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A Quantitative 1H NMR Method for Screening Cannabinoids in CBD Oils

Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weißenburger Straße 3, 76187 Karlsruhe, Germany
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Academic Editors: Jana Pulkrabova and Aristeidis Tsagkaris
Toxics 2021, 9(6), 136; https://doi.org/10.3390/toxics9060136
Received: 14 May 2021 / Revised: 3 June 2021 / Accepted: 5 June 2021 / Published: 10 June 2021
Toxicologically relevant levels of the psychoactive ∆9-tetrahydocannabinol (∆9-THC) as well as high levels of non-psychoactive cannabinoids potentially occur in CBD (cannabidiol) oils. For consumer protection in the fast-growing CBD oil market, facile and rapid quantitative methods to determine the cannabinoid content are crucial. However, the current standard method, i.e., liquid chromatography combined with tandem mass spectrometry (HPLC-MS/MS), requires a time-consuming multistep sample preparation. In this study, a quantitative nuclear magnetic resonance spectroscopy (qNMR) method for screening cannabinoids in CBD oils was developed. Contrary to the HPLC-MS/MS method, this qNMR features a simple sample preparation, i.e., only diluting the CBD oil in deuterochloroform. Pulse length-based concentration determination (PULCON) enables a direct quantification using an external standard. The signal intensities of the cannabinoids were enhanced during the NMR spectra acquisition by means of multiple suppression of the triglycerides which are a major component of the CBD oil matrix. The validation confirmed linearity for CBD, cannabinol (CBN), ∆9-THC and ∆8-THC in hemp seed oil with sufficient recoveries and precision for screening. Comparing the qNMR results to HPLC-MS/MS data for 46 commercial CBD oils verified the qNMR accuracy for ∆9-THC and CBD, but with higher limits of detection. The developed qNMR method paves the way for increasing the sample throughput as a complementary screening before HPLC-MS/MS. View Full-Text
Keywords: cannabidiol (CBD); ∆9-tetrahydrocannabinol (∆9-THC); cannabinol (CBN); ∆8-tetrahydrocannabinol (∆8-THC); cannabinoids; CBD oil; nuclear magnetic resonance spectroscopy (NMR); PULCON methodology; 1H NMR; qNMR cannabidiol (CBD); 9-tetrahydrocannabinol (∆9-THC); cannabinol (CBN); 8-tetrahydrocannabinol (∆8-THC); cannabinoids; CBD oil; nuclear magnetic resonance spectroscopy (NMR); PULCON methodology; 1H NMR; qNMR
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MDPI and ACS Style

Barthlott, I.; Scharinger, A.; Golombek, P.; Kuballa, T.; Lachenmeier, D.W. A Quantitative 1H NMR Method for Screening Cannabinoids in CBD Oils. Toxics 2021, 9, 136. https://doi.org/10.3390/toxics9060136

AMA Style

Barthlott I, Scharinger A, Golombek P, Kuballa T, Lachenmeier DW. A Quantitative 1H NMR Method for Screening Cannabinoids in CBD Oils. Toxics. 2021; 9(6):136. https://doi.org/10.3390/toxics9060136

Chicago/Turabian Style

Barthlott, Ines, Andreas Scharinger, Patricia Golombek, Thomas Kuballa, and Dirk W. Lachenmeier. 2021. "A Quantitative 1H NMR Method for Screening Cannabinoids in CBD Oils" Toxics 9, no. 6: 136. https://doi.org/10.3390/toxics9060136

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