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Synergies between compounds in food ingredients have been commonly obtained by the mixing of extracts produced individually. A different approach, based on the coextraction of plants and a new theoretical framework to identify synergistic and antagonistic effects in the coextracts, has been proposed in this study for the first time. The Pressurized Liquid Extraction (PLE) of rosemary and marjoram with parsley at several plant ratios was carried out and the antioxidant activity (ABTS and cellular assays) and phenolic compounds of the extracts were evaluated. Synergistic effects on the antioxidant activity of the extracts were identified from all the plant combinations. The HPLC-PAD analysis of the samples did not show a relation between the concentration of the main phenolic compounds in the coextracts and the observed antioxidant synergistic effects. The proposed theoretical framework may be successfully used for the determination of synergies in the bioactivity of extracts obtained by coextraction.

Pressurized liquid extraction (PLE) and ultrasound assisted extraction (UAE) were applied to extract phenolic antioxidants from defatted Brazil nut skin (DBNS) industrial by-product. Water/alcohol solvents (ethanol and methanol) (0 - 50 % v/v water) were used at temperatures of 50 - 200 °C in PLE and 50 °C was set in UAE. The effect on extraction yield, total phenolic compounds content (TPC), antioxidant capacity and phenolic characterization was determined. The temperature and water/alcohol mixture affected the dielectric constant, and this in turn influenced the yield, TPC, antioxidant activity and phenolic composition. In PLE, at 200 °C and 50 % (v/v) water/alcohol (ethanol and methanol) the highest yields (33.8 and 38.4 %, respectively), TPC (4673 and 5435 mg GAE/100 g DBNS) and antioxidant capacity (397 and 502 µmol TE/g DBNS) were obtained. Furthermore, at 50 °C, PLE had better extraction efficiency than UAE. Characterization of the extracts indicated that at 50 - 100 °C the extraction of protocatechuic acid and ellagic acid derivative were predominant, while at 150 - 200 °C catechin and vanillin derivatives stand out. In general, hydroxybenzoic acids and flavonoids were the most abundant phenolics, and the addition of 25 % v/v water to ethanol resulted in extracts with their highest concentration. Then, Brazil nut skin is an interesting phenolic-rich source with potential use to produce bioactive ingredients.

The effect of high-pressure homogenization (HPH) on the inactivation of Escherichia coli and the stability of the quality properties of Brazil nut beverages were studied. E. coli was used as target microorganism to validate the HPH process (pressures from 50 to 180 MPa and inlet temperatures (Ti) from 25 to 75 °C). Cold storage (5 °C) for 21 days was conducted to establish the shelf-life of BN beverages, in terms of their microbiological, physical, physicochemical, and sensorial stability. HPH-treated samples were compared to pasteurized BN beverages (63 °C for 20 min). The combination of Ti and the pressure of the HPH process (50 to 150 MPa/75 °C and 180 MPa/25 °C) had a significant effect on E. coli inactivation (8.2 log CFU/mL). During storage at 5 °C, the growth of mesophilic aerobes in processed BN beverages was controlled by the HPH process. Oxidative stability (TBAR assay) and physicochemical properties (pH, acidity, and °Brix) were evaluated during cold storage, showing good stability. Additionally, HPH-treated beverages showed a reduction in their particle size and the formation of more stable protein aggregates, which favored the beverages’ whiteness (color). The HPH process could be an alternative to pasteurization to obtain Brazil nut beverages with an acceptable microbiological shelf life (≥21 days at 5 °C) and high-quality characteristics without the use of any additives.

Synsepalum dulcificum (Richardella dulcifica) is a berry fruit from West Africa with the ability to convert the sour taste into a sweet taste, and for this reason, the fruit is also known as the “miracle berry” (MB). The red and bright berry is rich in terpenoids. The fruit’s pulp and skin contain mainly phenolic compounds and flavonoids, which correlate with their antioxidant activity. Different polar extracts have been described to inhibit cell proliferation and transformation of cancer cell lines in vitro. In addition, MB has been shown to ameliorate insulin resistance in a preclinical model of diabetes induced by a chow diet enriched in fructose. Herein, we have compared the biological activities of three supercritical extracts obtained from the seed—a subproduct of the fruit—and one supercritical extract obtained from the pulp and the skin of MB. The four extracts have been characterized in terms of total polyphenols content. Moreover, the antioxidant, anti-inflammatory, hypo-lipidemic, and inhibition of colorectal cancer cell bioenergetics have been compared. Non-polar supercritical extracts from the seed are the ones with the highest effects on the inhibition of bioenergetic of colorectal (CRC) cancer cells. At the molecular level, the effects on cell bioenergetics seems to be related to the inhibition of main drivers of the de novo lipogenesis, such as the sterol regulatory element binding transcription factor (SREBF1) and downstream molecular targets fatty acid synthase (FASN) and stearoyl coenzyme desaturase 1 (SCD1). As metabolic reprograming is considered as one of the hallmarks of cancer, natural extracts from plants may provide complementary approaches in the treatment of cancer. Herein, for the first time, supercritical extracts from MB have been obtained, where the seed, a by-product of the fruit, seems to be rich in antitumor bioactive compounds. Based on these results, supercritical extracts from the seed merit further research to be proposed as co

The supercritical defatting of H. illucens was scaled up at 450 bar and 60 °C from a 270 cm3 extraction cell to a vessel five times larger. Then, eight different H. illucens larvae batches, with variable content of oil (16.80–29.17% w/w) and moisture (4.45–15.95% w/w) were defatted. The effect of these parameters on yield and oil composition was analyzed. The presence of moisture in the larvae batch, in the range of the values studied, had no negative effect on the oil recovery efficiency, which was mainly determined by the initial content of oil in the larvae samples. Furthermore, no differences were determined in the fatty acid profile of the oils recovered, which were rich in saturated fatty acids, mainly lauric acid (ca. 50% w/w). Minor lipids, such as squalene and phytosterols, were determined in all the oil samples. The moisture content in the oils extracted was in the range of 0.118–1.706% w/w. Therefore, some samples exceeded the limits recommended for volatile matter in edible fats and oils (0.2%, including moisture). Yet, concerning the oil peroxide index, values were much lower than those corresponding to the oil extracted using hexane.

Borututu (Cochlospermum angolense Welw.) roots have been described as a rich source of phenolic compounds. Despite the potential of this plant for the production of bioactive extracts, studies reported until now have been scarce, and they have been based on the use of inefficient conventional extraction techniques. In this study, pressurized liquid extraction (PLE) was investigated for the production of borututu root extracts. Different temperatures (50–200 °C) and solvents (water, ethanol, and 50% ethanol:water) were applied. The total phenolic compound (TPC) content, the main phenolic compounds and the in vitro antioxidant activity of the extracts were evaluated. The results were compared with those obtained by conventional decoction with water. The highest concentrations of TPC and antioxidant activity were obtained with 50% ethanol:water, followed by water. The extract obtained with 50% ethanol:water at 150 °C had a TPC concentration of 343.80 mg/g and presented the largest antioxidant activity (1488 and 4979 µmol Trolox/g extract, determined by DDPH and ABTS assay, respectively). These values were considerably higher than those obtained by conventional decoction. Ellagic acid, and ellagic and methyl ellagic acid glycosides were the main phenolic compounds found in the extracts. Therefore, was PLE demonstrated to be a selective and efficient technique to obtain extracts with high concentrations of phenolic compounds and high antioxidant activity form borututu roots.

Los insectos comestibles destacan como una fuente alternativa de proteínas. No obstante, durante el procesado de algunas especies se genera igualmente una fracción grasa relevante, como es el caso de las larvas de Hermetia illucens (mosca soldado negra), siendo un coproducto de gran interés para alimentación animal y humana. Por tanto, estudiar la influencia del procesado tecnológico sobre esta fracción grasa es clave para garantizar su calidad y uso en diversos fines. En el presente estudio, se llevó a cabo la evaluación del efecto de distintas formas de procesado de las larvas de H. illucens sobre la composición, calidad y bioactividad de la grasa obtenida. En concreto, se evaluaron dos formas de sacrificio (congelación o escaldado), seguido de dos formas de secado (horno o liofilización) y, de dos formas de desgrasado (prensado o extracción con fluidos supercríticos, SFE). Atendiendo al rendimiento de grasa, para todas las combinaciones de tratamientos, fue preferible el procedimiento de SFE, consiguiéndose el menor rendimiento al combinar escaldado-liofilización-prensa. De manera general, el perfil de ácidos grasos no sufrió cambios relevantes en función del procesado. No obstante, sí se evidenció una evidente lipólisis, con la consecuente generación de acidez libre, en función del tratamiento. Así, la aplicación de métodos no térmicos de congelación junto con liofilización dio lugar a la mayor degradación de la grasa en forma de ácidos grasos libres. Sin embargo, esta acidez fue minoritaria al aplicar métodos térmicos, como sacrificio por escaldado y secado por horno. Por otro lado, la combinación de congelación-liofilización-prensado produjo el mejor estado oxidativo inicial. De igual manera, el proceso de liofilización-prensado produjo las grasas más estables durante su almacenamiento a lo largo de 6 meses. En cuanto a la bioactividad de la grasa, se encontró una relación significativa entre la estabilidad oxidativa y la actividad antioxidante de la grasa, su

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 a

The aim of this study was to evaluate the modulating effect of the processing of Hermetia illucens larvae on the antibacterial activity of the fat related to lipolysis to free fatty acids (FFAs), mainly as lauric acid. Blanching and freezing were compared for slaughtering, oven or freeze-drying for drying, and mechanical pressing or supercritical fluid for defatting. Freezing plus freeze-drying produced the highest FFAs content (21%), mainly as lauric acid (11%). In agreement, freezing plus freeze-drying was also the most effective method to obtain fats with higher antibacterial activity, regardless of the defatting method. The antibacterial activity was significantly more relevant for gram-positive bacteria, having a strain-dependent character. The most effective fat was bactericidal for Listeria monocytogenes and Bacillus subtilis and reduced Staphylococcus aureus growth. Therefore, it is possible to selectively modulate the antibacterial activity of the H. illucens fat due to lipolysis by the processing methods of larvae.

[Simple Summary] In addition to the potential of edible insects as an alternative source of proteins, the production of insect meals generates a significant amount of fat that is also of interest for food and feed. The consideration of the impact of processing factors on the quality of insect fats, such as oxidative stability, is indispensable to fully realize their value as a co-product. Therefore, this study aimed to understand how the different successive modes of processing of Hermetia illucens larvae (black soldier fly larvae, BSFL), such as slaughtering (by blanching or freezing), drying (by oven-drying or freeze-drying) and defatting (by mechanical pressing or supercritical CO2 SFE), as well as their interactions, affect the oxidation of the resulting fat and defatted meal. The preferred procedure would be a combination of freezing with freeze-drying and mechanical pressing, especially the combination of freeze-drying and mechanical pressing, for the best oxidative quality during storage. Such oxidative stability was strongly related to the antioxidant activity of the fats, which was conditioned by the processing methods used for BSFL. Therefore, this study provides guidance on selecting the best combinations of slaughtering, drying, and defatting processes for BSFL to obtain fats with the best oxidative quality., 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 steps.

Reversible and sub-lethal stresses to the mitochondria elicit a program of compensatory responses that ultimately improve mitochondrial function, a conserved anti-aging mechanism termed mitohormesis. Here, we show that harmol, a member of the beta-carbolines family with anti-depressant properties, improves mitochondrial function and metabolic parameters, and extends healthspan. Treatment with harmol induces a transient mitochondrial depolarization, a strong mitophagy response, and the AMPK compensatory pathway both in cultured C2C12 myotubes and in male mouse liver, brown adipose tissue and muscle, even though harmol crosses poorly the blood-brain barrier. Mechanistically, simultaneous modulation of the targets of harmol monoamine-oxidase B and GABA-A receptor reproduces harmol-induced mitochondrial improvements. Diet-induced pre-diabetic male mice improve their glucose tolerance, liver steatosis and insulin sensitivity after treatment with harmol. Harmol or a combination of monoamine oxidase B and GABA-A receptor modulators extend the lifespan of hermaphrodite Caenorhabditis elegans or female Drosophila melanogaster. Finally, two-year-old male and female mice treated with harmol exhibit delayed frailty onset with improved glycemia, exercise performance and strength. Our results reveal that peripheral targeting of monoamine oxidase B and GABA-A receptor, common antidepressant targets, extends healthspan through mitohormesis.

Edible insects are gaining attention as a source of bioactive compounds of great interest for health. To produce bioactive extracts from insects with a high concentration of bioactive compounds, defatting seems to be relevant for those fat-rich forms of insects as larvae. Supercritical fluid extraction (SFE) might be useful for both the defatting and subsequent extraction of the defatted sample to obtain bioactive extracts from edible insects. Different samples of black soldier fly (Hermetia illucens) larvae were defatted using SFE as an alternative to conventional defatting methods, and the optimal defatted flour was sequentially extracted by SFE employing different levels of ethanol as co-solvent. The resulting extracts were characterised by GC-MS-FID and their bioactivity was then assayed in terms of their antioxidant and pancreatic lipase inhibitory activities. The maximum fat yield by SFE (around 43%) was achieved at 450 bar, 60 degrees C and 100 g/min of CO2 flow, not being significantly different from conventional defatting with hexane. Extraction yield of SFE extracts increased along with the proportion of co-solvent. The composition of the extracts widely varied depending on the insect sample and the amount of co-solvent used, free amino acids and fatty acids being the two major chemical families among the different extracts. In terms of their bioactivity, a lipase inhibitory activity closer to 50% was exhibited by most extracts, which was favoured by the amount of co-solvent in one of the insect samples. Regardless of the significant differences observed between the insect samples, the exhibited DPPH radical inhibitory activity was weak. It is concluded that SFE is an interesting alternative to the conventional defatting of H. illucens, as well as an integrative and sequential process that allows producing bioactive extracts from this insect, especially towards the inhibition of the pancreatic lipase.

The mealworm (Tenebrio molitor Linnaeus 1758) is gaining importance as one of the most popular edible insects. Studies focusing on its bioactivities are increasing, although alternative forms of consumption other than the whole insect or flour, such as bioactive non-protein extracts, remain underexplored. Furthermore, the incidence of metabolic syndrome-related pathologies keeps increasing, hence the importance of seeking novel natural sources for reducing the impact of certain risk factors. The aim was to study the potential of a non-protein mealworm extract on metabolic syndrome-related pathologies, obtained with ethanol:water (1:1, v/v) by ultrasound-assisted extraction. We characterized the extract by gas-chromatography mass-spectrometry and assessed its hypolipidemic potential, its ability to scavenger free radicals, to attenuate the inflammatory response in microglial cells, to affect mitochondrial respiration and to enhance insulin sensitivity in mouse hepatocytes. The extract contained fatty acids, monoglycerides, amino acids, certain acids and sugars. The mealworm extract caused a 30% pancreatic lipase inhibition, 80% DPPH· scavenging activity and 55.9% reduction in the bioaccessibility of cholesterol (p = 0.009). The extract was effective in decreasing iNOS levels, increasing basal, maximal and ATP coupled respiration as well as enhancing insulin-mediated AKT phosphorylation at low insulin concentrations (p < 0.05). The potential of a non-protein bioactive mealworm extract against metabolic syndrome-related pathologies is shown, although further studies are needed to elucidate the mechanisms and relationship with compounds., [Simple Summary] Among edible insects, mealworm has gained attention due to its proven beneficial effects; however, mealworm products other than flour, such as concentrated forms or extracts different to proteins, are still rare. This novel food source can have a positive impact on multiple diseases such as via the metabolic syndrome. Our objective was to describe the composition of a mealworm extract and study its effect on metabolic syndrome-related pathologies. The extract interfered with the absorption of cholesterol and partially blocked the digestion of fats. It also reduced the inflammatory response, enhanced the sensitivity to insulin and showed strong antioxidant potential. Mealworm extract might be an interesting candidate for ameliorating the risk factors associated with the metabolic syndrome.

Nowadays, there is great interest in the discovery of food compounds that might inhibit gut microbial TMA production from its methylamine precursors. In this work, an innovative novel screening strategy capable of rapidly determining the differences in the metabolic response of Klebsiella pneumoniae, a bacteria producing TMA under aerobic conditions, to a library of extracts obtained from food and natural sources was developed. The proposed high-throughput screening (HTS) method combines resazurin reduction assay in 384-well plates and Gaussian Processes as a machine learning tool for data processing, allowing for a fast, cheap and highly standardized evaluation of any interfering effect of a given compound or extract on the microbial metabolism sustained by L-carnitine utilization. As a proof-of-concept of this strategy, a pilot screening of 39 extracts and 6 pure compounds was performed to search for potential candidates that could inhibit in vitro TMA formation from L-carnitine. Among all the extracts tested, three of them were selected as candidates to interfere with TMA formation. Subsequent in vitro assays confirmed the potential of oregano and red thyme hexane extracts (at 1 mg mL−1) to inhibit TMA formation in bacterial lysates. In such in vitro assay, the red thyme extract exerted comparable effects on TMA reduction (∼40%) as 7.5 mM meldonium (∼50% TMA decrease), a reported L-carnitine analogue. Our results show that metabolic activity could be used as a proxy of the capacity to produce TMA under controlled culture conditions using L-carnitine to sustain metabolism.

The production of specific insect extracts with bioactive properties for human health is an emerging and innovative field for the edible insects industry, but there are unexplored extraction factors that might modulate the bioactivity of the extracts. Ultrasound-assisted extracts from T. molitor and H. illucens were produced. Effects of defatting pre-treatment and extraction solvent were evaluated on extraction yield, antioxidant activity and pancreatic lipase inhibitory effect. Chemical characterisation of defatted extracts from H. illucens was performed by GC-MS-FID. Non-defatted extracts showed higher extraction yields. Defatted extracts had similar extraction yields (around 3%). Defatted extracts had higher antioxidant activity, T. molitor being stronger than H. illucens. Antioxidant activity of T. molitor methanol extract was higher than the rest of solvents. Aqueous ethanol improved the antioxidant activity of H. illucens extracts. All extracts inhibited lipase, but no significant effect of defatting and solvent was observed for T. molitor. A significant higher inhibitory activity was observed for H. illucens, the strongest being defatted 100% and 70% ethanol H. illucens extracts. H. illucens extracts contained free amino acids and disaccharides, together with minor fractions of lipids, sterols and organic acids. These results evidence the potential of extracts obtained from edible insects as antioxidants and inhibitors of the pancreatic lipase, a simultaneous multibioactivity that might be favoured by the defatting pre-treatment of the samples and the solvent of extraction.

In addition to their nutritional and physiological role, proteins are recognized as the major compounds responsible for the rheological properties of food products and their stability during manufacture and storage. Furthermore, proteins have been shown to be source of bioactive peptides able to exert beneficial effects on human health. In recent years, scholarly interest has focused on the incorporation of high-quality proteins into the diet. This fact, together with the new trends of consumers directed to avoid the intake of animal proteins, has boosted the search for novel and sustainable protein sources and the development of suitable, cost-affordable, and environmentally friendly technologies to extract high concentrations of valuable proteins incorporated into food products and supplements. In this review, current data on emergent and promising methodologies applied for the extraction of proteins from natural sources are summarized. Moreover, the advantages and disadvantages of these novel methods, compared with conventional methods, are detailed. Additionally, this work describes the combination of these technologies with the enzymatic hydrolysis of extracted proteins as a powerful strategy for releasing bioactive peptides.

Plant extracts are being studied in the development of novel edible food coatings. The antioxidant and antimicrobial compounds that naturally occur in some plants are the key substances that contribute to preserving food quality. Besides the plant material, the method utilized to produce the extract influences its chemical and preservative characteristics. In general, hydrodistillation produce plant products (essential oils) that are well recognized for containing high concentration of antioxidant or antimicrobial volatile compounds. Supercritical fluid technology produces high quality bioactive extracts with higher yield but lower concentration of volatile compounds, in comparison with hydrodistillation. In this work, six different natural extracts of five different plants were produced by hydrodistillation and supercritical fluid extraction, and their antioxidant and antimicrobial activities were compared. The most active extracts were used to produce chitosan-based edible coatings with the aim of assessing the effect of essential oils versus supercritical extracts on the preservation of strawberries.

Supercritical anti-solvent precipitation (SAS) using carbon dioxide is a novel technique that can be used to produce powdered ingredients in small size particles, facilitating their incorporation into food matrices. In this work, the SAS precipitation of a licorice root ethanolic extract was studied. SAS assays were carried out at 15–20 MPa, 308.15 and 313.15 K, and two different concentrations (9.6 and 14.2 mg/ml) of the ethanolic licorice extract. In the range of conditions investigated, SAS pressure and temperature did not affect significantly the precipitation yield, but phytochemicals recovery was higher with the lower licorice extract concentration. Moreover, the fractionation of licorice bioactives (liquiritin, liquiritigenin, isoliquiritigenin, glabridin and glycyrrhizic acid) was assessed, together with the content of total phenolic compounds and antioxidant activity of the powders and oleoresin by-products obtained. In this respect, precipitates and oleoresins presented significant differences in the concentration of some licorice bioactives, and higher antioxidant activity was observed in precipitates. Additionally, significant effect of pressure, temperature and licorice extract concentration on the morphology and particle size of precipitates was observed, recovering smaller and more regular particles at 15–20 MPa, 313.15 K and 9.6 mg/ml licorice extract concentration, attaining satisfactory yield and antioxidant activity.

The recent development of powerful “omics” technologies (genomics, transcriptomics, proteomics, metabolomics, and lipidomics) has opened new avenues in nutritional sciences toward precision nutrition, which is a genotype-directed nutrition that takes into account the differential responses to nutritional interventions based on gene variation (nutrigenetics) and the effect of nutrients on gene expression (nutrigenomics). Current evidence demonstrates that up to one third of the deaths caused by cancer could be prevented by acting on key risk factors, with diet being one of the most important risk factors due to its association with obesity. Additional factors such as composition of gut microbiome, the immune system, and the nutritional status will have an impact on the final outcome. Nutrient components and bioactive compounds from natural sources can have an impact on cancer progression or even the risk of cancer development by regulating gene expression and/or associated risk factors such as obesity and chronic inflammation. Nowadays, among the different methods to produce natural extracts, the green technology of supercritical fluid extraction (SFE) is quite popular, with a special interest on the use of supercritical CO2 for the extraction of compounds with low polarity. The success of nutritional interventions based on the use of nutraceuticals requires several steps: (i) in vitro and preclinical demonstration of their antitumoral effects; (ii) knowledge of their mechanism of action and molecular targets, which will allow for identification of the specific subgroups of patients who will benefit from them; (iii) the study of genetic variants associated with the differential responses; and (iv) innovative approaches of formulations to improve the in vivo bioavailability of the bioactive ingredients. Herein, we investigate the antitumoral properties and mechanism of action of a supercritical CO2 extract from Calendula officinalis, commonly known as marigold (marigo

Nowadays, obesity and its associated metabolic disorders, including diabetes, metabolic syndrome, cardiovascular disease, or cancer, continue to be a health epidemic in westernized societies, and there is an increased necessity to explore anti-obesity therapies including pharmaceutical and nutraceutical compounds. Considerable attention has been placed on the identification of bioactive compounds from natural sources to manage the metabolic stress associated with obesity. In a previous work, we have demonstrated that a CO2 supercritical fluid extract from yarrow (Yarrow SFE), downregulates the expression of the lipogenic master regulator SREBF1 and its downstream molecular targets FASN and SCD in a tumoral context. Since obesity and diabetes are strongly considered high-risk factors for cancer development, herein, we aimed to investigate the potential therapeutic role of Yarrow SFE in the metabolic stress induced after a high-fat diet in mice. For this purpose, 32 C57BL/6 mice were distributed in four groups according to their diets: standard diet (SD); SD supplemented with Yarrow SFE (SD + Yarrow); high-fat diet (HFD); and HFD supplemented with Yarrow SFE (HFD + Yarrow). Fasting glycemia, insulin levels, homeostasis model assessment for insulin resistance (HOMA-IR), lipid profile, gene expression, and lipid content of liver and adipose tissues were analyzed after three months of treatment. Results indicate improved fasting glucose levels in plasma, enhanced insulin sensitivity, and diminished hypercholesterolemia in the HFD + Yarrow group compared to the HFD group. Mechanistically, Yarrow SFE protects liver from steatosis after the HFD challenge by augmenting the adipose tissue buffering capacity of the circulating plasma glucose.

The kinetics of the supercritical fluid extraction of edible and discarded chia seeds was studied and modelled for the first time. The total oil was removed at 45 MPa and 60 °C after 240 min. The extraction kinetics was simulated using a dynamic model in gPROMS ModelBuilder environment and the kinetic parameters estimated. Triolein was chosen as a model compound of the chia oil. The agreement between the experimental yields and those calculated by the model was good with deviations in the range (1.2–6.6) %, except at 25 MPa and 60 °C (AARD = 9.5%).

Achillea millefolium L. is a plant widely used in traditional medicine. Nowadays, there is a growing concern about the study of its bioactive properties in order to develop food and nutraceutical formulations. Supercritical anti-solvent fractionation (SAF) of an A. millefollium extract was carried out to improve its antioxidant and anti-inflammatory activities. A selective precipitation of phenolic compounds was achieved in the precipitation vessel fractions, which presented an antioxidant activity twice than original extract, especially when fractionation was carried out at 10 MPa. The main phenolic components identified in this fraction were luteolin-7-O-glucoside, 3,5-dicaffeoylquinic acid, 6-hidroxyluteolin-7-O-glucoside and apigenin-7-O-glucoside. However, separator fractions presented higher anti-inflammatory activity than precipitation vessel ones, particularly at 15 MPa. This fact could be related to separator fractions enrichment in anti-inflammatory compounds, mainly camphor, artemisia ketone and borneol. Therefore, SAF produced a concentration of antioxidant and anti-inflammatory compounds that could be used as high-added valued ingredients.

Metabolic reprogramming is considered a hallmark of cancer. Currently, the altered lipid metabolism in cancer is a topic of interest due to the prominent role of lipids regulating the progression of various types of tumors. Lipids and lipid-derived molecules have been shown to activate growth regulatory pathways and to promote malignancy in pancreatic cancer. In a previous work, we have described the antitumoral properties of Yarrow (Achillea Millefolium) CO2 supercritical extract (Yarrow SFE) in pancreatic cancer. Herein, we aim to investigate the underlaying molecular mechanisms by which Yarrow SFE induces cytotoxicity in pancreatic cancer cells. Yarrow SFE downregulates SREBF1 and downstream molecular targets of this transcription factor, such as fatty acid synthase (FASN) and stearoyl-CoA desaturase (SCD). Importantly, we demonstrate the in vivo effect of Yarrow SFE diminishing the tumor growth in a xenograft mouse model of pancreatic cancer. Our data suggest that Yarrow SFE can be proposed as a complementary adjuvant or nutritional supplement in pancreatic cancer therapy.

Heather (Calluna vulgaris L.) and marigold (Calendula officinalis L.) are two rich sources of bioactive pentacyclic triterpenes. The supercritical carbon dioxide (SCCO2) extraction of these two plants was explored at a pressure range of 25–50 MPa, 50 °C, with or without fractionation, different extraction times (1.5–4.0 h) and using ethanol as a co-solvent (0 and 10% w/w). In order to determine potential synergisms, a combined extraction (heather + marigold 50:50) was also studied. In general, higher extraction yields were achieved when the co-solvent was added. Higher concentrations of total triterpenic acids were obtained in heather extracts, specially using ethanol. The co-solvent did not increase the terpene concentration in marigold extracts. For the combined extraction, an antagonist effect in the triterpene concentration was observed in absence of a co-solvent, whereas a synergistic effect was exhibited in its presence, especially for ursolic acid. In general, the extracts showed a certain anti-inflammatory effect, although a straight correlation with the analyzed triterpenic acids concentration was not exhibited. Moreover, the combined extraction exposed a similar anti-inflammatory activity in comparison with the individual plant extracts.

Licorice (Glycyrrhiza glabra L.) is a plant used widely in herbal medicines due to their several biological potentials. The supercritical extraction of licorice roots was investigated to assess the antioxidant and antimicrobial activity of the extracts. Extraction conditions were pressures from 15 to 40 MPa, 313.15 and 333.15 K, and ethanol cosolvent in the range of 0 to 20% mass. In the case of high-pressure extractions using pure carbon dioxide (CO2) fractionation of the supercritical extract was accomplished in a two-cell decompression system. Fractionation was carried out with the aim to examine the potential separation of the antioxidant and antimicrobial licorice compounds and thus increase the bioactive properties of the fractions obtained in each separation cell. Main licorice bioactive compounds, liquiritin, liquiritigenin, glycyrrhizin, isoliquiritigenin and glabridin, were identified by HPLC and quantified using standards. Extracts obtained with supercritical CO2 and ethanol cosolvent contain the higher amounts of phenolic compounds and also the higher antioxidant activity but exhibit low or even no antimicrobial activity. Using pure CO2 at high pressure coupled with the on-line fractionation of the extract, two samples were obtained which showed, respectively, lower phenolic compounds content and good antimicrobial capacity (first fraction) and higher phenolic compounds content and antioxidant capacity (second fraction). Thus, the advantages of supercritical on-line fractionation are demonstrated in the extraction of Licorice roots.

[Background] Typical hydrolysis times of saponins generally do not take into consideration the effect of time on the degradation of the target compounds, namely sapogenins. When producing natural extracts, it should be borne in mind that conducting hydrolysis to yield a target compound might also affect the final composition of the extracts in terms of other bioactive compounds. In our study, saponin‐rich extracts from fenugreek, quinoa, lentil, and soybean were produced and their acid hydrolysis to give sapogenin‐rich extracts was conducted over different periods (0–6 h). The disappearance of saponins and appearance of sapogenins was analyzed using high‐performance liquid chromatography–diode array detection–mass spectrometry (HPLC‐DAD‐MS) and gas chromatography–mass spectrometry (GC‐MS), respectively. The impact of hydrolysis on the phytosterols and tocopherol in the extracts was also evaluated., [Results] Fenugreek showed the highest saponin content (169 g kg−1), followed by lentil (20 g kg−1), quinoa (15 g kg−1), and soybean (13 g kg−1). Hydrolysis for 1 h caused the complete disappearance of saponins and the greatest release of sapogenins. Hydrolyzed fenugreek and quinoa extracts contained the highest amounts of sapogenins and minor fractions of phytosterols and tocopherol. Hydrolyzed extracts of lentil and soybean contained a major fraction of phytosterols and a low fraction of sapogenins. In all cases, sapogenins decreased after 1 h of hydrolysis, phytosterols slightly decreased, and tocopherol was unaffected. Standards of diosgenin and oleanolic acid also showed this decreasing pattern under acid hydrolysis conditions., [Conclusion] Hydrolysis times of 1 h for saponin‐rich extracts from the assayed seeds guarantee the maximum transformation to sapogenin‐rich extracts, along with phytosterols and tocopherol. Fenugreek and quinoa seeds are preferred for this.

Pancreatic cancer is one of the most aggressive tumors which occurrence is linked, together with genetic factors, to diet and lifestyle. Trying to potentiate the use of natural derived products from diet, here we propose a supercritical extract (SFE) as a nutritional supplement for cancer treatment. Yarrow SFE has demonstrated to be cytotoxic for pancreatic cancer cells (MIA PaCa-2), and able to brake 3D-sphere growth. In addition, it causes cell death through caspase 3/7 activation and therefore, triggering apoptosis. Moreover, treating MIA PaCa-2 with a chemotherapeutical agent used in clinic (5-Fluorouracil) after sensitizing them with Yarrow SFE has shown a synergetic effect between both. Finally, in a xenograft model, it has shown that animals who received Yarrow SFE extract develop a smaller tumor. In summary, our results indicate that Yarrow supercritical extract is a promising antitumoral co-adjuvant in pancreatic cancer treatment.

Pancreatic cancer is one of the most aggressive tumors which occurrence is linked, together with genetic factors, to diet and lifestyle. Trying to potentiate the use of natural derived products from diet, here we propose a supercritical extract (SFE) as a nutritional supplement for cancer treatment. Yarrow SFE has demonstrated to be cytotoxic for pancreatic cancer cells (MIA PaCa-2), and able to brake 3D-sphere growth. In addition, it causes cell death through caspase 3/7 activation and therefore, triggering apoptosis. Moreover, treating MIA PaCa-2 with a chemotherapeutical agent used in clinic (5-Fluorouracil) after sensitizing them with Yarrow SFE has shown a synergetic effect between both. Finally, in a xenograft model, it has shown that animals who received Yarrow SFE extract develop a smaller tumor. In summary, our results indicate that Yarrow supercritical extract is a promising antitumoral co-adjuvant in pancreatic cancer treatment.

En los últimos años, ha aumentado el uso de CO2 supercrítico (SCCO2) como antisolvente para la precipitación de compuestos bioactivos a partir de extractos vegetales. Este proceso de precipitación supercrítica antisolvente (SAS) permite emplear bajas temperaturas de procesamiento y evita el uso de disolventes orgánicos tóxicos. El objetivo de este trabajo, consistió en el fraccionamiento de compuestos bioactivos de romero (Rosmarinus oficinalis) mediante procesos SAS, evaluando las condiciones de extracción y el diseño de diferentes celdas de precipitación en las que se modificaron las conexiones de entrada y salida tanto del extracto como del SCCO2. El fraccionamiento de los compuestos se realizó a diferentes condiciones de presión (10-20 MPa), temperatura (40-60 ºC) y flujo másico de SCCO2 (50-60 g/min) durante 60 min, partiendo de una solución etanólica obtenida por ultrasonidos (UAE). De todas las fracciones obtenidas se determinó el contenido de compuestos fenólicos totales (TPC), el contenido en los principales compuestos antioxidantes del romero, ácido carnósico(CA) y ácido rosmarínico (RA), así como la actividad antioxidante. Además, la morfología de las partículas y la distribución de tamaño de partícula se determinaron mediante microscopia electrónica de barrido (SEM) y difracción láser respectivamente. Los resultados obtenidos por medio de la precipitación SAS en las diferentes condiciones mostraron una recuperación del extracto inicial entre un 80-90%. En las dos fracciones obtenidas, extracto seco en la celda de precipitación y fracción etanólica en el separador, los rendimientos fueron de 45-69% y 18-44%, respectivamente, dependiendo de las condiciones de precipitación. En el análisis de las fracciones se observó que el RA se concentró en la celda de precipitación hasta más del doble de la concentración inicial y el CA en el separador hasta casi el triple de la concentración inicial. El contenido en TPC fue superior en todos los casos al contenido del

La especie Cochlospermun angolensis (borututu) es un árbol nativo de las regiones tropicales de América Latina y África, ampliamente utilizado en la medicina tradicional. La raíz de borututu presenta una alta cantidad de compuestos fenólicos, sin embargo, su extracción se ha llevado a cabo únicamente mediante métodos tradicionales, utilizando principalmente agua como disolvente. En este trabajo se llevó a cabo la extracción de compuestos fenólicos mediante líquidos presurizados (PLE), a partir de la raíz y de las flores de borututu. Se estudiaron cuatro disolventes (agua, etanol, acetato de etilo y agua/etanol 50:50) y se aplicaron temperaturas entre 50 y 200 ºC. Como cabía esperar, el rendimiento de extracción aumentó con la temperatura y al aumentar la polaridad del disolvente (rendimiento del 57,3 % con agua a partir de la raíz y próximo al 50 % a partir de las flores). El rendimiento obtenido de las flores con acetato de etilo fue aproximadamente 2,5 veces superior al de la raíz, sugiriendo la presencia de una mayor cantidad de compuestos apolares en esta materia prima. Del mismo modo, la concentración de compuestos fenólicos (Folin-Ciocalteu) y la capacidad antioxidante (ensayo ABTS) aumentaron con la polaridad del disolvente. No obstante, la mayor concentración de estos compuestos y la mayor capacidad antioxidante de los extractos de la raíz se obtuvieron con la mezcla etanol/agua (374 mg GAE/g y 4,2 mmol Trolox/g).

Calendula officinalis, commonly known as marigold, has been used in traditional medicine for its anti-inflammatory and antiseptic virtues, and against gastric spasms. Here, we had obtained marigold extracts through supercritical CO2 extraction (SFE) and through ultrasonic assisted extraction (UAE), and we had characterized their bioactivity in the framework of cancer. We have found that marigold UAE extracts have a higher content of phenolic and flavonoid than marigold SFE extract, as well as a higher antioxidant activity. On the contrary, marigold SFE extract has a stronger cytotoxic and antiproliferative activity against pancreatic tumor-derived cells, being independent to its antioxidant effect. These results suggest that marigold SFE could be considered for further studies as a potential nutritional supplement which could improve current cancer therapies.

Chia seeds (Salvia hispanica) contain a large amount of oil (25-35% mass of dry seed) rich in polyunsaturated fatty acids - particularly linoleic (15-20) % and linolenic (60-65) % - of the total fatty acids. In our work, the influence of supercritical extraction (SCE) operating conditions, namely temperature (40 and 60 ºC) and pressure (25 and 45 MPa) at a constant CO2 flow rate (40 g/min), on oil yield from chia seeds is studied and presented. The extraction curves obtained at the experimental conditions examined are shown on Figure 1. The highest oil recovery (90.3 %) was achieved at 60 ºC and 45 MPa, while the lowest (64.5 %) was obtained at 40 ºC and 25 MPa. In addition, the kinetics of the SCE process was modeled and reported for the first time applying an approach, which reflects in a rigorous way the interplay between phase equilibria (solubility) and kinetics. The approach was deployed, validated and executed using gPROMS Model Builder. For the purposes of modeling, chia seed oil was represented as triolein and the calculation of its solubility in the scCO2 at the temperatures and pressures of interest to the experiment was realized applying a rigorous thermodynamic modelling framework. The qualitative and quantitative agreement between the SCE experimental data and the extraction curves simulated was good.

[Background] Pancreatic cancer is one of the most aggressive and mortal cancers. Although several drugs have been proposed for its treatment, it remains resistant and new alternatives are needed. In this context, plants and their derivatives constitute a relevant source of bioactive components which might efficiently inhibit tumor cell progression., [Methods] In this study, we have analyzed the potential anti-carcinogenic effect of different Asteraceae (Achillea millefolium and Calendula officinalis) and Lamiaceae (Melissa officinalis and Origanum majorana) plant extracts obtained by different green technologies (Supercritical CO2 Extraction –SFE- and Ultrasonic Assisted Extraction –UAE-) to identify efficient plant extracts against human pancreatic cancer cells that could constitute the basis of novel treatment approaches., [Results] Asteraceae extracts showed better results as antitumoral agents than Lamiaceae by inducing cytotoxicity and inhibiting cell transformation, and SFE extracts were most efficient than UAE extracts. In addition, SFE derived plant extracts from Achillea millefolium and Calendula officinalis displayed synergism with the chemotherapeutic 5-Fluororacil., [Conclusion] These results show how Yarrow and Marigold SFE-derived extracts can inhibit pancreatic cancer cell growth, and could be proposed for a comprehensive study to determine the molecular mechanisms involved in their bioactivity with the final aim to propose them as potential adjuvants in pancreatic cancer therapy.

The potential impact of increased levels of potassium (K+) in hydroponic solution on the production of bioactive compounds, which provide added value to products, is relevant for local economy and human health. This research pursues assessing different levels of K+ on the nutrition of basil, an important aromatic crop in the arid region of La Laguna, northern México, where water scarcity demands the conversion from open-field agriculture to hydroponics. A randomized complete block design with a factorial arrangement (3 × 4) was used to determine the content of nutraceutical components, including polyphenolic compounds, flavonoids, anthocyanins, vitamin C, chlorophylls, and the antioxidant capacity of three varieties of hydroponic basil, with four doses of K+ in the nutrient solution, 7, 9, 11 and 13 mmol L−1. The analysis of variance showed significant differences (p ≤ 0.001) in most of the response variables, caused by the genotype and doses of K+. The antioxidant capacity of assessed cultivars was improved when doses of K+ were increased in the nutrient solution. Furthermore, the antioxidant capacity was positively correlated to the content of flavonoids (r = 0.621), anthocyanins (r = 0.655) and total phenolic compounds (r = 0.549). In conclusion, the nutraceutical content was increased in basil when controlling K+ in the nutrient solution.

[Background]: Vaccinium meridionale Swartz (mortiño) constitutes a source of bioactive phytochemicals, but reports related to its efficient and green production are scarce. In this study, pressurized liquid extraction (PLE) and ultrasound-assisted extraction of mortiño were compared. Total phenolic content (TPC) and antioxidant capacity (ABTS) were determined. Beef burgers with 20 g kg of mortiño (MM) or its PLE extract (ME) were manufactured. Lipid oxidation (TBARS) and instrumental color changes were measured after refrigerated storage. [Results]: High TPC (up to 72 g gallic acid equivalent kg extract) was determined in mortiño extracts, which was positively correlated with antioxidant activity. TBARS values of beef burgers containing either MM or ME did not change after refrigerated storage, whereas lipid oxidation of control burgers increased significantly. The color of burgers with added MM or ME was different (lower b* and a* values) from that of control burgers. However, the evolution of color after storage was similar between control and ME samples. [Conclusion]: Mortiño extracts with high TPC can be obtained by PLE. Both mortiño and its PLE extract are able to control lipid oxidation of beef burgers, but the extract is preferred from the color quality point of view.

Saponins are bioactive compounds of increasing interest. The events that take place during digestion are highly related to their bioactivities, because saponins are poorly absorbed and have a long residence time in the intestinal tract. The poor bioavailability of saponins is explained by a sum of factors, but the more favorable properties of sapogenins result in higher bioavailability and bioactivity. The gastric and colonic transformations of saponins are relevant in the release of sapogenins. Saponins inhibit enzymes and cholesterol absorption, but specific chemical structures of saponins are relevant for an efficient activity. Finally, the recent research has pointed to saponins as “prebiotic-like” compounds. This review summarizes the current knowledge on the events that take place during digestion of saponins and sapogenins related to their bioactivities, with special emphasis on the factors that modulate their bioavailability, bioaccessibility, inhibition of digestive enzymes and cholesterol absorption, and the importance of the microbiota-saponins relationship.

The efficient production of saponin-rich extracts is of increasing interest due to the bioactive properties that have being demonstrated for these compounds. However, saponins have a poor bioavailability. In this respect, the knowledge about the bioaccessibility of saponins as a first step before bioavailability has been scarcely explored. In this study, the production of ultrasound-assisted extracts of saponins from edible seeds (quinoa, soybean, red lentil, fenugreek and lupin) was carried out with ethanol, ethanol:water or water. Extraction yield, total saponin (TSC), fat and total phenolics content (TPC) were determined. Then, the bioaccessibility of saponins after the in vitro gastrointestinal digestion of the extracts was determined and the effect of TPC and fat in the extracts on bioaccessibility was evaluated. The highest saponin-rich extracts were obtained by ethanol, being fenugreek and red lentil the richest extracts (12% and 10%, respectively). Saponins from ethanol:water extracts displayed variable bioaccessibility (from 13% for fenugreek to 83% for lentil), but a bioaccessibility closer to 100% was reached for all ethanol extracts. Correlation studies showed that TPC of the extracts negatively affected the bioaccessibility of saponins, whereas fat of the extracts enhanced this parameter. As summary, ultrasound-assisted extraction is shown as an efficient method for obtaining saponin-rich extracts from edible seeds, being ethanol the most advantageous solvent due to the richness of saponins and the successful bioaccessibility from these extracts, likely caused by the co-extracted fat with ethanol. Regardless of the extracts, phenolic compounds or fat may hinder or enhance the bioaccessibility of saponins, respectively. Additionally, an adequate balance between saponins to lipids has shown to be relevant on such an effect.

The digestion, absorption, uptake and bioavailability of a rosemary supercritical fluid extract encapsulated in oil in water emulsion were studied. Two emulsions with opposite surface charge were prepared, containing 7% canola oil, and either 2% lactoferrin or whey protein isolate. When absorption and uptake of carnosic acid and carnosol were followed on Caco-2 cell monolayers, there were no differences with protein type. However, when co-cultures of HT-29 MTX were employed, the presence of mucus caused a higher retention of carnosic acid in the apical layer for lactoferrin emulsions. The immune activity of the bioavailable fractions collected from cell absorption experiments was tested ex vivo on murine splenocytes. Although transport through the intestinal barrier models was low, the bioavailable fractions showed a significant effect on splenocytes proliferation. These results demonstrated the potential of using rosemary supercritical extract through protein stabilized oil in water emulsions, as a food with immunomodulatory functionality.

The extraction of marigold (Calendula officinalis) oleoresin with supercritical carbon dioxide SCCO2 was carried out in a small scale extraction vessel (2.7 × 10−4 m3) studying different extraction pressures (14, 24 and 34 MPa) and different flow rates (15, 30 and 45 g min−1) at 313 K. Then, using semi-empirical engineering scaling criteria (constant solvent lineal velocity or constant solvent residence time) and the Broken and Intact Cell (BIC) model, the scaling up to larger extraction vessels (1.35 × 10−3 m3 and 5.16 × 10−3 m3) was theoretically investigated. According to the BIC model, by keeping constant the CO2 residence time in the different size vessels a good reproduction of the kinetic behavior should be obtained. Nevertheless, experimental results did not confirm model predictions, and in fact none of the scaling criteria studied resulted adequate in the marigold supercritical extraction scaling up. Thus, using all the experimental overall extraction curves obtained, a new specific correlation was developed between the Schmidt number (Sc), CO2 mass flow, bed geometry and the supercritical mass transfer coefficients kYA with a good fit (R2 = 0.9767) for scaling up the supercritical extraction of marigold.

Cancer is among the leading causes of morbidity and mortality worldwide. Many of the chemotherapeutic agents used in cancer treatment exhibit cell toxicity and display teratogenic effect on nontumor cells. Therefore, the search for alternative compounds which are effective against tumor cells but reduce toxicity against nontumor ones is of great importance in the progress or development of cancer treatments. In this sense, scientific knowledge about relevant aspects of nutrition intimately involved in the development and progression of cancer progresses rapidly. Phytochemicals, considered as bioactive ingredients present in plant products, have shown promising effects as potential therapeutic/preventive agents on cancer in several in vitro and in vivo assays. However, despite their bioactive properties, phytochemicals are still not commonly used in clinical practice due to several reasons, mainly attributed to their poor bioavailability. In this sense, new formulation strategies are proposed as carriers to improve their bioefficacy, highlighting the use of lipid-based delivery systems. Here, we review the potential antitumoral activity of the bioactive compounds derived from plants and the current studies carried out in animal and human models. Furthermore, their association with lipids as a formulation strategy to enhance their efficacy in vivo is also reported. The development of high effective bioactive supplements for cancer treatment based on the improvement of their bioavailability goes through this association.

Asteraceae (Achillea millefolium and Calendula officinalis) and Lamiaceae (Melissa officinalis and Origanum majorana) extracts were obtained by applying two sequential extraction processes: supercritical fluid extraction with carbon dioxide, followed by ultrasonic assisted extraction using green solvents (ethanol and ethanol:water 50:50). The extracts were analyzed in terms of the total content of phenolic compounds and the content of flavonoids; the volatile oil composition of supercritical extracts was analyzed by gas chromatography and the antioxidant capacity and cell toxicity was determined. Lamiaceae plant extracts presented higher content of phenolics (and flavonoids) than Asteraceae extracts. Regardless of the species studied, the supercritical extracts presented the lowest antioxidant activity and the ethanol:water extracts offered the largest, following the order Origanum majorana > Melissa officinalis ≈ Achillea millefolium > Calendula officinalis. However, concerning the effect on cell toxicity, Asteraceae (especially Achillea millefolium) supercritical extracts were significantly more efficient despite being the less active as an antioxidant agent. These results indicate that the effect on cell viability is not related to the antioxidant activity of the extracts.

[ES]: Los fluidos supercríticos han abierto un amplio campo de posibilidades y nuevas alternativas en la tecnología de los alimentos. La razón principal es el hecho del empleo del CO2 como disolvente, una sustancia permitida en alimentos. Ciertamente, la extracción con fluidos supercríticos (SFE) de materiales vegetales sólidos es actualmente la aplicación más explotada. Bajo el concepto de química verde, La SFE es una de las más eficientes y prometedoras alternativas para la producción de extractos vegetales de alta calidad. La tecnología SFE puede considerarse como una técnica óptima de extracción de biomoléculas, debido a la completa ausencia de disolventes orgánicos durante el proceso y en el producto final, su adecuación para extraer especies termosensibles, la ausencia de daño oxidativo y la posibilidad de poder ser aplicada tanto a escala analítica como a escala industrial. El comportamiento cinético de la SFE de materiales vegetales en lecho fijo se suele representar mediante un gráfico de la masa extraída en función del tiempo, o en función de masa de disolvente consumido, comúnmente conocido como curva de extracción (OEC, Overall Extraction Curve). No solo el rendimiento másico varía durante el tiempo de extracción, sino también la composicióny las propiedades fisicoquímicas y biológicas del extracto. El escalado en un proceso de SFE busca reproducir la misma OEC en diferentes celdas de extracción con diferente capacidad y/o forma. Existe un gran número de modelos cinéticos en la literatura, los cuales han sido desarrollados y/o adaptados para representar la OEC de un proceso SFE. Estos modelos incluyen desde correlaciones simples basadas en cinéticas de primer orden, tales como el modelo de Barton, hasta modelos fenomenológicos integrales basados en la transferencia de masa diferencial en el interior de la celda de extracción. Sin embargo, los estudios o enfoques sobre el escalado SFE son escasos en la bibliografía y están basados en la aplicación de algu, [EN]: Supercritical fluids have opened a wide range of new alternatives for the expansion of food technology. Certainly, the most remarkable reason is the use of a substance permitted in foods, namely carbon dioxide (CO2), as solvent. The supercritical fluid extraction (SFE) of solid vegetable materials is currently one of the most exploited applications. Under the concept of green processing, SFE is one of the most efficient and promising alternatives to produce high-quality vegetal extracts. SFE technology can be awarded as a superior extraction technique for biomolecules because it is organic solvent free, adequate for thermo-sensitive species, avoid oxidation damage, and can be applied from analytical scale to large industrial scale. The kinetic behavior of SFE of vegetal packed beds is usually represented by the plot of the mass extracted as a function of time or as a function of the mass of spent solvent, commonly denoted Overall Extraction Curve (OEC). Not only mass yield varies along extraction time, but also composition, physicochemical and biological properties of the extract. SFE scaling aims to reproduce the same OEC in extraction vessels with different shape and/or capacity. A large number of kinetic models can be found in the literature, which were developed and/or adapted to represent the OEC of SFE processes, including simple correlations based on first order kinetics, such as the Barton model, to comprehensive phenomenological models based on mass transfer differential occurred in the cell extraction. Yet, more limited approaches and studies are available in the literature regarding SFE scaling, and are based on some thumb rules or semi-empirical approaches of traditional chemical engineering. In this PhD Thesis the kinetic behavior of two vegetal materials, namely Vaccinium meridionale Swartz (mortiño) and Calendula officinalis (calendula), was study. The OECs were obtained at different extraction pressures and temperatures, as well as at different