Person: Calvo Garrido, María Lourdes
Loading...
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
7 results
Search Results
Now showing 1 - 7 of 7
Item Modelling and Scaling-Up of a Supercritical Fluid Extraction of Emulsions Process(Processes, 2023) Tirado, Diego ; Cabañas Poveda, Albertina; Calvo Garrido, María LourdesSupercritical 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.Item 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 LourdesThe 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.Item 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 LourdesThis 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.Item 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.Item Inactivation of clostridium spores in honey with supercritical CO2 and in combination with essential oils(Processes, 2022) Dacal-Gutiérrez, Alejandro; Tirado, Diego ; Calvo Garrido, María LourdesThe 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 (<0.4% mass) improved the inactivation degree, with a 1.3-log reduction achieved at 60 °C. With this same mixture, a reduction of 3.7 logs was accomplished in a derivative with 70% moisture. Honey was very sensitive to the temperature of the applied CO2. The obtained product could be used as a novel food, food ingredient, cosmetic, or medicine.Item Modelling and scaling-up of a supercritical fluid extraction of emulsion process(Processes, 2023) Tirado, Diego ; Cabañas Poveda, Albertina; Calvo Garrido, María LourdesSupercritical 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.