Rapid distinction and semiquantitative analysis of THC and CBD by silver-impregnated paper spray mass spectrometry

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Abstract

The control over the amount of psychoactive THC (Δ-9tetrahydrocannabinol) in commercial cannabidiol (CBD) products has to be strict. A fast and simple semiquantitative Ag(I)-impregnated paper spray mass spectrometric method for differentiating between THC and CBD, which show no difference in standard single-stage or tandem MS, was established. Because of a different binding affinity to Ag(I) ions, quasi-molecular Ag(I) adducts [THC + Ag]+ and [CBD + Ag]+ at m/z 421 and 423 give different fragmentation patterns. The product ions at m/z 313 for THC and m/z 353 and 355 for CBD can be used to distinguish THC and CBD and to determine their ratio. Quantification of THC/CBD ratios in commercial CBD oils was accomplished with a low matrix effect (−2.2 ± 0.4% for THC and −2.0 ± 0.3% for CBD). After simple methanol extraction (recovery of 87.3 ± 1.2% for THC and 92.3 ± 1.4% for CBD), Ag(I)-impregnated paper spray analysis was employed to determine this ratio. A single run can be completed in a few minutes. This method was benchmarked against the UHPLC-UV method. Ag(I)impregnated paper spray MS had the same working range (THC/CBD = 0.001−1) as UHPLC-UV analysis (R2 = 0.9896 and R2 = 0.9998, respectively), as well as comparable accuracy (−2.7 to 14%) and precision (RSD 1.7−11%). The method was further validated by the analysis of 10 commercial oils by Ag(I)-impregnated paper spray MS and UHPLC-UV analysis. Based on the determined relative concentration ratios of THC/CBD and the declared CBD concentration, 6 out of 10 CBD oils appear to contain more THC than the Dutch legal limit of 0.05%.

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Zuilhof, H., Salentijn, G. I. J., Huang, S., Claassen, F. W., van Beek, T. A., Chen, B., & Zeng, J. (2021). Rapid distinction and semiquantitative analysis of THC and CBD by silver-impregnated paper spray mass spectrometry. Analytical Chemistry, 93(8), 3794–3802. https://doi.org/10.1021/acs.analchem.0c04270

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