Reference : SFC-MS as a preventive tool for the quality control of potentially adulterated cannab...
Scientific congresses and symposiums : Unpublished conference/Abstract
Physical, chemical, mathematical & earth Sciences : Chemistry
Human health sciences : Pharmacy, pharmacology & toxicology
http://hdl.handle.net/2268/227217
SFC-MS as a preventive tool for the quality control of potentially adulterated cannabis with synthetic cannabinoids
English
Jambo, Hugues mailto [Université de Liège - ULiège > Département de pharmacie > Chimie analytique >]
Dispas, Amandine mailto [Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments >]
Avohou, Tonakpon Hermane mailto [Université de Liège - ULiège > Département de pharmacie > Chimie analytique >]
André, Sébastien mailto [Université de Liège - ULiège > > > Master sc. pharma., à fin.]
Hubert, Cédric mailto [Université de Liège - ULiège > Département de pharmacie > Département de pharmacie >]
Lebrun, Pierre mailto [Arlenda S.A. > > > >]
Ziemons, Eric mailto [Université de Liège - ULiège > Département de pharmacie > Département de pharmacie >]
Hubert, Philippe mailto [Université de Liège - ULiège > Département de pharmacie > Chimie analytique >]
19-Oct-2018
Yes
International
SFC 2018
17 - 19 October 2018
Strasbourg
France
[en] Recent years have been the stage to a shift in cannabis policies and trends that have impacted cannabis usage and public perception. It has also caught the attention of the pharmaceutical industry and cannabis is increasingly evaluated as a medicine in the treatment of various conditions. On the other hand, there has also been a rise in the development and distribution of synthetic cannabinoids which are synthetic compounds that have the same pharmacological action as the natural cannabinoids found in the plant. They are mostly used as recreational drugs and because their potency and toxicity are not always known, they can lead to severe adverse effects after consumption. The detection of counterfeiting cannabis with synthetic cannabinoids is essential to produce safe cannabis-based medicines. Our aim was to develop a generic supercritical fluid chromatography hyphenated to mass spectrometry (SFC-MS) method that could help in detecting such adulterations using representative synthetic cannabinoids from multiple classes.

Method development started with a screening of stationary phases using seven different SFC-dedicated columns. The Torus 1-AA (amino-anthracene) provided the best retention and resolution for the analytes and was selected for the study. Likewise, the mobile phase modifier composition (methanol/water 98:2 v/v) was set after these preliminary tests.

The next step performed was the optimization of the method using a design of experiments (DoE) and Bayesian design space (DS) methodology. The temperature, pressure, isocratic and gradient time were selected as parameters for the DoE (central composite design). The separation criterion (S) was set to -0.5 to maximize the separation capacity of the generic method. This Quality by Design (QbD) approach is advantageous as it permits the testing of various conditions within the design space (DS) to achieve a desirable separation since unassessed compounds will probably be encountered during routine analysis.

Finally, the quantitative performances were demonstrated by means method validation based on total error approach for the quantification of a selected synthetic cannabinoid in fiber type cannabis plant matrix. Sample preparation was performed with solid-liquid extraction (SLE) followed by filtration and dilution. The acceptance limits were set at ±15% and the β-expectation tolerance limits at 90 % probability level. The results show that the method is valid over the whole dosing range assessed of 2.5 - 7.5% (w/w) with the LOD equal to 14.40 ng/mL.

The implementation of this method should be straightforward considering the ease of sample preparation, the use of a fast and green SFC separation and the high specificity and sensitivity achieved with mass spectrometry. Ensuring medicinal cannabis quality is challenging and this work adds an innovative tool that should prove useful in the context of counterfeit drugs tracking.
Centre Interdisciplinaire de Recherche sur le Médicament - CIRM
FEDER Projet PHARE ; Région wallone Projet Vibra4Fake ; Fonds Léon Fredericq
Researchers ; Professionals
http://hdl.handle.net/2268/227217

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