Silymarin extraction using gas expanded liquids

Trabajo presentado a la 2nd European Sample Preparation Conference (EuSP), celebrada en Grecia del 14 al 16 de marzo de 2022.Peer reviewe

Gas-Expanded Liquids Extraction

Gas Expanded Liquids (GXL) are mixtures of liquid solvents (organic, water) and gases or supercritical fluids with diverse physicochemical properties halfway between pure liquids and supercritical fluids. The possibility of changing their properties by introducing small changes in pressure, temperature, and/or solvent/gas ratio, makes these solvents a very interesting and appropriate option for developing green extraction protocols for food analysis. In general, GXLs have similar densities as the solvent used in their composition, while having improved mass transfer through reduced viscosity, increased solute diffusivity, and decreased interfacial tension. Some other advantages are related to the wide range of polarities that can be obtained, depending on the liquid selected. Moreover, the substitution of a liquid fraction for a gas reduces the final use of organic solvent, thus improving the green character of GXLs. In the present chapter, the physicochemical properties of GXL are addressed along together with the description of applications in the food science and technology area.Peer reviewe

Optimization of pressurized liquid extraction and in vitro neuroprotective evaluation of Ammodaucus ieucotrichus. Untargeted metabolomics analysis by UHPLC-MS/MS

This article belongs to the Special Issue Analytical Methods for Characterization and Isolation of Natural Products.Ammodaucus leucotrichus is a spontaneous plant endemic of the North African region. An efficient selective pressurized liquid extraction (PLE) method was optimized to concentrate neuroprotective extracts from A. leucotrichus fruits. Green solvents were tested, namely ethanol and water, within a range of temperatures between 40 to 180 °C. Total carbohydrates and total phenolics were measured in extracts, as well as in vitro antioxidant capacity (DPPH radical scavenging), anticholinesterase (AChE) and anti-inflammatory (LOX) activities. Metabolite profiling was carried out by ultra-high-performance liquid chromatography coupled to quadrupole time-of-flight tandem mass spectrometry (UHPLC-ESI-q-TOF-MS/MS), identifying 94 compounds. Multivariate analysis was performed to correlate composition with bioactivity. A remarkable effect of the temperature using water was observed: the higher temperature, the higher extraction yield, the higher total phenolic content, as well as the higher total carbohydrates content. The water extract obtained at 180 °C, 10.34 MPa and 10 min showed meaningful anti-inflammatory (IC50LOX = 39.4 µg/mL) and neuroprotective activities (IC50AChE = 55.6 µg/mL). The Principal Components Analysis (PCA) and the cluster analysis correlated these activities with the presence of carbohydrates and phenolic compounds.This work has been funded by the project AGL2017-89417-R and (Spanish Ministry of Science and Innovation).Peer reviewe

Silymarin extraction for Silybum marinuim seeds using pressurized liquid extraction as a green and efficient technology

Resumen del trabajo presentado al Green Chemistry Postgraduate Summer School, celebrado en Venecia (Italia) del 4 al 9 de julio de 2021.Peer reviewe

Extraction of bioactives compounds from Silybum marianum using gas expanded liquid extraction

Resumen del póster presentado al 23rd International Symposium on Advances in Extraction Technologies (ExTech), celebrado on-line del 30 de junio al 2 de julio de 2021.For over then 2000 years, Milk thistle has been used as one of the most important medicinal plant as a remedy for liver disease. It has also been reported to have anti-tumor, anti-aging, antidiabetic, cardioprotective and neuroprotective effects. In 2019, milk thistle seed products placed in the 10th and 23rd in U.S. natural channel and U.S. mainstream multi‐outlet sales with more than $26 million. The aim of numerous studies has been to improve novel and efficient extraction techniques to produce high-quality extracts respecting the Green Chemistry Concepts. Among them, Gas-Expanded Liquids (GXLs) are the mixture between liquid solvents and pressurized compressible gas such us CO2. Thus, the objective of this work was to develop and evaluate the CO2 –expanded liquids (CXLs) as a new and green promising method for the extraction of bioactives such as Silymarin from Silybum marianum. Extraction solvent consisted on mixtures of CO 2 -Ethanol-water under different conditions, besides kinetic study was evaluated. The best yield reached 55.97% using a ternary mixture of solvents composed by Ethanol:CO2:H2O (60:25:15) at 40C° and 90bar in 160min. Moreover, the extracts obtained have been chemically and functionally characterized. HPLC-ESI-MS/MS (triple quadrupole) and invitro assays such as the anti-inflammatory and anti-cholinergic activities respectively.This work has been funded by the project AGL2017-89417-R (Spanish Ministry of Science and Innovation).Peer reviewe

One-step sustainable extraction of Silymarin compounds of wild Algerian milk thistle (Silybum marianum) seeds using Gas Expanded Liquids

This work was financially supported by the projects PDC2021-120814-I00 funded by MCIN/AEI/ 10.13039/501100011033 (Spanish Ministry of Science and Innovation) and by Projects 202170E057 (Bioprospección de plantas endémicas de Argelia mediante tecnologías de extracción sostenibles) and INCGLO0019 (Bioprospección de recursos agrícolas locales, una vía para alcanzar los Objetivos de Desarrollo Sostenible) both funded by CSIC. N. Abderrezag gratefully acknowledges the University of Salah Boubnider Constantine3 (Algeria) for financial support.This work was financially supported by the projects PDC2021-120814-I00 funded by MCIN/AEI/ 10.13039/501100011033 (Spanish Ministry of Science and Innovation) and by Projects 202170E057 (Bioprospección de plantas endémicas de Argelia mediante tecnologías de extracción sostenibles) and INCGLO0019 (Bioprospección de recursos agrícolas locales, una vía para alcanzar los Objetivos de Desarrollo Sostenible) both funded by CSIC. N. Abderrezag gratefully acknowledges the University of Salah Boubnider Constantine3 (Algeria) for financial support.Peer reviewe

Bioprospecting neuroprotective extracts from Algerian plants using green compressed fluid extractions

Resumen del póster presentado al 2º Iberian Meeting on Supercritical Fluids (2º Encuentro Ibérico de Fluidos Supercríticos/2º Encontro Ibérico de Fluidos Supercríticos - EIFS), held in Coimbra – Portugal, on 28 February- 2 March 2022.This work has been funded by the projects PID2020-113050RB-I00, PDC2021-120814-I00 and EQC2021-007112-P funded by MCIN/AEI /10.13039/501100011033 and The European Union Next GenerationEU/ PRTR respectively. N. Abderrezag are grateful to the Salah Boubnider Constantine 3 university, Constantine, Algeria for the fellowship.Peer reviewe