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Dynamical processes and order behind the pronounced 1H NMR paramagnetic relaxation enhancement induced in [P6,6,6,14]3[GdCl6]-based ionic liquid mixtures
Publication . Beira, Maria J.; Silva, Gonçalo M.C.; Eusébio, Tiago M.; Figueirinhas, João L.; Cordeiro, Rui; Cruz, Carlos; Corvo, Marta C.; Almeida, Pedro L.; Rosatella, Andreia A.; Afonso, Carlos A.M.; Filipe, Eduardo J.M.; Parella, Teodor; Cabrita, Eurico J.; Sebastião, Pedro J.; CENIMAT-i3N - Centro de Investigação de Materiais (Lab. Associado I3N); DCM - Departamento de Ciência dos Materiais; Faculdade de Ciências e Tecnologia (FCT); UCIBIO - Applied Molecular Biosciences Unit; DQ - Departamento de Química; Elsevier
NMR relaxometry is a technique that allows the molecular dynamics study of chemical compounds across a broad time scale, ranging from slow translational diffusion or collective motions to fast rotations. The present work is a 1H NMR relaxometry and diffusometry study of systems based on [P6,6,6,14][Cl] and [P6,6,6,14]3[GdCl6] ionic liquids, complemented by X-ray diffractometry measurements. The use of the X-ray profiles enabled the determination of an almost temperature independent interdigitated disposition of the cations that is at the origin of local order fluctuations. This structure also affects the paramagnetic relaxation enhancement, which is very significant for these systems and is achieved at very low metal concentrations (around 1mM). The present study provides a comprehensive analysis that is consistent for all the analyzed systems and across the different experimental techniques, despite the experienced technical challenges related to extremely short relaxation times. Additionally, the Electrochemical Impedance Spectroscopy profiles of the neat [P6,6,6,14][Cl] sample were explained by an analogous equivalent circuit model that allowed for a global analysis consistent with the diffusometry and X-ray diffractometry results. The representation of the real and imaginary parts of the impedance allowed for a visual deconvolution of the contributions of the different circuit blocks considered in the model.
Process Development for GMP-Grade Full Extract Cannabis Oil
Publication . Costa, Maria do Céu; Gomes, Ana Patrícia; Vinhas, Iva; Rosa, Joana; Pereira, Filipe; Moniz, Sara; Gonçalves, Elsa M.; Pestana, Miguel; Silva, Mafalda; Rodrigues, Luís Monteiro; DeMeo, Anthony; Marynissen, Logan; Marques da Costa, António; Rijo, Patrícia; Sassano, Michael; GeoBioTec - Geobiociências, Geoengenharias e Geotecnologias; Faculdade de Ciências e Tecnologia (FCT); MDPI - Multidisciplinary Digital Publishing Institute
Background/Objectives: The industrial extraction and purification processes of Cannabis sativa L. compounds are critical steps in creating formulations with reliable and reproducible therapeutic and sensorial attributes. Methods: For this study, standardized preparations of chemotype I were chemically analyzed, and the sensory attributes were studied to characterize the extraction and purification processes, ensuring the maximum retention of cannabinoids and minimization of other secondary metabolites. The industrial process used deep-cooled ethanol for selective extraction. Results: Taking into consideration that decarboxylation occurs in the process, the cannabinoid profile composition was preserved from the herbal substance to the herbal preparations, with wiped-film distillation under deep vacuum conditions below 0.2 mbar, as a final purification step. The profiles of the terpenes and cannabinoids in crude and purified Full-spectrum Extract Cannabis Oil (FECO) were analyzed at different stages to evaluate compositional changes that occurred throughout processing. Subjective intensity and acceptance ratings were received for taste, color, overall appearance, smell, and mouthfeel of FECO preparations. Conclusions: According to sensory analysis, purified FECO was more accepted than crude FECO, which had a stronger and more polarizing taste, and received higher ratings for color and overall acceptance. In contrast, a full cannabis extract in the market resulted in lower acceptance due to taste imbalance. The purification process effectively removed non-cannabinoids, improving sensory quality while maintaining therapeutic potency. Terpene markers of the flower were remarkably preserved in SOMAÍ’s preparations’ fingerprint, highlighting a major qualitative profile reproducibility and the opportunity for their previous separation and/or controlled reintroduction. The study underscores the importance of monitoring the extraction and purification processes to optimize the cannabinoid content and sensory characteristics in cannabis preparations.
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Fundação para a Ciência e a Tecnologia
Programa de financiamento
Concurso de avaliação no âmbito do Programa Plurianual de Financiamento de Unidades de I&D (2017/2018) - Financiamento Base
Número da atribuição
UIDB/04567/2020