High-pressure phase equilibria of the pseudo-ternary system carbon dioxide + ethanol + fish oil

Ponencia presentada en: 16th European Meeting on Supercritical Fluids, 25 a 28 de abril de 2017, LisboaThis work provides experimental phase equilibrium data of the pseudo-ternary system CO2 + ethanol + fish oil, a system of interest in pharmaceutical and food-industry applications such as the enzymatic production of fatty acid ethyl esters at mild, non-oxidative conditions. Measurements were carried out in a high-pressure variable-volume view cell in the temperature range 323.15-343.15 K and at pressures from 10 to 30 MPa. The Peng-Robinson equation of state was used to satisfactorily correlate experimental data.European Regional Development Fund (ERDF), Spanish Government (MINECO) and Junta de Castilla y León for financial support (projects CTQ2012-39131-C02-01 and BU055U16). RM acknowledges MINECO (BES-2013-063937

Phase behaviour of the pseudo-ternary system carbon dioxide + ethanol + fish oil at high pressures

This work provides experimental fluid phase equilibrium data of the pseudo-ternary mixture CO2 + ethanol + fish oil, a system of interest in pharmaceutical and food-industry applications such as the production of omega-3-enriched lipid derivatives at mild, non-oxidative conditions. Experimental tie-lines were obtained by means of an analytical isothermal method with recirculation of the vapour phase. Measurements were carried out in the temperature range 323.15 K–343.15 K and at pressures from 10 MPa to 30 MPa. The Peng-Robinson equation of state coupled with the conventional van der Waals mixing rules with two adjustable parameters was used for experimental data correlation.Spanish Government through MINECO and Junta de Castilla y León for financial support of the projects CTQ2012-39131-C02-01 and BU055U16, respectively, 16 both co-financed by the European Regional Development Fund (ERDF

High pressure carbon dioxide technology: application to orange juice

Ponencia presentada en: 16th European Meeting on Supercritical Fluids, 25 a 28 de abril de 2017, LisboaHigh pressure carbon dioxide (HPCD) treatment has been applied to orange juice as alternative non-thermal treatment. Kinetics inactivation for pectin methyl esterase has been determined at different operating conditions. PME residual activity was correlated succesfully to the two-fraction model. Some quality parameters such as colour, pH, calcium content, turbidity and particle size distribution (PSD) were also determined right after HPCD treatment. PSD shows that HPCD treatment results in a homogenization effect with a volume increase of small particles and a volume decrease of large particles regarding the non-treated orange juice.MINECO (CTQ2015-64396-R). R. Melgosa acknowledges MINECO for a grant (BES-2013-063937).Spanish Government through MINECO (CTQ2015-64396-R). R. Melgosa acknowledges MINECO for a grant (BES-2013-063937

Bioactive Compounds of a Wheat Bran Oily Extract Obtained with Supercritical Carbon Dioxide

Producción CientíficaA wheat bran oily extract obtained with supercritical carbon dioxide at 25.0 ± 0.1 MPa and 40 ± 2 °C has been analyzed in order to determine some valuable bioactive compounds as alkylresorcinols, α-linolenic acid, steryl ferulates, tocopherols and phenolic compounds, which levels were around 47, 37, 18, 7 and 0.025 mg/g oily extract, respectively. To our knowledge, this is the first time that the presence of steryl ferulates has been observed in a supercritical fluid extract of wheat bran and that γ-tocopherol has been described in wheat bran oily extracts. Other common quality parameters, directly correlated with oxidative degradation, were also evaluated. Acidity values around 15% oleic acid were detected, while low levels of hydroperoxides (around 2.4 meq O2/kg) and very low levels of hexanal (0.21 ppb) were found. Composition of the wheat bran oily extract was stable during 155 days of storage at 21 °C and darkness, and only a slight decrease in alkylresorcinols and tocopherols contents (13% and 20%, respectively) was observed. These results indicated an attractive potential of the obtained oily extract for industrial applications as food ingredients, nutraceuticals, and others.HASENOSA grant (ITC-20113029)Junta de Castilla y León (JCyL) y el Fondo Europeo de Desarrollo Regional (FEDER) grant (BU301P18

Impact of microwave radiation on in vitro starch digestibility, structural and thermal properties of rice flour: From dry to wet treatments

Producción CientíficaMicrowave radiation (MW) is an environment-friendly technology used to physically modify flours. Rice flour was MW-treated at different moisture content (MC) (3 %, 8 %, 13 %, 15 %, 20 % and 30 %). In vitro starch digestibility was determined and related to the changes caused by MW treatment to flours' structure and thermal properties, which were influenced by MC. A reduction of 49 % and 65 % in the gelatinization enthalpy of samples treated at 20 % and 30 % MC denoted a partial gelatinization. A loss of granular crystallinity in treated samples was confirmed by XR-diffraction and FTIR, particularly at 15 %, 20 % and 30 % MC. MW promoted the formation of random-coil, α-helix and β-turn protein structure, and the disappearance of LF-β-sheet. Morphological differences were found between samples treated at 8 % MC (loss of polygonal structure, protein layer covering granules' surface and small holes) and 30 % MC (rounded and aggregated granules, covered with exudate amylose). In vitro starch digestibility revealed that samples treated at 20 % and 30 % MC showed 40 % and 47 % higher rapidly digestible starch, 48 % and 70 % lower slowly digestible starch and 90 % lower resistant starch than the untreated flour. Flour MC in MW-treatment allowed the modulation of structural and thermal characteristics of rice flour and consequently its starch hydrolysis rate.Ministerio de Ciencia e Innovación (PID2019-110809RB-I00)Junta de Castilla y León/ FEDER (VA195P20)National Science Centre (NCN Poland) and Norway Grants (UMO-2020/ 37/KST5/03602

Production and concentration of monoacylglycerols rich in omega-3 polyunsaturated fatty acids by enzymatic glycerolysis and molecular distillation

Production of monoacylglycerols (MAGs) rich in x-3 polyunsaturated fatty acids (n-3 PUFAs) was conducted through short path distillation (SPD) of an acylglycerol mixture (containing 67% MAGs) produced by enzymatic glycerolysis of sardine oil with glycerol. A stepwise SPD process in a UIC KDL 5 system (vacuum 10 3 mbar, feeding flow 1.0 mL/min) was proceeded: the first distillation performed at evaporator temperature (TE) of 110 C to remove glycerol completely and most of FFAs; and the second distillation at optimized TE 155 C; resulting in a stream distillate with 91% purity and 94% overall recovery of MAGs. This work also demonstrated that SPD is able to concentrate n-3 PUFAs in MAG form by distilling at proper TE e.g. 125 C, where n-3 PUFAs are concentrated in the residues. Moreover, this work mapped out a complete processing diagram for scalable production of n-3 PUFAs enriched MAGs as potential food emulsifier and ingredient.Spanish Government through MINECO and the European Regional Development Fund (ERDF) for financial support to the project CTQ2012-39131-C02-01

Productos naturales en la prevención y tratamiento del Síndrome Metabólico

El término “Síndrome Metabólico” (SM) se utiliza para definir una combinación de patologías en una misma persona (diabetes tipo 2, obesidad, dislipemia, hipertensión arterial). Existen diferentes criterios para definir este síndrome, utilizándose en España el del US National Cholesterol Education Program. Los objetivos de este trabajo fueron conocer los criterios de definición, y recopilar las alternativas terapéuticas naturales para la prevención y tratamiento del SM. Se realizó una revisión bibliográfica de artículos científicos sobre el SM así como sobre plantas o productos naturales para su tratamiento o prevención, obtenidos de diversas bases científicas. Se ha constatado que existen alternativas naturales eficaces junto al tratamiento farmacológico convencional para el SM, pero ninguna terapia es efectiva si no va acompañada de una serie de cambios en el estilo de vida

Glicerolisis de aceite de sardina catalizada por una lipasa dependiente de agua en diferentes tert-alcoholes como medio de reacción

The production of monoacylglycerol rich in polyunsaturated fatty acids (PUFA) via enzymatic glycerolysis of sardine oil in a homogeneous system was evaluated. Reactions were conducted in two different tert-alcohols. Based on the phase equilibrium data, the amount of solvent added to create a homogeneous system has been calculated and optimized. The immobilized lipase used in this work was Lipozyme RM IM from Rhizomucor miehei, a water dependent lipase. The amount of water added as well as other reaction parameters were studied to evaluate the optimum conditions for monoacylglycerol obtencion. An initial reactant mole ratio glycerol to sardine oil 3:1, 12 wt% of water based on glycerol content and 10 wt% of lipase loading (based on weight of reactants), achieved a MAG yield of around 70%, with nearly 28 wt% PUFA, with low free fatty acid content (lower than 18 wt%).En este trabajo se ha estudiado la producción de monoacilglicéridos, ricos en ácidos grasos poliinsaturados (AGPI), mediante glicerolisis enzimática de aceite de sardina. La reacción se ha llevado a cabo en dos tert-alcoholes para conseguir de esta forma un medio homogéneo de reacción. La cantidad de disolvente añadida al medio de reacción se ha optimizado y calculado en base al equilibrio de fases de los componentes del sistema. La lipasa empleada como biocatalizador ha sido la enzima inmovilizada Lipozyme RM IM de Rhizomucor miehei, una lipasa dependiente de agua. Se ha estudiado el efecto de distintos parámetros cinéticos, así como de la cantidad de agua añadida al medio de reacción, en la producción de monoacilglicéridos. De los resultados obtenidos, se puede concluir que, para una relación molar inicial de reactantes glicerol:aceite de sardina de 3:1, un 12 % en peso de agua en base al glicerol y un 10 % en peso de lipasa, en base al peso de reactantes; se puede llegar a conseguir un rendimiento en monoacilglicéridos alrededor del 70 % en peso, con casi un 28 % en peso de AGPI y un bajo contenido en ácidos grasos libres (menor del 18 % en peso).Spanish Government through MINECO and the European Regional Development Fund (ERDF) for financial support to the project CTQ2012-39131-C02-01. They wish to thank Novozymes A/S for kindly supplying the enzymes. RM acknowledges MINECO for an FPI grant (reference BES-2013-063937)

Green determination of brominated flame retardants and organochloride pollutants in fish oils by vortex assisted liquid-liquid microextraction and gas chromatography-tandem mass spectrometry

A "green", simple, and low-cost sample extraction procedure involving the use of a deep eutectic solvent (DES) in a vortex assisted liquid-liquid microextraction (VALLME) technique followed by gas chromatography-tandem mass spectrometry (GC-MS/MS) analysis was developed for the simultaneous determination of different PBDEs congeners and OCPs residues in fish oils. After evaluation of different eutectic mixtures, the extraction parameters (volume of DES, amount of oil sample and extraction time) were optimized by means of experimental design in order to maximise extraction efficiency. The developed method was validated in terms of linearity, accuracy and precision, presenting limits of detection in the low ng g−1 level. Its application in the analysis of five fish oil samples, allowed the detection of all the target analytes at levels up 21.5 ng g−1. Fish oils used in animal feed showed to be more contaminated than fish oils for human consumption.Sara C. Cunha and José O. Fernandes thanks REQUIMTE, FCT Fundação para a Ciência e a Tecnologia) and FEDER through the project UID/ QUI/50006/2013 - POCI/01/0145/FEDER/007265 with financial support from FCT/MEC through national funds and co-financed by FEDER, under the Partnership Agreement PT2020. Sara C. Cunha acknowledges FCT for IF/01616/2015 contract. Angela G. Solaesa acknowledges University of Burgos for her pre-doctoral contract and Iberoamerican Santander Research Grant (2017) for the mobility financial support. Thanks to European Regional Development Fund (ERDF) and Junta de Castilla y León for financial support of project BU055U16

Enzymatic activity and conformational and morphological studies of four commercial lipases treated with supercritical carbon dioxide

This work investigates the effect of supercritical carbon dioxide (SC-CO2) treatment on four commer-cial lipases. The influence of experimental conditions: temperature (35–70◦C), pressure (10–25 MPa),exposure time (1–3 h) and depressurization steps (1–3) on the residual activity was studied. Activityenhancement was verified for free enzymes (Palatase 20000 L and Lipozyme CALB L) treated at mildconditions; while the highest temperature and pressure and the longest exposure time assayed led toactivity losses. On the other hand, activity losses or no significative effect of the treatment in the enzymeactivity were observed on immobilized enzymes (Lipozyme RM IM and Lipozyme 435). Qualitative stud-ies were also performed: Fluorescence emission spectra showed changes in the conformational structureof both two free enzymes after SC-CO2treatment. Scanning electron micrographs showed morphologicalalterations in the immobilization supports of the treated enzymes; while infrared spectra did not showchemical modifications.(MINECO) and the EuropeanRegional Development Fund (ERDF) for financial support to theproject CTQ2012-39131-C02-01