sample clean up

• Published in: Journal of pharmaceutical and biomedical analysis 2021-10, Vol.205, p.114344-114344, Article 114344
• Main Authors: Duchateau, Céline, Canfyn, Michaël, Desmedt, Bart, Kauffmann, Jean-Michel, Stévigny, Caroline, De Braekeleer, Kris, Deconinck, Eric
• Format: Article
• Language: English
• Subjects: Cannabidiol; CBD oils; MRM GC-MS/MS; Sample clean up
• ISSN: 0731-7085; 1873-264X
• DOI: 10.1016/j.jpba.2021.114344

•Development and validation of a routine GC-MS/MS MRM method with QuEChERS sample clean up.•CBD quantification, legality check and cannabinoids screening.•Only 45% of 18 CBD oil samples complied for the CBD content. All samples complied for Δ9-THC content. [Display omitted] Quality control of CBD oils on the Belgium market showed that the CBD content not always corresponds to the label claim. There is a pressing need to develop new analytical methods specifically developed to the assay of such oily samples. Analytical issues are, however, encountered for routine analyses due to the matrix complexity, high cost of cannabinoid standards and low Δ9-THC concentrations. An oily matrix could cause technical damages to analytical instruments and reduce the lifetime of the chromatographic columns. This paper proposes a procedure combining a sample cleanup by QuEChERS, removing the oily matrix, followed by a validated MRM GC-MS/MS method for the routine analysis of CBD oil samples. Eighteen CBD samples were selected on the Belgium market for analysis. This method allows the quantification of CBD, the legality check for the Δ9-THC content by a CBN standard and the screening of seven other cannabinoids namely CBN, CBDV, CBT, CBC, Δ8-THC, THCV and CBG. The method was validated at three concentration levels (0.5–1–2% (w/v)) for CBD and (0.05–0.1–0.2% (w/v)) for CBN. The detection limits for CBT, CBD, CBC, Δ8-THC, CBN and for the other cannabinoids of interest, were 10 and 14 ng/mL respectively. The accuracy profile values for CBD and CBN showed that the β-expectation tolerance intervals did not exceed the acceptance limits of ± 20%, meaning that 90% of future measurements will be included within this error range.