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High-pressure homogenization (HPH) is an emerging technology for obtaining physical and microbial stability of plant-based milks, but there is little information on the effects of this technology on the phytochemical components of the processed plant food beverage and during its cold storage. The effect of three selected HPH treatments (180 MPa/25 °C, 150 MPa/55 °C, and 50 MPa/75 °C) and pasteurization (PAS) (63 °C, 20 min) on minor lipid constituents, total proteins, phenolic compounds, antioxidant capacity, and essential minerals of Brazil nut beverage (BNB) were studied. Additionally, the study of the possible changes in these constituents was carried out during cold storage at 5 °C for 21 days. The fatty acid profile (dominated by oleic acid and linoleic acid), free fatty acid content, protein, and essential minerals (notable source of Se and Cu) of the processed BNB remained almost stable to treatments (HPH and PAS). Specifically, reductions in squalene (22.7 to 26.4%) and γ-γ-tocopherol (28.4 to 36%) were observed in beverages processed via both non-thermal HPH and thermal PAS, but β-sitosterol remained unchanged. Total phenolics were reduced (24 to 30%) after both treatments, a factor that influenced the observed antioxidant capacity. The studied individual phenolics in BNB were gallic acid, catechin, epicatechin, catechin gallate, and ellagic acid, being the most abundant compounds. During cold storage (5 °C) up to 21 days, changes in the content of phytochemicals, minerals, and total proteins were not noticeable for any treated beverages, and no lipolysis processes were promoted. Therefore, after the application of HPH processing, Brazil nut beverage (BNB) maintained almost unaltered levels of bioactive compounds, essential minerals, total protein, and oxidative stability, remarkable characteristics for its potential development as a functional food.

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. HIGHLIGHTS High temperature and water/alcohol mixtures improves TPC and antioxidant capacity At given temperature, TPC values are linearly correlated with water/alcohol dielectric constant Extraction temperature modifies the abundance and profile of phenolic compounds Hydroxybenzoic acids and flavanols are predominant phenolics in Brazil nut skins At 50 °C, PLE have a better extraction efficiency of phenolic compounds than UAE GRAPHICAL ABSTRACT

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., This work is jointly supported by research grant AGL2017-89055-R (Ministerio de Ciencia e Innovación, MICINN)., We acknowledge support of the publication fee by the CSIC Open Access Publication Support Initiative through its Unit of Information Resources for Research (URICI).

This article belongs to the Special Issue Extraction and Fractionation Processes of Functional Components in Food Engineering., 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., This research was funded by the Spanish Ministry of Science and Innovation, projects PID2019-104218RB-I00/AEI/2015-66886R and PID2019-110183RB-C22/AEI/10.13039/501100011033.

This article belongs to the Special Issue Phenolic Compounds in Herbs: Characterization, Antioxidant Properties and Health Benefits., Melissa officinalis L. and Origanum majorana L., within Lamiaceae family, and Calendula officinalis L. and Achillea millefolium L., within the Asteraceae, have been considered a good source of bioactive ingredients with health benefits. In this study, the supercritical fluid extraction (SFE) using pure CO2, and the ultrasound assisted extraction (UAE) were proposed as green techniques to obtain plant-based extracts with potential antioxidant and anti-inflammatory activities. Higher values of total phenolic content and antioxidant activity were achieved in UAE ethanol:water (50:50, v/v) extracts. Meanwhile, UAE pure ethanol extracts showed greater anti-inflammatory activity. RP-HPLC-PAD-ESI-QTOF-MS/MS analysis showed a vast number of phenolic compounds in the extracts, including unreported ones. O. majorana ethanol:water extract presented the highest content of phenolics and antioxidant activity; among its composition, both rosmarinic acid and luteolin glucoside derivatives were abundant. The pure ethanol extract of A. millefolium resulted in an important content of caffeoylquinic acid derivatives, luteolin-7-O-glucoside and flavonoid aglycones, which could be related to the remarkable inhibition of TNF-α, IL-1β and IL-6 cytokines. Besides, borneol and camphor, found in the volatile fraction of A. millefolium, could contributed to this latter activity. Thus, this study points out that O. majorana and A. millefolium are considered a promising source of bioactive ingredients with potential use in health promotion., Authors thanks to the Spanish Government (Project: PID2019-110183RB-C22/AEI/10.13039/501100011033) and Comunidad Autónoma de Madrid (ALIBIRD2020-CM (S2018/BAA-4343)) for financial support.

This article belongs to the Special Issue Insects and Their Derivatives for Human Practical Uses., 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., This research was funded by the Community of Madrid, grant number ALIBIRD2020-CM, S2018/BAA-4343.

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., The authors gratefully acknowledge the financial support from Comunidad de Madrid through the Programa de I+D en Tecnologías, Spain (ALIBIRD-CM S2013/ABI-2728). Somaris E. Quintana is grateful for the funding provided by Gobernación de Bolivar and Fundación Ceiba, Colombia. Olimpia Llalla is grateful to Programa Nacional de Innovación Agraria-PNIS of Perú (Contract No. 152-2018-INIA-PNIA-PASANTIA).

Several plant extracts are being investigated to produce edible coatings, mainly due to their antioxidant and antimicrobial activities. In this study, licorice root extracts were produced by ultrasound‐assisted extraction and were combined with chitosan to elaborate edible coatings. Different solvents and temperatures were used in the extraction process, and the antioxidant and antimicrobial activity of the extracts were assessed. The most bioactive extracts were selected for the development of the edible coatings. The rheological properties of the coatings were studied, and they were applied on strawberry to evaluate their physicochemical and microbiological properties. The addition of licorice extract to chitosan resulted in positive effects on the rheological properties of the coatings: the incorporation of phytochemicals to chitosan decreased the shear stress and improved the restructuring ability of the coating solutions. The films presented a reduction of the Burger model parameter, indicating a reduction of rigidity. Furthermore, the strawberry coated with chitosan and licorice extract maintained good quality parameters during storage and showed the best microbiological preservation in comparison with controls. Hence, the use of chitosan with licorice extract is a potential strategy to produce edible coating for improving the postharvest quality of fruits, This research was funded by Comunidad Autónoma de Madrid, grant number P2013/ABI27, project Bolívar Gana con Ciencia, MinCiencias Contract 368-2019 and Programa Nacional de Innovación Agraria—PNIA of Perú, Contract: No. 152-2018-INIA-PNIA-PASANTIA

This article belongs to the Special Issue Dietary Patterns, Dietary Indices for Colorectal Cancer, Mortality and the Related Disease., 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., This work was supported by the Spanish Ministry of Science (Plan Nacional I + D + i AGL2016-76736-C3), Regional Government of Community of Madrid (P2013/ABI-2728, ALIBIRD-CM; P2018/BAA-4343-ALIBIRD2020-CM), the Ramón Areces Foundation, and the EU Structural Funds.

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 (marigold SFE) in the context of pancreatic cancer. Mechanistically, marigold SFE induces the expression of BMP8B, which leads to an energetic catastrophe ending up with autophagy-induced cell death (AICD). As metabolic reprogramming is a well-recognized hallmark of cancer, the direct impact of marigold SFE on pancreatic cancer cell metabolism encourages further research of its potential as a coadjuvant in pancreatic cancer therapy. Finally, we discuss innovative formulation approaches to augment the clinical therapeutic potential of marigold SFE in nutritional interventions., This work was supported by the Spanish Ministry of Science (Plan Nacional I + D + i AGL2016-76736-C3), Regional Government of Community of Madrid (P2018/BAA-4343-ALIBIRD2020-CM), Ramón Areces Foundation, and EU Structural Funds.

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%)., J. A. P. Coelho, R. M. Filipe and R. P. Stateva acknowledge the funding received from the European Union’s Horizon 2020 research and innovation programme under the Marie Sklodowska-Curie grant agreement No. 778168. J. A. P. Coelho, and R. M. Filipe acknowledge the funding received from Fundação para a Ciência e a Tecnologia, Portugal, under projects UID/ECI/04028/2013 and UID/QUI/00100/2013. Chia seeds were generously supplied by PRIMARIA (www.primaria.biz).

Although triacylglycerols (TAG) are the major constituents of chia oil, it also contains minor lipid fractions that include phospholipids (PL) among other desirable components. Its amphiphilic character and excellent biocompatibility make PL appropriate for numerous applications with technological and nutritional significanceand potential health benefits. Given the difficulties entailed by the PL isolation, the efficiency for extracting such compounds using two environmental friendly techniques, pressurized liquid extraction (PLE) and supercritical fluid extraction (SFE) was evaluated. By using PLE with food-grade ethanol (EtOH), an oil recovery close to 100% was achieved in just 10 min. This oil extract was particularly rich in α-linolenic acid (ALA; 70%) as compared to the oil extracted by SFE (56%). In the case of SFE, the oil recovery was only 87% but increased to 99% when ethanol was added to CO2. However the use of co-solvent did not affect the fatty acid profile of the supercritical extracts or their TAG composition, where the high molecular weight TAG species were the predominant in all cases. With the exception of SFE without co-solvent, all methods applied were capable of extracting the PL fraction, although the content and distribution of the individual components present in this fraction differed markedly depending on the extraction conditions used. In this context, the use of a sequential extraction process, combining SFE and PLE was particularly interesting. The re-extraction by PLE of the chia cake, previously defatted by SFE, allowed to obtain an oil extract highly enriched in PLs, whose content exceeded 16% and with a higher PL species than the rest of the oil extracts., This study was supported in part by grants from the Spanish Ministry of Science, Innovation and Universities, Spain (AGL2017-87884 MINECO/AEI/FEDER, UE); by the Comunidad de Madrid through the B Programa de Actividades en Tecnologías, Spain (ALIBIRD-CM S2013/ABI-2728).

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 authors gratefully acknowledge the financial support from Ministerio de Economía y Competitividad of Spain (Projects AGL2017-89055-R and AGL2016-76736-C3-1-R). Somaris E. Quintana is grateful for the funding provided by Gobernación de Bolivar and Fundación Ceiba, Colombia, in the project “Bolívar Gana con Ciencia”.

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., This work was supported by the Ministerio de Economía y Competitividad, Spain (AGL2016-76736-C3-1-R) and the Community of Madrid, Spain (ALIBIRD-CM S2013/ABI-2728). Joaquín Navarro del Hierro thanks the Ministerio de Educación, Cultura y Deporte for funding his research with a FPU predoctoral contract (FPU 15/04236). Teresa Herrera thanks the Community of Madrid for her contract (Fondo Social Europeo, Programa Operativo de Empleo Juvenil e Iniciativa de Empleo Juvenil YEI).

Background: Vaccinium meridionale Swartz (mortino) 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 mortino were compared. Total phenolic content (TPC) and antioxidant capacity (ABTS•+ ) were determined. Beef burgers with 20 g kg-1 of mortino (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-1 extract) was determined in mortino 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: Mortino extracts with high TPC can be obtained by PLE. Both mortino 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. © 2017 Society of Chemical Industry.; © 2017 Society of Chemical Industry.

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., This work was partly funded by the Natural Sciences and Engineering Council of Canada, through the Canada Research Chair program and the Spanish Ministry of Economy and Competitiveness (FORCANCER project, AGL2013- 48943-C2-1-R). EA work was supported by the Alfonso Martin Escudero Foundation, through a Post-Doctoral Fellowship.

In this work the fractionation of an ethanolic extract of Achillea millefolium L. (yarrow) using supercritical carbon dioxide anti-solvent technique was studied, with the target of increasing the concentration of phenolic compounds in the precipitated fraction. The effect of pressure on the selective precipitation was analyzed, together with the morphology and particle size distribution of the precipitates. In the range of pressures studied (10–20 MPa), up to a 3 fold increase of the total phenolic compound concentration was observed in the precipitates in comparison with the ethanolic yarrow extract. In addition, the selective fractionation of the main phenolic compounds identified in the extract (3,5-dicaffeoylquinic acid, a glycoside form of apigenin and luteolin, as well as the aglycones) was analyzed. Particle sizes around 250–330 μm were produced with a nozzle of 101.6 μm inner diameter, due to the formation of aggregates. In this respect, increasing pressure from 10 to 15 MPa resulted in smaller particles, while further pressure increasing had no significant effect on particle size decrease., The authors gratefully acknowledge the financial support from Ministerio de Economía y Competitividad of Spain (project AGL2013-48943-C2) and the Comunidad Autónoma de Madrid (ALIBIRD, project number S2013/ABI-2728).

Supercritical extracts of marigold (ME) were produced and characterized. The bioaccessibility of terpenes, especially that of pentacyclic triterpenes (PT), the particle-size distribution, and antioxidant activity after the in vitro codigestion of ME with olive oil (OO) were determined. ME produced without cosolvent was richer in taraxasterol, lupeol, α-amyrin, and β-amyrin than extracts with cosolvent. All terpenes showed high bioaccessibility without OO (>75%). Significant correlations were found between the molecular properties of compounds (logP and number of rotatable bonds) and their bioaccessibility. Codigestion with OO enhanced the bioaccessibility (around 100% for PT), which could be related to a higher abundance of low-size particles of the digestion medium. The antioxidant activity of the digested ME increased around 50%, regardless of OO. PT-rich extracts from marigold display high bioaccessibility and improved antioxidant activity after in vitro digestion, although complete bioaccessibility of PT can be reached by codigestion with oil, without affecting antioxidant activity., This work was supported by the Ministerio de Economia y Competitividad, Spain (AGL2013−48943-C2-1-R) and the Community of Madrid, Spain (ALIBIRD-CM S2013/ABI-2728). J.N.d.H. thanks the Universidad Autonoma de Madrid for funding his collaboration scholarship during his Official Master’s Degree studies.

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., The authors gratefully acknowledge the financial support from Ministerio de Economía y Competitividad of Spain (Projects AGL2016-76736-C3-1-R and AGL2015-64522-C2-R). Somaris E. Quintana is grateful for the funding provided by Gobernación de Bolivar and Fundación Ceiba, Colombia.

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., This work was supported by Spanish Government (FORCHRONIC Project: AGL-2016-76736-C3-1-R) and Comunidad Autónoma de Madrid (ALIBIRD, project: P2013/ALI2728).

The simultaneous fractionation and precipitation of an ethanolic extract of rosemary (Rosmarinus officinalis L.) using supercritical carbon dioxide anti-solvent technique was studied, with the target of separate in two different fractions the key antioxidants of rosemary (i.e. rosmarinic acid, carnosic acid and carnosol). The effect of pressure and temperature on the fractionation process was investigated, together with the morphology and particle size distribution of the precipitates. Additionally, the chemical composition of the oleoresins were analyzed and reported. In the range of pressures (9–20 MPa) and temperatures (313–333 K) used in this work, the precipitates presented a 2–3 fold enrichment of rosmarinic acid, while carnosic acid and carnosol were concentrated (2–3 fold enrichment) in the oleoresin fractions. Furthermore, in general, oleoresins presented higher antioxidant activity than precipitates. Particles produced with a nozzle of diameter 101.6 μm were smaller and more spherical with increasing pressure (mean value 4–10 μm at 20 MPa) and decreasing temperature., The authors gratefully acknowledge the financial support from Ministerio de Economía y Competitividad of Spain (Proyect AGL2016-76736-C3-1-R). Somaris E. Quintana is grateful for the funding provided by Gobernación de Bolivar and Fundación Ceiba, Colombia, in the project “Bolívar Gana con Ciencia”.

Ethanol extracts (EE) from fenugreek and quinoa seeds with different total content of inhibitory compounds (TIC, total saponin plus phenolic) were prepared with and without concentration of TIC (CEE –concentrated EE-, and EE, respectively). Their inhibitory activity on pancreatic lipase and α-amylase was assessed by traditional in vitro methods (with or without orbital shaking), and by simulating intestinal digestion. CEE contained higher contents of TIC than EE, being fenugreek superior to quinoa (p, This work was supported by the Ministerio de Economía y Competitividad, Spain (AGL2016-76736-C3-1-R) and the Community of Madrid, Spain (ALIBIRD-CM S2013/ABI-2728). Teresa Herrera thanks the Community of Madrid for her contract (Fondo Social Europeo, Programa Operativo de Empleo Juvenil e Iniciativa de Empleo Juvenil YEI). Joaquín Navarro del Hierro thanks the Ministerio de Educación, Cultura y Deporte, Spain for funding his research with a FPU predoctoral contract (FPU 15/04236).

[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., This work was supported by the Ministerio de Economía y Competitividad, Spain (AGL2016‐76736‐C3‐1‐R) and the Community of Madrid, Spain (ALIBIRD‐CM S2013/ABI‐2728). Teresa Herrera thanks the Community of Madrid for her contract (Fondo Social Europeo, Programa Operativo de Empleo Juvenil e Iniciativa de Empleo Juvenil YEI). Joaquín Navarro del Hierro thanks the Ministerio de Educación, Cultura y Deporte for funding his research with a Formación de Profesorado Universitario (FPU) predoctoral contract (FPU 15/04236).

This article belongs to the Special Issue Advances in Supercritical Fluid Food Science and Technology., 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., The authors gratefully acknowledge the financial support from Ministerio de Economía y Competitividad of Spain (project AGL2013-48943-C2) and the Comunidad Autónoma de Madrid (ALIBIRD, project number S2013/ABI-2728).

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., This work was supported by Ministerio de Economía y Competitividad del Gobierno de España (MINECO, Plan Nacional I+D+i AGL2013-48943-C2 and AGL2016-76736-C3), Gobierno regional de la Comunidad de Madrid (P2013/ABI-2728, ALIBIRD-CM) and EU Structural Funds.