Abstract
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.
Highlights
In recent years, hemp products have experienced a strong increase in popularity.Besides hemp-based foods, consumer products containing cannabidiol (CBD) and in particular “CBD oils” are currently high in demand [1] and the market for CBD-containing dietary supplements continues to grow [2]
Different solubility and chemical stability properties of cannabinoids were found within the investigated pure solvents and mixtures
CD3 OD was not suitable for the nuclear magnetic resonance spectroscopy (NMR) measurement of CBD oils because the sample matrix consisting of an edible oil did not dissolve
Summary
Besides hemp-based foods (e.g., hemp seed oil, hemp flour), consumer products containing cannabidiol (CBD) and in particular “CBD oils” are currently high in demand [1] and the market for CBD-containing dietary supplements continues to grow [2]. The term “CBD oil” originates from the non-psychoactive cannabidiol (CBD) which naturally occurs in the hemp plant. CBD is marketed using unauthorized health or disease-related claims [1,2]. Despite the lack of clinical evidence, CBD is advertised as a natural remedy for treating anxiety, depression, pain, inflammatory and sleep disorders, and even cancer [2,4]. CBD oils are formulated as mixtures of an edible oil with extracts of the leaves and flowers of the hemp plant
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