Kinetic study of pilot-scale supercritical CO2 extraction of rosemary (Rosmarinus officinalis) leaves

NOTICE: This is the author’s version of a work that was accepted for publication in Journal of Supercritical Fluids. Changes resulting from the publishing process, such as peer review, editing, corrections, structural formatting, and other quality control mechanisms may not be reflected in this document. Changes may have been made to this work since it was submitted for publication. A definitive version was subsequently published in Journal of Supercritical Fluids, 55 (2011). http://dx.doi.org/10.1016/j.supflu.2010.09.030Rosmarinus officinalis (rosemary) extracts were obtained in a supercritical pilot-scale plant. Based on experimental information available in the literature for analytical or low-scale processes, extraction temperature and pressure were selected to be 313 K and 30 MPa. At these extraction conditions, the kinetic behavior of the pilot-scale overall extraction curve were determined with respect to yield, antioxidant activity and carnosic acid content. The overall extraction curve was represented using Sovova’s model; the average deviation between measured and calculated yields was lower than 2%. Mass transfer coefficients in the fluid and solid phases were determined and were compared with previous data reported in the literature for low-scale rosemary supercritical extraction. A two-stage depressurization procedure was accomplished and the effect of both on-line fractionation and extraction time on the antioxidant activity of the samples collected was studied. The antioxidant activity of the different fractions could be straight correlated with the carnosic acid content with a regression coefficient of 0.92This work has been financed by Universidad Autónoma de Madrid and Comunidad Autónoma de Madrid (ALIBIRD-S2009/AGR-1469) and project FUN-C-FOOD, CSD2007-00063 (CONSOLIDER-INGENIO) from Ministerio de Ciencia e Innovación, Spain

The interaction of slaughtering, drying, and defatting methods differently affects oxidative quality of the fat from black soldier fly (Hermetia illucens) larvae

The interrelation effect of slaughtering, drying, and defatting methods of BSFL on the oxidative quality of the derived fat was studied. Blanching and freezing were compared as slaughtering methods, followed by oven or freeze-drying for drying and mechanical pressing or SFE for defatting. The oxidative state and stability of the extracted fat and defatted meals were monitored immediately after their production, using peroxide value (PV) and Rancimat test, and over 24 weeks of storage. Slaughtering and drying methods had an independent effect on PV, with freezing and freeze-drying being the best methods. Mechanical pressing and SFE were comparable and superior to conventional hexane defatting. Interactions were observed between slaughtering and defatting, drying and defatting, and between all three factors. Generally, freeze-drying combined with any of the slaughtering and defatting methods resulted in the lowest PVs, with mechanical pressing being preferred. Freeze-drying plus mechanical pressing also produced the most stable fats during storage according to the evolution of PV, while the combination of blanching and SFE produced the least stable. A significant correlation was found between the PV at 24 weeks and the antioxidant activity of the fats. Contrary to storage assays, in accelerated Rancimat assays, freeze-dried samples were the least stable, which was partially attributed to the significant correlation with the acid values of the samples. Defatted meals followed a similar pattern to the extracted fat, except for worse oxidation for SFE defatting. Therefore, the different processing methods of slaughtering, drying, and defatting of BSFL differently affect lipid oxidation, with interactions between such successive stepsThis research was funded by the Spanish National Plans of Aquaculture of the Ministry of Agriculture, Fisheries and Food, project ACUINSECT (Optimization of insect flours as sustainable ingredient for aquaculture fee

Simulador gastrointestinal dinámico (simgi®): Una herramienta potencialmente útil en nutrición clínica

The human gastrointestinal tract harbours the most complex and abundant community of the human body, the colon being where the highest microbial concentration is found (10 12 cell/g). The intestinal microbiota exerts metabolic, trophic and protective functions which are important in the maintenance of the host health. Over recent decades, numerous studies have attempted to provide scientific evidence about the environmental factors that can impact on human health through the modulation of the intestinal microbiota composition. However, this approach is changing, and a new focus on assessing changes at functional level is being developed. If we apply this dual approach to the role played by the diet, it is obvious the need of dynamic gastrointestinal simulation models such as simgi®, that allow to evaluate the transformations undergone by food and/or food ingredients during their transit through the gastrointestinal tract, as well as to determine potential changes in the composition and functionality of the intestinal microbiota after food ingestion. So far the studies using the simgi® have confirmed its potential applications in the area of food as a prior step to its application in clinical nutrition to prevent and/or treat diseases associated with intestinal dysbiosis and metabolic disorders. Likewise, this review includes feasible perspectives of the use of simgi® in clinical research concerning to diseases related to the intestinal microbiota.Dentro de la microbiota humana, el tracto gastrointestinal alberga el ecosistema más complejo y abundante del cuerpo humano, siendo el colon donde se encuentra la concentración más alta de microorganismos (1012 cel/g). La microbiota intestinal desempeñaa funciones metabólicas, tróficas y de protección que son de gran importancia para el hospedador. Durante las últimas décadas, son numerosos los estudios que han tratado de aportar evidencias científicas acerca de los factores que, a través de cambios en la composición de la microbiota intestinal, influyen en la salud humana. Sin embargo, esta aproximación está cambiando, y son cada vez más los expertos que apuestan por evaluar cambios a nivel de funcionalidad de la microbiota. Si aplicamos este enfoque dual al papel desempeñado por la dieta, resulta obvia la necesidad de disponer de modelos dinámicos de simulación gastrointestinal, como es el simgiR, que permitan evaluar las transformaciones que sufren los alimentos y/o ingredientes alimentarios durante el tránsito por el tracto gastrointestinal, así como para determinar los posibles cambios en la composición y funcionalidad de la microbiota intestinal derivados de la ingesta de alimentos. Los estudios llevados a cabo hasta el momento con el simgiR constatan sus potenciales aplicaciones en el área de los alimentos como paso previo a su aplicación en nutrición clínica, para prevenir y/o tratar enfermedades asociadas a disbiosis intestinal, así como trastornos metabólicos. Asimismo, esta revisión recoge posibles perspectivas de utilización del simgiR en la investigación clínica relativa a enfermedades vinculadas con disfunciones de la microbiota intestinalEste trabajo ha sido realizado gracias a la financiación del MINECO (proyecto AGL2015- 64522-C2-R) y la Comunidad de Madrid (Programa ALIBIRD-CM S2013/ABI-2728-CM). Alba Tamargo es beneficiaria de un contrato en el Programa de Garantía Juvenil-CSIC financiado gracias al Fondo Social Europeo. Irene Gil Sánchez es beneficiaria de una beca FPU del MECD (FPU14/0576

Evaluation of the interrelated effects of slaughtering, drying, and defatting methods on the composition and properties of black soldier fly (Hermetia illucens) larvae fat

The interrelated effect of different slaughtering, drying and defatting methods of black soldier fly larvae (BSFL) on the lipid composition and properties of the fat was studied. Blanching and freezing were compared as slaughtering methods, oven or freeze-drying as drying methods, and mechanical pressing or supercritical fluid extraction (SFE) as defatting methods. The different modes of slaughtering, drying, and defatting, along with both binary and ternary interactions caused significant effects on processes yields, lipid composition, moisture content and thermal properties. Thus, considering the defatting degree and the yield in total valued products (defatted meal plus fat), the combination of blanching, freeze-drying plus mechanical pressing was the worst option (51.2% and 87.5%, respectively). In contrast, the other combinations demonstrated better and comparable efficiency, although SFE is preferable for defatting (83.2% and 96.9%, respectively). The content of major fatty acids (lauric, palmitic and myristic acids) was significantly affected by the BSFL treatments, although with unsignificant impact on the total saturated fatty acids content. To preserve the integrity of the fat, the combination of blanching and oven-drying was preferred, as non-thermal methods of slaughtering and drying caused intense lipolysis, releasing free fatty acids (FFA) in the range of 18.6–23.5%. To achieve the lowest moisture content in the fats (≤0.1%), oven-drying with mechanical pressing were desired, regardless of the slaughtering method; while values > 1% were reached for freezing, freeze-drying and SFE. Both differences in FFA and moisture contents caused different thermal behaviors in the samples. Specially, the melting temperature was lower for samples with higher FFA and moisture contents, with a notable difference when freezing, freeze-drying and SFE were combined (14.5 ◦C vs 30.6 ◦C, as the mean value for the rest of samples). The different modes of processing did not affect the minor lipid compounds. Therefore, the modes employed for slaughtering, drying, and defatting of BSFL determine, either individually or in combination, the process yields, composition, and properties of the fatThis research was funded by the Spanish National Plans of Aquaculture of the Ministry of Agriculture, Fisheries and Food, project ACUINSECT (Optimization of insect flours as sustainable ingredient for aquaculture feed) with the support of the European Maritime and Fisheries Fund (FEMP

Influencia del contenido en grasa y de los tratamientos tecnológicos en la calidad y vida útil de la leche

En esta tesis se ha abordado el estudio del efecto de los distintos tratamientos tecnologicos como el tratamiento térmico, la homogenezacion y la alta presión en la calidad de la leche entera y desnatada. Se han realizado estudios con leche procesada a escala de laboratorio, en los que se alternaba el orden de aplicación del tratamiento termico y de la homogeneización, con leche procesada con un tratamiento UHT directo e indirecto en planta piloto y se han analizado diferentes lotes de leche UHT directo procesadas industrialmente. El estudio realizado a escala de laboratorio ha puesto de manifiesto que la homogeneización de la leche desnatada promueve la proteolisis, sobre todo si el proceso se realiza despues del tratamiento termico. Los resultados obtenidos en el estudio de la leche sometida a los tratamientos termicos en planta piloto, mostraron que la leche desnatada procesada mediante UHT directo experimenta, durante la conservación, una degradación proteolítica mas intensa que la leche entera sometida al mismo tratamiento, y en el caso de tratamiento UHT indirecto, la homogeneización realizada previamente al tratamiento térmico inhibe la proteolisis en la leche entera. Esto se traduce en que la leche entera homogeneizada, antes de ser sometida a este tratamiento térmico indirecto en planta piloto, experimenta, durante la conservación una degradación proteica menor que la leche sometida exclusivamente al tratamiento UHTindirecto.Peer Reviewe

Antioxidant activity of heather (Calluna vulgaris) PLE extracts

Póster presentado en las I Jornadas Científicas CIAL Forum 2014, celebrado en Madrid el 5 de junio de 2014.El brezo (Calluna vulgaris) es una especie botánica de la familia de la ericáceas, con un alto contenido en fitoquímicos y gran diversidad de actividades biológicas. Sobre esta planta se han descrito actividades anti-inflamatorias, analgésicas, hepatoprotectoras y antioxidantes, relacionadas principalmente con su alto contenido en ácidos triterpénicos y compuestos fenólicos. Los compuestos fenólicos como quercetina, herbacetina y canulina están presentes tanto en la raíz como en las hojas, las flores y los tallos. Además, en el brezo están presentes otro tipo de compuestos, los ácidos triterpénicos, donde los mayoritarios son el ácido ursólico, su isómero, el ácido oleanólico y el ácido betulínico. La extracción con líquidos presurizados (PLE) es una técnica de extracción novedosa que extrae analitos con un disolvente en caliente y presurizado. Las condiciones empleadas aceleran la solubilidad del analito y la cinética del proceso y evitan que el disolvente alcance su punto de ebullición, manteniéndose en estado líquido y produciendo una rápida y segura extracción de los analitos de interés. El objetivo de este trabajo fue evaluar el efecto de la temperatura y del disolvente en la extracción PLE de una mezcla de hojas y flores de brezo con la finalidad de obtener un extracto con alta capacidad antioxidante. Se realizaron extracciones PLE, con temperaturas de extracción de entre 80 y 200ºC y disolventes polares como agua, etanol y una mezcla de etanol/agua (50:50) y se utilizaron acetato de etilo y lactato de etilo con el objetivo de extraer los ácidos triterpénicos. En todos los extractos obtenidos se determinó el rendimiento del proceso, el contenido en compuestos fenólicos totales y en triterpenos fenólicos. La actividad antioxidante se evaluó posteriormente mediante el método de captura del radical libre del DHHP.Los autores agradecen al proyecto ALIBIRD-S2009/AGR-1469 de la Comunidad Autónoma de Madrid.Peer reviewe

Simultaneous extraction of rosemary and spinach leaves and its effect on the antioxidant activity of products

Mixed vegetal extracts are interesting target of new products as nutraceuticals, superior ingredients for the design of functional food, singular ingredients for cosmetics, etc. In this work the extraction of a mixture of spinach and rosemary leaves (50 wt.% of each plant) was investigated in terms of its antioxidant activity, and compared with the extraction of the separate species. Phenolic diterpenes of rosemary and carotenoids of spinach were target compounds due their recognized biological activities. Two different extraction techniques were applied, namely pressurized liquid extraction using hexane at two different temperatures (100 and 150 C) and supercritical fluid extraction with pure carbon dioxide at 40 C and two different pressures (20 and 30 MPa). For each extraction technique and conditions three different raw materials were employed: spinach leaves, rosemary leaves and the mixture 50:50 of spinach and rosemary leaves. The antioxidant activity of the samples produced was evaluated with the ABTS assay and showed to be enhanced when the species are simultaneously extracted, with antioxidant values around 20% higher than the values corresponding to mixing the extracts obtained by separate. A possible synergic effect between carotenoids and phenolic diterpenes was studied, although no specific synergic activity could be observed. However, the enhanced antioxidant activity could be attributed to a definite increase of the concentration of carnosic acid, which was observed in the samples produced by the simultaneous extraction. © 2013 Elsevier B.V. All rights reserved.This work has been supported by project INNSAMED IPT-300000-2010-34 (subprogram INNPACTO) from Ministry of Science and Innovation (Spain) and project ALIBIRD-S2009/AGR-1469 from Autonomous Community of Madrid.Peer Reviewe

Effect of the simultaneous extraction of rosemary and spinach leaves on the antioxidant activity of the extracts

Trabajo presentado al 10th International Symposium on Supercritical Fluids celebrado en San Francisco (US) del 13 al 16 de mayo de 2012.Several spices and some herbs have received increased attention as sources of effective natural antioxidants. Particularly, rosemary (Rosmarinus officinalis L.) is a Lamiaceae plant with high content of phenolic antioxidant substances, and spinach (Spinacia oleracea L.) is a natural source of carotenoids (lutein and β-carotene) which were also recognized to possess antioxidant activity. In this work the simultaneous extraction of leaves of a rosemary/spinach mixture (50 weight % of each plant) was investigated and compared with the extraction of the separate species. Three different extraction techniques were applied: (i) solid-liquid extraction at ambient pressure and using ethanol or hexane at 50ºC, (ii) accelerated solvent extraction (ASE) with the same liquid solvents but at higher temperatures (100 and 150ºC) and pressure (100 bar); and (iii) supercritical fluid extraction (SFE) with pure CO2 at 40ºC and different pressures (200 and 300 bar). All extracts obtained were studied in terms of the presence of antioxidant substances. Carotenoids and phenolic compounds were identified and quantified by HPLC analysis. Despite the extraction procedure and conditions applied, the results obtained show a linear behavior in terms of extraction yield and composition of key antioxidant compounds. The antioxidant activity of all samples was determined by the DPPH test and the effect of the simultaneous extraction (the mixed spinach/rosemary plant matrix) on the antioxidant activity of the extracts was analyzed and discussed.This work has been supported by project INNSAMED IPT-300000-2010-34 (subprogram INNPACTO) from Ministerio de Ciencia e Innovación (Spain) and Comunidad Autónoma de Madrid (project ALIBIRDS2009/AGR-1469).Peer Reviewe

Isolation of essential oil from different plants and herbs by supercritical fluid extraction

Supercritical fluid extraction (SFE) is an innovative, clean and environmental friendly technology with particular interest for the extraction of essential oil from plants and herbs. Supercritical CO 2 is selective, there is no associated waste treatment of a toxic solvent, and extraction times are moderate. Further, supercritical extracts were often recognized of superior quality when compared with those produced by hydro-distillation or liquid-solid extraction. This review provides a comprehensive and updated discussion of the developments and applications of SFE in the isolation of essential oils from plant matrices. SFE is normally performed with pure CO 2 or using a cosolvent; fractionation of the extract is commonly accomplished in order to isolate the volatile oil compounds from other co-extracted substances. In this review the effect of pressure, temperature and cosolvent on the extraction and fractionation procedure is discussed. Additionally, a comparison of the extraction yield and composition of the essential oil of several plants and herbs from Lamiaceae family, namely oregano, sage, thyme, rosemary, basil, marjoram and marigold, which were produced in our supercritical pilot-plant device, is presented and discussed. © 2012 Elsevier B.V.This work has been supported by project AGL2010-21565 (subprogram ALI) and project INNSAMED IPT-300000-2010-34 (subprogram INNPACTO) from Ministerio de Ciencia e Innovación (Spain) and Comunidad Autónoma de Madrid (project ALIBIRD-S2009/AGR-1469).Peer Reviewe

Colección de extractos naturales

Resumen del póster presentado a las II Jornadas Científicas CIAL-Fórum, celebradas durante los dias 16 y 17 de noviembre de 2016 en el Instituto de Investigación en Ciencias de la Alimentación (CIAL).El Laboratorio de Extractos Naturales del CIAL cuenta con una gran experiencia en la extracción de materias primas de origen vegetal (hojas, tallos, raíces, semillas, cortezas, flores, frutos, etc.) utilizando tecnologías enmarcadas en el ámbito de la química verde. Las infraestructuras de la Plataforma Novalindus del CIAL en lo que se refiere a procesos de extracción con fluidos a altas presiones, combinadas con las tecnologías a presión ambiente del laboratorio de Extractos Naturales (extracción sólido-líquido, Soxhlet, hidrodestilación, extracción asistida por enzimas, ultrasonidos) y disolventes verdes (especialmente de grado alimentario como etanol y agua), permiten la extracción selectiva de biomoléculas de interés en el campo de los ingredientes alimentarios funcionales (ácidos grasos, carotenoides, monoterpenos y sesquiterpenos, ácidos triterpénicos, alcaloides, antocianinas, ácidos fenólicos, etc.) mediante procesos GRAS (Generally Recognized as Safe). La Colección de Extractos Naturales creada reúne hasta la fecha 37 muestras de extractos de brezo, caléndula, tomillo, romero, mejorana, melisa, milenrama, mortiño, semillas de uva, obtenidos mediante la aplicación de la variedad de tecnologías disponibles en diferentes condiciones de extracción. Esta diversidad de extractos contribuye al aislamiento y el estudio de compuestos bioactivos, con el objetivo último de desarrollar ingredientes que puedan ser utilizados en el diseño de productos para mejorar el estado de salud y/o reducir el riesgo de padecer enfermedades.Los autores agradecen la financiación otorgada por la Comunidad de Madrid (ALIBIRD S2013/ABI-2728). V. Soulard agradece a la región Aquitaine y a la Escuela Nacional Superior de Química, Biología y Física de Burdeos por la financiación de su estancia en el Departamento de Producción y Caracterización de Nuevos Amientos del CIALPeer reviewe