Person:
Calvo Garrido, María Lourdes

First Name

María Lourdes

Last Name

Calvo Garrido

URI

https://hdl.handle.net/20.500.14352/76255

Affiliation

Universidad Complutense de Madrid

Faculty / Institute

Ciencias Químicas

Department

Ingeniería Química y de Materiales

Area

Ingeniería Química

Identifiers

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Search Results

Now showing 1 - 10 of 25

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 Lourdes
The 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.
Project number: 172
Formación en Química Sostenible y su relación con los Objetivos de Desarrollo Sostenible
() Cabañas Poveda, Albertina; Pérez Velilla, Eduardo; Vázquez Villa, Henar; García Melo, Fátima; Calvo Garrido, Lourdes; González Mac-Dowell, Luis; Acción Salas, Fernando; Parrón Nieto, Andrea; Valero Herrero, Patricia; Calvo Garrido, María Lourdes
En el proyecto se propone la realización de trabajos en grupo dirigidos a los alumnos de Química General de 1º en los que se desarrollen los principios de la Química Sostenible y se relacionen con los Objetivos de Desarrollo Sostenible. Las mejores presentaciones serán grabadas en video para su difusión.
Inactivation of Clostridium Spores in Honey with Supercritical CO2 and in Combination with Essential Oils
(Processes, 2022) Dacal Gutierrez, Alejandro; Tirado Armesto, Diego Felipe; Calvo Garrido, Lourdes; Calvo Garrido, María Lourdes
The presence of tens of Clostridium botulinum spores per gram of honey can cause infantile botulism. Thermal treatment is insufficient to inactivate these resistant forms. This study explored the effectiveness of supercritical CO2 (scCO2 ) on its own and combined with lemon (LEO), clove (CLEO), and cinnamon (CEO) essential oils on the inactivation of Clostridium sporogenes (CECT 553) as a surrogate of Clostridium botulinum. In water, the degree of inactivation at 10 MPa after 60 min increased with the increasing temperature, reducing the population by 90% at 40 ◦C and by 99.7% at 80 ◦C. In contrast, when applied to honey, scCO2 did not inactivate Clostridium spores satisfactorily at temperatures below 70 ◦C, which was related to the protective effect of honey. Meanwhile, scCO2 modified with CEO
One-step Sustainable Preparation of Superparamagnetic Iron Oxide Nanoparticles Supported on Mesoporous SiO2
(Journal of Supercritical Fluids, 2020) Chamorro, Elena; Granados García Tenorio, María José; Calvo Garrido, María Lourdes; Torralvo Fernández, María José; Sáez Puche, Regino; Cabañas Poveda, Albertina
Superparamagnetic iron oxide nanoparticles (SPIONs) supported on high surface area mesoporous SiO2 are advanced materials of great interest in catalysis, adsorption and biomedicine. Here we present a new process to prepare SPION/SiO2 materials by the impregnation and insitu decomposition of Fe(NO3)3.9H2O on mesoporous SiO2 supports in a 25-50% mol ethanol + CO2 mixture at 523 K and 25.0 MPa. -Fe2O3 nanoparticles (NPs) of average size between 6-9 nm were distributed homogeneously on the supports. NPs deposited into the SBA-15 mesopores but mostly on the external surface of MCM-41. Materials prepared with the highest ethanol content were very homogeneous. Magnetic measurements confirmed the superparamagnetic nature of the materials at room temperature. The process proposed is sustainable and scalable, avoids tedious preparations and the additional high temperature treatment under a controlled atmosphere, as the metal decomposition is performed insitu in the CO2-expanded liquid mixture.
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 Lourdes
Alperujo, 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.
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 Lourdes
The 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).
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 Lourdes
Cosolvents 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.
Modelling and Scaling-Up of a Supercritical Fluid Extraction of Emulsions Process
(Processes, 2023) Tirado, Diego ; Cabañas Poveda, Albertina; Calvo Garrido, María Lourdes
Supercritical CO2(scCO2) is utilized in the supercritical fluid extraction of emulsions (SFEE) to swiftly extract the organic phase (O) from an O/W emulsion. The dissolved substances in the organic phase precipitate into small particles and remain suspended in the water (W) with the aid of a surfactant. The process can be continuously conducted using a packed column in a counter-current flow of the emulsion and scCO2, at moderate pressure (8–10 MPa) and temperature (37–40 ◦C). To ensure the commercial viability of this technique, the organic solvent must be separated from the CO2 to facilitate the recirculation of both streams within the process while minimizing environmental impact. Thus, the aim of this work was to design a plant to produce submicron materials using SFEE, integrating the recovery of both solvents. First, experimental equilibrium data of the ternary system involved (CO2/ethyl acetate/water) were fitted with a proper thermodynamic model. Then, simulations of the whole integrated process at different scales were carried out using Aspen Plus®, along with economical evaluations. This work proposes the organic solvent separation with a distillation column. Thus, the two solvents can be recovered and recycled to the process in almost their entirety. Furthermore, the particles in the aqueous raffinate are produced free of solvents and sterilized for further safe use. The costs showed an important economy scale-up. This work could ease the transfer of the SFEE technology to the industry.
The encapsulation of hydroxytyrosol-rich olive oil in Eudraguard® protect via supercritical fluid extraction of emulsions
(Journal of Food Engineering, 2021) Tirado, Diego ; Latini, Angela; Calvo Garrido, María Lourdes
The SFEE technology was used to micronize the food-approved-biopolymer Eudraguard® protect. After setting the ratio of emulsion phases to 20:80 ethyl acetate:water, higher surfactant (0.1–10.0%) and lower polymer (1–10%) concentrations reduced the size of the particles. By halving the stirring speed to 1250 rpm during the homogenization of the emulsion, larger particles were formed. All these manipulations allowed the creation of particles ranging from 10 nm to 200 nm. A higher viscosity of the organic phase, achieved with 2% vitamin E, increased the particle size to 300 nm. Afterwards, SFEE was used to encapsulate hydroxytyrosol-rich olive oil (HT-oil), obtained from alperujo, in Eudraguard® protect for its preservation. Spherical non-aggregate particles were formed with an average of 230 nm. High degrees of encapsulation were possible (up to 99%) resulting in loadings of HT-oil in the obtained particles of 39% with 0.7 mg HT per g of particle.
Inactivation of Legionella in aqueous media by high-pressure carbon dioxide
(The Journal of Supercritical Fluids, 2022) Martín-Muñoz, David; Tirado, Diego ; Calvo Garrido, María Lourdes
This work aimed to investigate the inactivation of Legionella in aqueous media using high-pressure carbon di- oxide (HPCD). Both discontinuous and continuous operations were tested. During batch treatments, the increased pressure improved the inactivation of Legionella, probably due to better dispersion and dissolution of the HPCD in the aqueous medium. Inactivation also increased with temperature. After 10 min and 26 ◦C it was not necessary to exceed 20 MPa, where reductions higher than 4.2 log were reached. At 10 MPa, reductions higher than 3.1 log were reached, good enough for real aqueous environments, which rarely exceed 102 CFU mL−1. Total inactivation was reached at 38 ◦C at all pressures. For a given temperature, treatment with HPCD was always much more effective than thermal treatment. During continuous treatments, a contact time of 1 min at 28 ◦C and 10 MPa were enough for the total inactivation of Legionella in co-current flow with a CO2/suspension mass ratio of 1. Simulation with Aspen Plus® revealed that depressurization of the sterile water to remove gaseous CO2 cooled it sufficiently to be used as a cooling service.