Person: Calvo Garrido, María Lourdes
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First Name
María Lourdes
Last Name
Calvo Garrido
Affiliation
Universidad Complutense de Madrid
Faculty / Institute
Ciencias Químicas
Department
Ingeniería Química y de Materiales
Area
Ingeniería Química
Identifiers
10 results
Search Results
Now showing 1 - 10 of 10
Item The Selective Supercritical Extraction of High-value Fatty Acids from Tetraselmis suecica using the Hansen Solubility Theory(Chemical engineering transactions, 2019) Calvo Garrido, Lourdes; Tirado Armesto, Diego Felipe; Rousset, Amandine; Calvo Garrido, María LourdesThe aim of this work was to test the utility of the Hansen theory to predict the best cosolvent for supercritical carbon dioxide (sc-CO2) to reach the selective extraction of fatty acids from Tetraselmis suecica. The order in the cosolvent power was established with five organic solvents used in food production: acetone, diethyl ether, ethanol, n-hexane and methanol. Predictions focused on the selective extraction of oleic, linoleic and αlinolenic acid. The cosolvent power depended on the fatty acid, but in general, the best cosolvent for the three target compounds was ethanol. Predictions were validated through equilibrium data and extraction yields from T. suecica. Operating at 305.15 K and 20 MPa, the extracted oil with the sc-CO2-ethanol (5 % mass fraction) mixture significantly improved the content of the target fatty acids compared with pure sc-CO2; e.g. the αlinolenic acid content was 16 % in the oil obtained with pure sc-CO2 while it was 25 % in the oil obtained with sc-CO2 + 5 % ethanol. However, the Hansen theory predicted that the miscibility enhancement of the fatty acids caused by increasing ethanol concentrations in the supercritical solvent mixture was not progressive. In fact, at high pressures and high ethanol concentrations, it was predicted up to less than half the miscibility enhancement.Item A selective extraction of hydroxytyrosol rich olive oil from alperujo(Journal of Food Engineering, 2019) Calvo Garrido, Lourdes; Tirado Armesto, Diego Felipe; Fuente, Esther de la; Calvo Garrido, María LourdesAlperujo, the solid-liquid waste generated by the current two-phase method of olive oil extraction, was dried, milled and treated with supercritical carbon dioxide (sc-CO2) to obtain a hydroxytyrosol (HT)-rich oil. At first, extraction rates were analysed as a function of operating variables and the pre-condition of the raw material. Samples with particle size diameter<0.80mm and in equilibrium moisture (1%) with the atmosphere, improved oil extraction yield almost 40% compared with samples with the whole range of particle sizes. Extraction yield improved with solvent flow rate, but a minimum residence time was required. The optimum was 0.18 kg h−1 (7.5 kg CO2 h−1 kg biomass−1). Higher pressures and lower temperatures resulted in higher extraction yields; at 30 MPa and 323 K the extraction curve slope was close to the theoretical oil solubility and the yield was 13%, like that obtained with n-hexane by Soxhlet (14%). However, the HPLC-DAD analysis identified higher HT concentration (1900 ppm) in the supercritical extracts at the highest temperature. Consequently, at 373 K, the total phenol content and the antioxidant capacity of the extracts was uppermost. No HT was found in the n-hexane extracts.Item The Hansen theory to choose the best cosolvent for supercritical CO2 extraction of β-carotene from Dunaliella salina(The Journal of Supercritical Fluids, 2019) Tirado Armesto, Diego Felipe; Calvo Garrido, María LourdesThe Hansen solubility theory was used to predict the best cosolvent for supercritical carbon dioxide (sc-CO2) to achieve the selective extraction of β-carotene from Dunaliella salina. Among four organic cosolvents, ethanol was predicted to be the best based on minima Ra values. The predictions were validated through equilibrium data and extraction curves from the microalgae. The addition of ethanol reduced the bubble pressures, and therefore increased the solubility of the β-carotene. With 5% mass fraction, at 318.15 K and 20 MPa, the extraction yield was 25 g carotenoids kg microalgae−1, much more than in pure sc-CO2 (6 g).Item Prediction of the best cosolvents to solubilise fatty acids in supercritical CO2 using the Hansen solubility theory(Chemical Engineering Science, 2018) Tirado Armesto, Diego Felipe; Tenorio, María José; Cabañas Poveda, Albertina; Calvo Garrido, María LourdesCosolvents are employed to improve the extraction efficiency and modify the selectivity of the main solvent. However, choosing a proper cosolvent in supercritical extraction is an arduous task. This study aimed to predict the best cosolvents for the supercritical CO2 extraction of oleic and linoleic acids using the Hansen solubility theory. Calculations were performed for eight organic cosolvents used in food and pharmaceutical production. The best cosolvents for the solubilization of both fatty acids were short-chain alcohols, ethanol and methanol. The predictions were validated with bubble pressures of the mixtures with a 0.003 fatty acid molar fraction at temperatures of 313.2 K and 323.2 K. The experimental results agreed with the predictions. The effect of pressure was well predicted via the direct relationship between pressure and the solvent density. However, the impact of temperature was not properly foreseen because the variation of solute vapour pressure was not considered. The Hansen theory predicted that the miscibility enhancement of the solute in the supercritical mixture is maximum at low pressures and low cosolvent concentrations, as was experimentally confirmed.Item Sterilization of Biological Weapons in Technical Clothing and Sensitive Material by High-Pressure CO2 and Water(Industrial & Engineering Chemistry Research, 2018) Calvo Garrido, Lourdes; Casas Huertas, Javier; Calvo Garrido, María LourdesThis work explores the effectiveness of highpressure CO2 on inactivation of Bacillus thuringiensis spores as a surrogate of B. anthracis spores (anthrax). The investigation was done in combatant equipment and several electronic devices. It was possible to sterilize this sensitive material by the environmentally friendly mixture formed by high-pressure CO2 and water. The presence of water in mass proportions ranging from 20 to 30% relative to the material was essential. However, it was continuously introduced in small amounts (<4% in relation to CO2), entrained by the CO2, so as not to have an adverse impact on materials. A low external pH enhanced the inactivation. Therefore, by using CO2 mixed with water acidified with citric acid to 3.3, the spores were killed at only 45 °C. The much less aggressive conditions of the treatment allowed preservation of the quality of the technical fabrics and the functionality of the electronic devices.- Project number: 242
Item Laboratorio integrado de prácticas de simulación de fundamentos y procesos químicos con fluidos supercríticos(2019) Calvo Garrido, Lourdes; Cabañas Poveda, Albertina; Pando García-Pumarino, Concepción; García Baonza, Valentín; González Mac-Dowell, Luis; Tirado Armesto, Diego Felipe; Cuadra Mendoza, Isaac Alfonso; Menéndez Carbajosa, Alicia Marta; Calvo Garrido, María LourdesEl objetivo del proyecto ha sido crear un laboratorio integrado de prácticas de simulación relacionadas con fundamentos termodinámicos y procesos con fluidos supercríticos, destinado a los alumnos de Química e Ingeniería Química. Item The parameters that affect the supercritical extraction OF 2,4,6- trichloroanisol from cork(Journal of Supercritical Fluids, 2018) Viguera Sáenz, Miguel; Prieto, C.; Casas, E.; Cabañas Poveda, Albertina; Calvo Garrido, Lourdes; Calvo Garrido, María LourdesThe contamination of wine by 2,4,6-trichloroanisol (TCA) derived from the cork stopper is a huge problem for the wine industry. This work shows the results of TCA extraction using supercritical CO2. Cork granules (6% moisture) were placed forming a fixed bed within a high-pressure vessel. The CO2 was made to continuously flow over this. The TCA removal was compared at different operating conditions (pressure, temperature, flow rate or extraction time). TCA removal was not possible in dried cork. Density had a positive impact in TCA removal due to the solvent capacity increase. An increase in the supercritical fluid temperature over 60 °C impaired the TCA extraction. High residence times benefited the extraction. At high CO2 density of 585 kg m−3 , TCA elimination below the detection level was achieved in 8 min residence time. This required relatively low solvent to cork mass ratios (43 kg CO2 kg−1 ).Item Teaching supercritical fluid fractionation using Aspen-Plus(Nuevos desafíos en la enseñanza superior, 2018) Prieto, Cristina; Calvo Garrido, María Lourdes; Calvo Garrido, María Lourdes; Membiela, Pedro ; Casado, Natalia; Cebreiros, María Isabel; Vida, ManuelItem Astaxanthin encapsulation in ethyl cellulose carriers by continuous supercritical emulsions extraction: A study on particle size, encapsulation efficiency, release profile and antioxidant activity(Journal of Supercritical Fluids, 2019) Tirado, Diego ; Palazzo, Ida; Scognamiglio, Mariarosa; Calvo Garrido, María Lourdes; Della Porta, Giovanna; Reverchon, ErnestoSupercritical emulsions extraction (SEE)technology was used to encapsulate astaxanthin (AXT)in ethyl cellulose (EC). The operating parameters were 8 MPa and 311 K with an L/G ratio of 0.1 (CO2 flow rate of 1.4 kg/h). Several emulsion formulations were tested, fixing the oil-water ratio at 20:80 (ethyl acetate/water)and varying EC concentration in the oily phase from 1.0–2.5% mass and the surfactant amount in the water phase from 0.1 to 0.6% mass. Both parameters influenced carriers morphology, size and distribution; a correlation between the EC amount in oily phase and its dynamic viscosity was proposed to explain the droplets/carriers size variation observed. Carriers aggregation was monitored at surfactant concentration higher than 0.3% mass. The best emulsion formulation was obtained using 1.0% mass of EC in the oily phase and 0.1% mass of surfactant in the water phase; in these conditions spherical nanocarriers with unwrinkled and smooth surface were obtained with a size of 242 nm and Poly Dispersity Index of 0.16. EC mass recovery was of 90%. Higher carrier mean size of 363 nm (Poly Disperity Index of 0.31)was measured when AXT was encapsulated in the same conditions, achieving an encapsulation efficiency of 84%. The carriers were loaded with 21 mg/g of AXT and showed an excellent antioxidant capacity, measured as Trolox equivalent (Trolox equivalent per kg of pure AXT), and equivalent to 3900 M Trolox. In vitro release profiles obtained in a simulated intestinal fluid (SIF)at pH 7.2 and 310 K, showed a release of 70% of the total encapsulated AXT after 10 h.Item The Selective Supercritical Extraction of High-value Fatty Acids from Tetraselmis suecica using the Hansen Solubility Theory(Chemical Engineering Transactions, 2019) Tirado, Diego ; Rousset, Amandine; Calvo Garrido, María LourdesThe aim of this work was to test the utility of the Hansen theory to predict the best cosolvent for supercritical carbon dioxide (sc-CO2) to reach the selective extraction of fatty acids from Tetraselmis suecica. The order in the cosolvent power was established with five organic solvents used in food production: acetone, diethyl ether, ethanol, n-hexane and methanol. Predictions focused on the selective extraction of oleic, linoleic and α-linolenic acid. The cosolvent power depended on the fatty acid, but in general, the best cosolvent for the three target compounds was ethanol. Predictions were validated through equilibrium data and extraction yields from T. suecica. Operating at 305.15 K and 20 MPa, the extracted oil with the sc-CO2-ethanol (5 % mass fraction) mixture significantly improved the content of the target fatty acids compared with pure sc-CO2; e.g. the α-linolenic acid content was 16 % in the oil obtained with pure sc-CO2 while it was 25 % in the oil obtained with sc-CO2 + 5 % ethanol. However, the Hansen theory predicted that the miscibility enhancement of the fatty acids caused by increasing ethanol concentrations in the supercritical solvent mixture was not progressive. In fact, at high pressures and high ethanol concentrations, it was predicted up to less than half the miscibility enhancement.