The analysis of cannabinoids in cannabis samples bysupercritical fluid chromatography and ultra-high-performanceliquid chromatography: A comparison study
[en] The aim of this work was to develop a supercritical fluid chromatographic method to study the applicability of this emerging technique to cannabinoid analysis and showcase its advantages. During method development, the authors focused on nine phyto-cannabinoids to assess the selectivity needed to potentially perform the quantitation of each cannabinoid. After method development, robustness studies were carried out on this method to gain more information about its qualitative behaviour (in terms of critical resolutions) when varying some crucial parameters (concentration of additive, column temperature, starting gradient conditions and column batch). Once the robustness was evaluated and the parameters most affecting the selected responses were individuated, the SFC method was applied for a simulated routine use to generate quantitative results concerning the concentrations of the main cannabinoids in real cannabis samples. The samples were also analyzed by means of an ultra-high-performance liquid chromatographic method currently used in the laboratory for the same objective. Finally, the results obtained with both analytical methods were compared to evaluate their accordance. The Bland-Altman method was applied as a statistical strategy to evaluate the degree of accordance between the results generated and display the data in a difference plot. The UHPSFC quantitative results were in accordance with the UHPLC results, demonstrating the applicability of this technique for cannabinoid analysis.
Research center :
CIRM - Centre Interdisciplinaire de Recherche sur le Médicament - ULiège
Disciplines :
Human health sciences: Multidisciplinary, general & others
Author, co-author :
Deidda, Riccardo ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Schelling, Cédric; Université de Genève - UNIGE > School of Pharmaceutical Sciences
Roussel, Jean-Marc; Mâcon, France > Consultant
Dispas, Amandine ; Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
De Bleye, Charlotte ; Université de Liège - ULiège > Département de pharmacie > Département de pharmacie
Ziemons, Eric ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Hubert, Philippe ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Veuthey, Jean-Luc; Université de Genève - UNIGE > School of Pharmaceutical Sciences
Language :
English
Title :
The analysis of cannabinoids in cannabis samples bysupercritical fluid chromatography and ultra-high-performanceliquid chromatography: A comparison study
Publication date :
26 November 2020
Journal title :
Analytical Science Advances
eISSN :
2628-5452
Publisher :
Wiley-VCH
Special issue title :
SUPERCRITICAL FLUIDS
Pages :
1-13
Peer reviewed :
Peer Reviewed verified by ORBi
Funders :
Fonds Léon Fredericq [BE] Walloon region [BE] CE - Commission Européenne [BE]
Whiting PF, Wikff RF, Deshpande S, et al. Cannabinoids for medical use: a systematic review and meta-analysis. JAMA. 2015;313(24):2456-2473.
UNODC. Recommended Methods for the Identification and Analysis of Cannabis and Cannabis Products. New York, NY: UNODC; 2009. https://www.unodc.org/documents/scientific/ST-NAR-40-Ebook_1.pdf. Accessed July 10, 2020.
Citti C, Braghiroli D, Vandelli MA, Cannazza G. Pharmaceutical and biomedical analysis of cannabinoids: a critical review. J Pharm Biomed Anal. 2018;147:565-579.
Andre CM, Hausman JF, Guerriero G. Cannabis sativa: the plant of the thousand and one molecules. Front Plant Sci. 2016;7:19. 10.3389%2Ffpls.2016.00019.
Fischedick JT, Hazekamp A, Erkelens T, Choi YH, Verpoorte R. Metabolic fingerprinting of Cannabis sativa L., cannabinoids and terpenoids for chemotaxonomic and drug standardization purposes. Phytochemistry. 2010;71:2058-2073.
Brenneisen R. Chemistry and analysis of phytocannabinoids and other cannabis constituents. In: ElSohly M, ed.Marijuana and the Cannabinoids Forensic Science and Medicine. New York: Humana Press; 2006:17-49.
Burstein S. Cannabidiol (CBD) and its analogs: a review of their effects on inflammation. Bioorg Med Chem. 2015;23(7):1377-1385.
Corroon J, Phillips JA. A cross-sectional study of cannabidiol users. Cannabis Cannabinoid Res. 2018;3(1):152-161.
Hädener M, König S, Weinmann W. Quantitative determination of CBD and THC and their acid precursors in confiscated cannabis samples by HPLC-DAD. Forensic Sci Int. 2019;299:142-150.
Pavlovic R, Nenna G, Calvi L, et al. Quality traits of “cannabidiol oils”: cannabinoids content, terpene fingerprint and oxidation stability of European commercially available preparations. Molecules. 2018;23(5):1230-1251.
Zivovinovic S, Alder R, Allenspach MD, Steuer C. Determination of cannabinoids in Cannabis sativa L. samples for recreational, medical, and forensic purposes by reversed-phase liquid chromatography-ultraviolet detection. J Anal Sci Technol. 2018;9:27.
Leghissa A, Hildenbrand ZL, Schug KA. A review of methods for the chemical characterization of cannabis natural products. J Sep Sci. 2018;41(1):398-415.
Giese MW, Lewis MA, Giese L, Smith KM. Development and validation of a reliable and robust method for the analysis of cannabinoids and terpenes in cannabis. J AOAC Int. 2015;98(6):1503-1522.
Béres T, Černochová L, SĆ Zeljković, et al. Intralaboratory comparison of analytical methods for quantification of major phytocannabinoids. Anal Bioanal Chem. 2019;411(14):3069-3079.
Calvi L, Pentimalli D, Panseri S, et al. Comprehensive quality evaluation of medical Cannabis sativa L. inflorescence and macerated oils based on HS-SPME coupled to GC-MS and LC-HRMS (Q-exactive orbitrap®) approach. J Pharm Biomed Anal. 2018;150:208-219.
Deidda R, Avohou HT, Baronti R, et al. Analytical quality by design: development and control strategy for a LC method to evaluate the cannabinoids content in cannabis olive oil extracts. J Pharm Biomed Anal. 2019;166:326-335.
Fekete S, Sadat-Noorbakhsh V, Schelling C, et al. Implementation of a generic liquid chromatographic method development workflow: application to the analysis of phytocannabinoids and Cannabis sativa extracts. J Pharm Biomed Anal. 2018;155:116-124.
Dispas A, Marini R, Desfontaine V, et al. First inter-laboratory study of a supercritical fluid chromatography method for the determination of pharmaceutical impurities. J Pharm Biomed Anal. 2018;161:414-424.
Wang M, Wang YH, Avula B, et al. Decarboxylation study of acidic cannabinoids: a novel approach using ultra-high-performance supercritical fluid chromatography/photodiode array-mass spectrometry. Cannabis Cannabinoids Res. 2016;1(1):262-271.
Jambo H, Dispas A, Avohou HT, et al. Implementation of a generic SFC-MS method for the quality control of potentially counterfeited medicinal cannabis with synthetic cannabinoids. J Chromatogr B. 2018;1092:332-342.
Miller LM, Pinkston JD, Taylor LT. Analysis of cannabis products by supercritical fluid chromatography. In: Vitha MF, ed. Modern Supercritical Fluid Chromatography Carbon Dioxide Containing Mobile Phases. Hoboken, NJ: John Wiley & Sons, Inc; 2020:77-78.
Deidda R, Orlandini S, Ph Hubert, Hubert C. Risk-based approach for method development in pharmaceutical quality control context: a critical review. J Pharm Biomed Anal. 2018;161:110-121.
ICH Harmonised Tripartite Guideline. Pharmaceutical development Q2(R1). In: International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use 2005. https://www.ema.europa.eu/en/documents/scientific-guideline/ich-q-2-r1-validation-analytical-procedures-text-methodology-step-5_en.pdf. Accessed July 10, 2020.
Borman PJ, Chatfield MJ, Damjanov I, Jackson P. Method ruggedness studies incorporating a risk based approach: a tutorial. Anal Chim Acta. 2011;703(2):101-103.
Losacco GL, Veuthey JL, Guillarme D. Supercritical fluid chromatography – Mass spectrometry: recent evolution and current trends. TrAC, Trend Anal Chem. 2019;118:731-738.
Dispas A, Lebrun P, Ziemons E, Marini R, Rozet E, Ph Hubert. Evaluation of the quantitative performances of supercritical fluid chromatography: from method development to validation. J Chrom A. 2014;1353:78-88.
Miller LM, Pinkston JD, Taylor LT. Detection in packed column SFC. In: Vitha MF, ed. Modern Supercritical Fluid Chromatography Carbon Dioxide Containing Mobile Phases. Hoboken, NJ: John Wiley & Sons, Inc; 2020:77-78.
Bland JM, Altman DG. Statistical methods for assessing agreement between two methods of clinical measurement. Lancet. 1986;1(8476):307-310.
Giavarina D. Understanding Bland Altman analysis. Biochem Med (Zagreb). 2015;25(2):141-151. 10.11613%2FBM.2015.015.