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In recent years, as part of sustainable development policies, the revaluation of end-of-life products has become more and more widespread. In terms of sustainability, in a scenario of circular economy food sustainability aims, inter alia, at making an effective re-use of natural resources as a starting point for the obtainment of high added-value products. With the aim of promoting the valorization of the wine sector wastes, the present study took into account the leaves of Vitis vinifera L. cv. Aglianico from the Campania Region (Italy). The use of deep eutectic solvents as a greener alternative to the most common organic solvents, joint to ultrasound-assisted maceration, and LC-MS tools, allowed us to define for the first time a six-month quantitative variation of flavonol derivatives, and in particular of quercetin 3-O-glucuronide, based on the collection time and the leaf height on the grapevine. Results underlined that the influence of abiotic factors, such as exposure to sunlight, which is pivotal in the biosynthesis of such compounds, should be strictly considered for their full recovery.

Plants of genus Cichorium (Asteraceae) can be used as vegetables with higher nutritional value and as medicinal plants. This genus has beneficial properties owing to the presence of a number of specialized metabolites such as alkaloids, sesquiterpene lactones, coumarins, unsaturated fatty acids, flavonoids, saponins, and tannins. Cichorium endivia L., known as escarole, has achieved a common food status due to its nutritionary value, bitter taste, and the presence of healthy components, and is eaten cooked or raw in salads. Presently, wastes derived from the horticultural crops supply chain are generated in very large amounts. Vegetable waste comprises the discarded leaves of food sources produced during collection, handling, transportation, and processing. The external leaves of Cichorium endivia L. are a horticultural crop that is discarded. In this work, the phytochemical profile, antioxidant, and anti-inflammatory activities of hydroalcoholic extract obtained from discarded leaves of three cultivars of escarole (C. endivia var. crispum ‘Capriccio’, C. endivia var. latifolium ‘Performance’ and ‘Leonida’) typical horticultural crop of the Campania region were investigated. In order to describe a metabolite profile of C. endivia cultivars, the extracts were analysed by HR/ESI/Qexactive/MS/MS and NMR. The careful analysis of the accurate masses, the ESI/MS spectra, and the 1H NMR chemical shifts allowed for the identification of small molecules belonging to phenolic, flavonoid, sesquiterpene, amino acids, and unsaturated fatty acid classes. In addition, the antioxidant potential of the extracts was evaluated using cell-free and cell-based assays, as well as their cytotoxic and anti-inflammatory activity. All the extracts showed similar radical-scavenging ability while significant differences between the three investigated cultivars emerged in the cell-based assays. The obtained data were ascribed to the content of polyphenols and sesquiterpenes in the extracts. Accordingly, C. endivia by-products can be deemed an interesting material for healthy product formulations.

Green extraction methods using a combination of mechanical, enzymatic, and green chemical treatments were evaluated for the sequential extraction of carotenoid pigments, protein, and chitin from crab processing discards. Key objectives included avoiding the use of hazardous chemical solvents, conducting as close to a 100% green extraction as possible, and developing simple processes to facilitate implementation into processing plants without the need for complicated and expensive equipment. Three crab bio-products were obtained: pigmented vegetable oil, pigmented protein powder, and chitin. Carotenoid extractions were performed using vegetable oils (corn, canola, and sunflower oils), giving between 24.85% and 37.93% astaxanthin recovery. Citric acid was used to demineralize the remaining material and afforded a pigmented protein powder. Three different proteases were used to deproteinate and isolate chitin in yields between 17.06% and 19.15%. The chitin was still highly colored and therefore decolorization was attempted using hydrogen peroxide. Characterization studies were conducted on each of the crab bio-products isolated including powder X-ray diffraction analysis on the chitin (80.18% crystallinity index, CI, achieved using green methods). Overall, three valuable bio-products could be obtained but further research is needed to obtain pigment-free chitin in an environmentally friendly manner.

Capsicum chinense Jacq., from the Yucatan peninsula, is recognized worldwide for its pungency, flavor, and secondary metabolites content. This has resulted in an increase in its production, which has led to an increase in the number of byproducts considered waste, mainly its leaves. Capsicum chinense leaves have been demonstrated to contain polyphenols with bioactive properties (antioxidant, anti-inflammatory, antiobesogenic capacity, etc.); hence, the extraction of polyphenols through the use of natural deep eutectic solvents (NADES) with a green technology, such as an ultrasonic probe, could help to revalue these leaves by maximizing the extraction efficiency and preserving their bioactive properties. The objective of this study was to optimize the composition of a eutectic solvent for obtaining an extract rich in polyphenols from the Capsicum chinense leaf using a sonic probe. The optimum conditions of the composition of NADES for obtaining the highest Antioxidant capacity (Ax, 79.71% inhibition) were a 0.8 mol glucose to 1 mol of choline chloride ratio, and 12% water. In addition, with this composition, the Total Polyphenol Content (TPC) obtained was 165.39 mg GAE/100 g dry leaf, and the individual polyphenols, such as vanillin (19.15 mg/100 g dry leaf) and ferulic acid (1.35 mg/100 g dry leaf), were optimized. The habanero pepper leaf extract obtained using a eutectic solvent and a sonic probe demonstrated a high potential for use as an ingredient in the development of nutraceuticals (i.e., functional foods).

This research aimed to optimize pressure (10–20 MPa) and temperature (45–60 °C) conditions for supercritical fluid extraction (SFE) of Makwaen pepper (Zanthoxylum myriacanthum) extract (ME) in comparison to conventional hydro-distillation extraction. Various quality parameters, including yield, total phenolic compounds, antioxidants, and antimicrobial activities of the extracts, were assessed and optimized using a central composite design. The optimal SFE conditions were found to be 20 MPa at 60 °C, which resulted in the highest yield (19%) and a total phenolic compound content of 31.54 mg GAE/mL extract. IC50 values for DPPH and ABTS assays were determined to be 26.06 and 19.90 μg/mL extract, respectively. Overall, the ME obtained through SFE exhibited significantly better physicochemical and antioxidant properties compared to ME obtained through hydro-distillation extraction. Gas chromatography-mass spectrometry (GC-MS) analysis revealed that beta-pinene was the major component in the ME obtained through SFE (23.10%), followed by d-limonene, alpha-pinene, and terpinen-4-ol at concentrations of 16.08, 7.47, and 6.34%, respectively. On the other hand, the hydro-distillation-extracted ME showed stronger antimicrobial properties than the SFE-extracted ME. These findings suggest that both SFE and hydro-distillation have the potential for extracting Makwaen pepper, depending on the intended purpose of use.

The recovery of valuable bioactive compounds from the main underutilised by-products of the food industry is one of the greatest challenges to be addressed in circular economy. Potato peels are the largest waste generated during potato processing. However, they could be a potential source of valuable bioactive compounds, such as polyphenols, that can be reused as natural antioxidants. Currently, environmentally benign enabling technologies and new types of non-toxic organic solvents for the extraction of bioactive compounds may dramatically improve the sustainability of these processes. This paper focuses on the potential inherent in the valorisation of violet potato peels (VPPs) by recovering antioxidants using natural deep eutectic solvents (NaDES) under ultrasound (US)- and microwave (MW)-assisted extraction. Both the enabling technologies provided performances that were superior to those of conventional extractions in terms of antioxidant activity determined by the DPPH· (2,2-diphenyl-1-picrylhydrazyl) assay. In particular, the most promising approach using NaDES is proven to be the acoustic cavitation with a Trolox eq. of 1874.0 mmolTE/gExtr (40 °C, 500 W, 30 min), vs. the 510.1 mmolTE/gExtr of hydroalcoholic extraction (80 °C, 4 h). The shelf-life of both hydroalcoholic and NaDES-VPPs extracts have been assessed over a period of 24 months, and found that NaDES granted a 5.6-fold shelf-life extension. Finally, the antiproliferative activity of both hydroalcoholic and NaDES-VPPs extracts was evaluated in vitro using the MTS assay on human tumour Caco-2 cells and normal human keratinocyte cells (HaCaT). In particular, NaDES-VPPs extracts exhibited a significantly more pronounced antiproliferative activity compared to the ethanolic extracts without a noteworthy difference between effects on the two cell lines.

The purpose of this study was to select the best green extraction technique to recover the bioactive compounds in Calabrian Bergamot waste (Pomace). Different experimental variables such as solvent, time, and temperature were tested and the main physicochemical characteristics and antioxidant activity and constituents, such as total flavonoids, individual flavonoids, and limonoids (UHPLC-DAD) were analyzed. Later, the best extraction methodology was applied to characterize the individual portions that compose the bergamot pomace (albedo/pulp, seeds, and juice) of three different Calabrian cultivars: Fantastico, Femminello, and Castagnaro. Results of this study evidence that bergamot waste possesses a high antioxidant content that can be potentially used for further applications in the food industry.

Perceived as a healthy food, almond beverages are gaining ever-increasing consumer preference across nonalcoholic vegetable beverages, ranking in first place among oilseed-based drinks. However, costly raw material; time and energy consuming pre- and posttreatments such as soaking, blanching and peeling; and thermal sterilization hinder their sustainability, affordability and spread. Hydrodynamic cavitation processes were applied, for the first time, as a single-unit operation with straightforward scalability, to the extraction in water of almond skinless kernels in the form of flour and fine grains, and of whole almond seeds in the form of coarse grains, up to high concentrations. The nutritional profile of the extracts matched that of a high-end commercial product, as well as showing nearly complete extraction of the raw materials. The availability of bioactive micronutrients and the microbiological stability exceeded the commercial product. The concentrated extract of whole almond seeds showed comparatively higher antiradical activity, likely due to the properties of the almond kernel skin. Hydrodynamic cavitation-based processing might represent a convenient route to the production of conventional as well as integral and potentially healthier almond beverages, avoiding multiple technological steps, while affording fast production cycles and consuming less than 50 Wh of electricity per liter before bottling.

The application of seaweed extract-based biostimulants is a promising approach for achieving sustainable agriculture, with an enormous potential of improving crop yield and mitigating climate change effects. Abiotic stressors, such as drought, are major factors resulting in tomato (Solanum lycopersicum L.) yield losses and seaweed-based biostimulants have been proposed as an eco-friendly strategy to counteract this negative impact. Chondrus crispus is a common red seaweed widely used as source of carrageenans, not yet explored as a plant biostimulant. In this study, a protein hydrolysate-rich C. crispus extract, by-products of the carrageenan extraction, was tested on tomato plants under well-watered condition and water shortage. The foliar application of the protein-rich C. crispus extract conferred drought tolerance to tomato plants resulting in less noticeable visual stress symptoms. Treated plants showed higher shoot height and biomass under both well-watered and water deficit conditions, evidencing the double effect exerted by this new biostimulant, as plant growth promoter and drought stress protector. The treatment with the biostimulant had an effect on levels of abscisic acid and proline, and triggered the expression of Solyc02g084840, a drought marker gene. Finally, a label-free mass spectrometric approach allowed us to identify phycoerythrins and phycocyanins as major bioactive proteins contained in the extract. Altogether, these results indicate that the foliar application of protein hydrolysate-rich extracts from C. crispus improved tomato plant growth and tolerance to drought stress, suggesting a new opportunity for further applications in the agriculture and horticultural sectors. Xunta de Galicia | Ref. ED431F 2020/01 COST | Ref. CA18224 Ministerio de Ciencia, Innovación y Universidades | Ref. RTI2018-096376-B-I00 Ministerio de Ciencia, Innovación y Universidades | Ref. PRE2019-090567 Ministerio de Ciencia, Innovación y Universidades | Ref. RYC2018-024454-I

The fruits of Rosa pimpinellifolia are rich sources of (poly)phenols, however they are underutilized due to the limited information available. The influence of the pressure, temperature, and co-solvent concentration (aqueous ethanol) of the supercritical carbon dioxide extraction (SCO2-aqEtOH) on the extraction yield, total phenolic-, total anthocyanin-, catechin-, cyanidin-3-O-glucoside contents, and total antioxidant activity of black rosehip was investigated simultaneously. The maximum obtained total phenolic and total anthocyanin contents under the optimized extraction conditions (280 bar, 60 °C and 25% ethanol, v/v) were 76.58 ± 4.25 mg gallic acid equivalent and 10.89 ± 1.56 mg cyanidin-3-O-glucoside equivalent per g of the dry fruits, respectively. The optimal extract obtained by SCO2-aqEtOH was compared to two other extraction procedures: ultrasonication using ethanol as solvent (UA-EtOH) and pressurized hot water extraction (PH-H2O). The bioaccessibility and cellular metabolism of the phenolic compounds in the different black rosehip extracts were assessed using an in vitro digestion coupled with a human intestinal Caco-2 cell model. The in vitro digestive stability and cellular uptake of the phenolic compounds had no significant difference among the different extraction methods. The results of this study confirm the efficiency of SCO2-aqEtOH extraction for phenolic compounds and, in particular, for anthocyanins, and could be used to produce new functional food ingredients from black rosehip with high antioxidant power containing both hydrophilic and lipophilic compounds.

The citrus industry produces large amounts of waste rich in bioactive compounds that have important effects on human health. Their extraction was performed using organic solvents, and a greener alternative to those solvents are natural deep eutectic solvents (NADES). The present study aimed to obtain and optimize extracts rich in polyphenols and flavonoids from orange peels using NADES and monitor polyphenol stability in the extracts for 30 days. The software COSMOtherm (conductor-like screening model) was used to screen fourteen NADES. The most promising solvents were lactic acid:glucose (LA:Glu) with an extraction yield of 1932 ± 7.83 mgGAE/100 gdw for TPC (total polyphenol content) and 82.7 ± 3.0 mg/100 gdw for TFC (total flavonoid content) and in the case of L-proline:malic acid (LP:MA) was 2164 ± 5.17 mgGAE/100 gdw for TPC and 97.0 ± 1.65 mg/100 gdw for TFC. The extraction process using LA:Glu and LP:MA was optimized, and the results showed that the selected variables (%NADES, solid:liquid ratio, and extraction time) had a significant influence on the extraction of TPC and TFC. Results showed that NADES improve the stability of TPC. These findings revealed that NADES are efficient for the extraction of bioactive compounds from orange by-products, and these extracts can represent an alternative for the food industry to enrich food products with natural ingredients. Ministry of Science and Innovation (Spain) State Research Agency (PID-2019-111331RB-I00/AEI/10.13039/501100011033) “Bicentennial Generation” scholarship from the Ministry of Education of the Republic of Peru of the national scholarship programme of PRONABEC 5.561 JCR (2021) Q1, 35/144 Food Sciences & Technology 0.726 SJR (2021) Q1, 69/338 Food Science No data IDR 2021 UEV

Artichoke wastes after processing represent 60–70% of the raw material and are a potential source of inulin and polyphenols, bioactive compounds that can be valorized as food ingredients or nutraceutical products. The aim of this work was to assess and optimize the extraction of these compounds from artichoke wastes using water or water–ethanol mixtures as extracting agents. For simultaneous inulin and polyphenol extraction and to achieve high antioxidant activity in extracts, the best process conditions using water as an extracting agent were T = 89 °C and t = 139 min, where 80% of the inulin content, 60% of the total phenolic content (TPC) and 56% of the antioxidant activity (Aox) were obtained. For water–ethanol extractions, the best results were obtained with EtOH = 22.4%, T = 81 °C and t = 217 min, leading to extraction yields of 90% of TPC, 38% of Aox and 58% of inulin content. From these results, we recommend the use of water for the recovery of inulin and polyphenols from artichoke wastes. Although the extraction yield of polyphenols is lower in water treatments, the amount extracted is considerable and it is a greener option when compared with water–ethanol mixtures.

Polyphenols are natural antioxidants and play a vital role in inhibiting oxidative stress induced by the body’s free radicals. Banana peels are a significant agro-industrial waste. This waste could be utilized to extract polyphenols to process various functional foods and nutraceuticals. An investigation was executed to extract polyphenols from banana peel using the sonication and maceration techniques. Three different polar solvents, methanol, ethanol and acetone, were used at four different concentrations: 25%, 50%, 75% and 100%. Yield (%), Total Polyphenolic Content (TPC), Total Flavonoid Content (TFC) and 1,1-diphenyl-2-picryl-hydrazyl (DPPH) Radical Scavenging assays were performed. The results from the current study articulate that extraction by sonication yields a higher quantity of polyphenols than the maceration technique. The study also concludes that ethanol leads to better extraction than other solvents used in this study.

Carob syrup is one of the most important carob products, which can have applications in pastry and confectionery, as a fruit preservative, but also in the pharmaceutical field because of the antimicrobial activity due to its polyphenol content. Carob syrup is traditionally made through a very time-consuming process, involving solid–liquid extraction in boiling water and concentration at a high temperature (>100 °C), which potentially causes the degradation of the active compounds (i.e., procyanidins or flavonol glycosides). Therefore, in this work, an alternative and less drastic method based on ultrasound technology was proposed to produce carob syrup. Processing conditions (i.e., time, temperature, and liquid–solid ratio) influencing the extraction of total soluble solids (TSS) and total phenolic compounds (TPC) were optimized using a central composite design coupled to response surface methodology. Reliable mathematical models allowed us to predict the highest TSS (24 ± 2 °Brix) and TPC (1.7 ± 0.5 mg/mL) values that could be obtained at 15 min, 35 °C, and 2 mL/g. Finally, a different HPLC-DAD phenolic pattern was determined between syrups produced by traditional and ultrasound methods; epicatechin, 4-hydroxycoumaric acid, and ferulic acid were more concentrated in the former, while procyanidin B2, myricitrin, and quercitrin were prevalent in the latter one.

In this study, deep eutectic solvents (DESs) were synthesized using different ratios of choline chloride (CC) and dicarboxylic acids, and their eutectic temperatures were determined. The DES synthesized using CC and glutaric acid (GA), which showed a higher extraction efficiency than conventional solvents, was used for the extraction of flavonoid components from Pyrus ussuriensis leaves (PUL), and the extraction efficiency was evaluated using the response surface methodology. The flavonoid components rutin, hyperoside, and isoquercitrin were identified through high-performance liquid chromatography (HPLC), equipped with a Waters 2996 PDA detector, and HPLC mass spectrometry (LC-MS/MS) analyses. The optimum extraction was achieved at a temperature of 30 °C using DES in a concentration of 30.85 wt.% at a stirring speed of 1113 rpm and an extraction time of 1 h. The corresponding flavonoid content was 217.56 μg/mL. The results were verified by performing three reproducibility experiments, and a high significance, with a confidence range of 95%, was achieved. In addition, the PUL extracts exhibited appreciable antioxidant activity. The results showed that the extraction process using the DES based on CC and GA in a 1:1 molar ratio could effectively improve the yield of flavonoids from PUL.

We are now seeing an increase in the production of agri-food waste, which is an essential resource for the recovery of bioactive compounds that may be employed as innovative natural ingredients in cosmetics. To date, the approach to cosmetics preservation has seen a significant shift in the search for biological components that give healthier alternatives for customers and help businesses operate in an environmentally friendly manner. To achieve this goal, we studied pomegranate extracts using the peel and, for the first time, extracts from the male flowers of a wide pomegranate variety cultivated in the Marche region, specifically, the Wonderful, Mollar de Elche, Parfianka, and less-studied G1 varieties. We studied the phenol compounds profile, antioxidant capacity, antimicrobial activity, and cell viability of the obtained pomegranate extracts. The identification and quantification of phenol compounds belonging to different classes, such as hydrolysable tannins, hydroxybenzoic acid, hydroxycinnamic acid, dihydroflavonol, gallocatechin, and anthocyanins, were performed using UPLC-ESI-MS/MS. Punicalagin isomers and punicalin resulted in the most abundant polyphenols found in the peel and male flower extracts. Mollar de Elche 2020 peel extract revealed a high concentration of punicalagin A and B (7206.4 mg/kg and 5812.9), while the content of gallic acid revealed high results in the G1 and Parfianka varieties. All extracts were spectrophotometrically analysed to determine their total phenol content (TPC) using the Folin–Ciocalteu method and their antioxidant capacity (AC). In terms of the total phenol obtained by the Folin–Ciocalteu colorimetric method, Mollar de Elche 2020 extracts reported the highest TPC content of 12.341 µmol GAE/g. Results revealed that the Mollar de Elche and Wonderful 2020 peel extracts demonstrated the highest TPC and AC. Furthermore, AC results indicated that the peel extracts displayed higher AC than the male flower extract due to the high punicalagin content detected by UPLC analysis. The antimicrobial activity testing revealed that the Wonderful and G1 2020 peel extracts resulted active against Escherichia coli, while all extracts exhibited promising anticandidal activity. Additionally, the cytocompatibility was evaluated in keratinocytes HaCaT cells by testing concentrations of pomegranate extracts ranging from 0.15 to 5.00 mg/mL. Extracts were non-toxic for the cells in the tested concentration range. The acquired results may help exploit pomegranate agri-food waste products provided by the Marche region’s short supply chain for their use as an antimicrobial and antioxidant booster in the formulation of cosmetic products.

Kiwifruit (Actinidia chinensis) is a nutrient-dense fruit abundant in vitamin C and phenolic compounds, and it exhibits strong antioxidant capacity. However, the antioxidants in ‘Jinfeng’ kiwifruit have seldom been extracted and analyzed, and the conditions for the extraction of kiwifruit antioxidants by ultrasound-assisted extraction (UAE) have seldom been investigated. In this study, response surface methodology (RSM) was used to optimize UAE conditions to extract antioxidants from ‘Jinfeng’ kiwifruit. In addition, the antioxidant capacity, contents of total phenolics and total flavonoids, ascorbic acid, and the profiles of antioxidants were also analyzed. The results showed that the optimal UAE conditions included 68% ethanol, liquid/solid ratio at 20 mL/g, extraction time at 30 min, extraction temperature at 42 °C, and ultrasonic power at 420 W. Under these conditions, the ABTS value of kiwifruit was 70.38 ± 1.38 μM TE/g DW, which was 18.5% higher than that of the extract obtained by conventional solvent extraction. The total phenolic and flavonoid contents were 15.50 ± 0.08 mg GAE/g DW and 5.10 ± 0.09 mg CE/g DW, respectively. Moreover, 20 compounds were tentatively identified by UPLC–MS/MS, and the content of main compounds, such as procyanidin B2, neochlorogenic acid, and epicatechin, were determined by HPLC–DAD. This research revealed the profiles of antioxidant phytochemicals in ‘Jinfeng’ kiwifruit, which can be a good dietary source of natural antioxidants with potential health functions.

Nelumbo nucifera Gaertn., or the so-called sacred lotus, is a useful aquatic plant in the Nelumbonaceae family that has long been used to prepare teas, traditional medicines as well as foods. Many studies reported on the phytochemicals and biological activities of its leaves and seeds. However, to date, only few studies were conducted on its stamen, which is the most important ingredient for herbal medicines, teas and other phytopharmaceutical products. Thus, this present study focuses on the following: (1) the application of high-performance liquid chromatography with photodiode array detection for a validated separation and quantification of flavonoids from stamen; (2) the Nelumbo nucifera stamen’s in vitro and in cellulo antioxidant activities; as well as (3) its potential regarding the inhibition of skin aging enzymes for cosmetic applications. The optimal separation of the main flavonoids from the stamen ethanolic extract was effectively achieved using a core-shell column. The results indicated that stamen ethanolic extract has higher concentration of in vitro and in cellulo antioxidant flavonoids than other floral components. Stamen ethanolic extract showed the highest protective effect against reactive oxygen/nitrogen species formation, as confirmed by cellular antioxidant assay using a yeast model. The evaluation of potential skin anti-aging action showed that the stamen extract has higher potential to inhibit tyrosinase and collagenase compared with its whole flower. These current findings are the first report to suggest the possibility to employ N. nucifera stamen ethanolic extract as a tyrosinase and collagenase inhibitor in cosmetic applications, as well as the utility of the current separation method.

14 pages, 3 figures, 2 tables.-- This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license, A novel approach of bioactive lipid extraction by different green solvents was carried out on squid (Doryteuthis gahi) by-products. By-products (viscera, heads, skin, tails, etc.), considered as a single product, were subjected to the following solvent systems: ethanol, acetone, ethyl acetate, 1/1 ethanol/acetone, 1/1 ethanol/ethyl acetate, and 1/1 acetone/ethyl acetate. Analyses carried out included lipid yield, lipid class content, and fatty acid (FA) composition. Results were compared to the lipid extract obtained by the traditional procedure (1/1 chloroform/methanol). Lipid yields obtained by green solvents led to a 33.4–73.2% recovery compared to traditional extraction; the highest values (p < 0.05) were obtained by ethanol-containing systems. Compared to the traditional procedure, ethanol systems showed an 85.8–90.3% recovery of phospholipid compounds and no differences (p > 0.05) in the ω3/ω6 ratio. Green-extracting systems led to higher average values for eicosapentaenoic acid content (15.66–18.56 g·100 g−1 total FAs) and polyene index (1.93–3.29) than chloroform/methanol extraction; differences were significant (p < 0.05) for systems including acetone and ethyl acetate. No differences (p > 0.05) were detected for docosahexaenoic acid content between the traditional procedure and green systems, with all values being included in the 31.12–32.61 g·100 g−1 total FA range. The suitability of EtOH-containing green systems for extraction of bioactive lipid compounds from squid by-products was concluded, This research was funded by the SPANISH MINISTRY OF RESEARCH AND INNOVATION, grant number RTI2018-095659-B-I00 (2019–2022), and the APC was partially funded by the Spanish National Research Council (CSIC)

Until now, the red algae Gelidium sesquipedale has been primarily exploited for agar production, leaving an undervalued biomass. In this work, the use of eco-friendly approaches employing ultrasound-assisted extraction (UAE) and green solvents was investigated to valorize the algal minor compounds. The green methods used herein showed an attractive alternative to efficiently extract a broad spectrum of bioactive compounds in short extraction times (15 to 30 min vs. 8 h of the conventional method). Using the best UAE conditions, red seaweed extracts were characterized in terms of total phenolics (189.3 ± 11.7 mg GAE/100 g dw), flavonoids (310.7 ± 9.7 mg QE/100 g dw), mycosporine-like amino acids (MAAs) (Σ MAAs = 1271 mg/100 g dw), and phycobiliproteins (72.4 ± 0.5 mg/100 g dw). Additionally, produced algal extracts exhibited interesting antioxidant and anti-enzymatic activities for potential applications in medical and/or cosmetic products. Thus, this study provides the basis to reach a superior valorization of algal biomass by using alternative methods to extract biologically active compounds following eco-friendly approaches. Moreover, the strategies developed not only open new possibilities for the commercial use of Gelidium sesquipedale, but also for the valorization of different algae species since the techniques established can be easily adapted.

The current study evaluates the Pulsed Electric Field (PEF) technique for the extraction of polyphenols from the plants Rosa canina, Calendulaofficinalis and Castanea sativa. These plants are traditionally used both for the preparation of therapeutic decoctions and the aromatization of beverages (alcoholic or not). Pulses of 10 μs duration were used to apply electric field intensities ranging from 1.2 to 2.0 kV cm−1. The period of the phenomenon was set to 1 ms, with a total extraction time of 20 min. The total polyphenol content as well as the identified polyphenolic compounds of the extracts were determined for monitoring and evaluation. To estimate the PEF effect, control extracts were prepared using the same process as PEF extracts but without the application of electric field. For all the three plant materials studied, the PEF technique appeared to be successful in increasing polyphenols extraction. The application of a moderate to high electric field, up to 1.4 kV cm−1, resulted in increased total and individual polyphenols recovery, reaching 63.79% and 84%, respectively, in the case of Rosa canina fruits.

Olive leaves (OLL), an agricultural waste by-product, are considered a significant bioresource of polyphenols, known as bioactive compounds. This study evaluates the pulsed electric field (PEF) technique for the extraction of polyphenols from OLL. The study parameters included a series of “green” solvents (ethanol, water as well as mixtures of them at a 25% step gradient) and different input values for the pulse duration of PEF. The phytochemical extraction degree was evaluated using total phenol concentration (Folin–Ciocalteu method) and high-performance liquid chromatography (HPLC) analyses, while the antioxidant activity was assessed using differential scanning calorimetry (DSC). The results obtained from the PEF extracts were compared with those of the extracts produced without the PEF application. The highest PEF effect was observed for aqueous ethanol, 25% v/v, using a pulse duration of 10 μs. The increase in the total polyphenols reached 31.85%, while the increase in the specific metabolites reached 265.67%. The recovery in polyphenols was found to depend on the solvent, the pulse duration of treatment and the structure of the metabolites extracted.

A comparative study of bioactive lipids extraction from black cumin (Nigella sativa L.) and basil (Ocimum basilicum L.) seeds using conventional petroleum-based solvent and green solvent 2-methyltetrahydrofuran (MeTHF) was performed. MeTHF extraction allowed obtaining the highest oil yield in black cumin (34%). Regarding fatty acids composition, linoleic acid (61%) and α-linolenic (78%) were relevant in black cumin and basil green and conventionally extracted oils, respectively. Besides, MeTHF allowed obtaining higher tocopherols and total phenolics contents in black cumin (400 mg/kg of oil and 12 mg EGA/g oil) and basil (317 mg/kg oil and 5 mg EGA/g oil) compared to hexane-extracted ones. The content of major phenolic compounds in the two seed oils, trans-hydroxycinnamic acid, rosmarinic acid, and thymol was enhanced by MeTHF extraction. Furthermore, MeTHF-extracted oils possess stronger antioxidant activities (radical scavenging, total antioxidant, and β-carotene bleaching activities) and high and similar anti-inflammatory capacity to hexane-extracted oils. In conclusion, the results revealed that MeTHF is efficient to replace hazardous solvents to extract oil from black cumin and basil seeds rich in compounds relevant to the human diet, including essential polyunsaturated fatty acids (n-6 and n-3), tocopherols, and phenolic compounds with improved biological activities.

Larch (Larix decidua) bark is a sawmill waste, traditionally used for antiseptic, expectorant and dermatological (wound healing, eczema, psoriasis) purposes. In this work, we developed a food-grade dry larch bark extract (LBE) from sawmill by-products using hydro-alcoholic extraction. The antibacterial activity of LBE was evaluated against respiratory-tract pathogens, i.e. Staphylococcus aureus, Streptococcus pyogenes, Streptococcus pneumoniae, Klebsiella pneumoniae, Pseudomonas aeruginosa and Haemophilus influenza, and it was compared to that of grapefruit seed extract (GSE), a commercially available raw material commonly proposed as antibacterial ingredient for over-the-counter products. Procyanidins (PACs) and other polyphenols contents in LBE were determined by HPLC-FLD-MS and HPLC-DAD-MSn, respectively. The antimicrobial activity of LBE and GSE was assessed using the micro-plate dilution technique in concentration range of 2–200 µg/mL, and the safety of these dosages was assessed in cellular and animal models. LBE showed considerable contents of PACs (15% w/w, especially B-type) and other polyphenols (3.8% w/w), among which the characteristic spiropolyphenols larixinol and epilarixinol were identified, together with the flavonoids isoquercitrin and rutin, already reported as growth inhibitors of different respiratory-tract pathogens. LBE showed higher antimicrobial activity compared to GSE, demonstrated by a growth inhibition range of 10–40% towards five of six strains tested, compared to 10–15% of GSE. These results suggest that LBE may represent a natural and sustainable source of active compounds with antibacterial activity for pharmaceutical and nutraceutical applications.

This study exploited the application of pulsed electric field (PEF) on the recovery of polyphenols from aerial parts of Sideritis scardica, tepals of Crocus sativus, and fruits of Vitis vinifera. Short pulses of 10 μs in a period of 1 ms were applied to the plant material, while different electric field intensities, 1.2 to 2.0 kV/cm were tested to optimize the procedure. The content in total polyphenols and the polyphenolic profile of the plant extracts were evaluated. Along with PEF samples, control samples were prepared for comparison. PEF treatment enhanced the recovery in total polyphenols for all the three plants examined. A significant increase was noticed in each plant tested and PEF condition applied, though lower electric field intensities up to 1.4 kV/cm proved to be more effective. Under the optimum electric field intensities, 1.4 kV/cm for V. vinifera and 1.2 kV/cm for S. scardica and C. sativus, increases of 49.15%, 35.25%, and 44.36% in total polyphenol content, respectively, were achieved. Additionally, an 85% increase of quercetin 3-rutinoside for V. vinifera, a 56% of apigenin 7-O-glucoside for S. scardica, and a 64% increase for kaempferol 3-O-glucoside for C. sativus were obtained.

Extracts rich in bioactive compounds added to edible films have allowed the development of active packaging that increases the shelf life of food. However, it is necessary to search for solvents that are nontoxic and not harmful to the environment, with natural deep eutectic solvents (NADES) being an attractive and easily synthesized alternative. This research aimed to design NADES by lyophilization to be used in the extraction of anthocyanins from the Chilean Luma chequen (Molina) A. Gray berry, and subsequently adding them to the matrix of edible ƙ-carrageenan films. For this purpose, ultrasound-assisted extraction (UAE) was used and the anthocyanin content was evaluated with the pH differential method. The antioxidant capacity of extracts was determined by DPPH assay and the antibacterial capacity by diffusion agar tests. The results obtained indicate that the designed NADES are efficient at extracting anthocyanins, reaching concentrations between 81.1 and 327.6 mg eq cyanidin 3-glucoside/100 g dw of L. chequen (Molina) A. Gray. The extracts reached inhibition diameters between 5 and 34 mm against Escherichia coli, Staphylococcus aureus, and Salmonella typhi strains. Once the extracts were incorporated into ƙ-carrageenan films, active edible films with antioxidant and antibacterial capacities were obtained.

Renewable feedstock from perennial industrial crops, including those cultivated on marginal land in a short-rotation coppice system, could be an important contribution to the bioeconomy. The majority of data available on the topic are limited to the production of bioenergy from this type of biomass. According to the concept of bioeconomy, biomass-based bioproducts have priority over energy production. This paper characterizes the chemical composition and antioxidant activity of extracts from bark (b), wood (w) or a mixture of bark and wood (b + w) from Salix purpurea, Salix viminalis and Populus nigra obtained using supercritical carbon dioxide (scCO2), scCO2 and water (1%, w/w) or only water. Generally, a high concentration of polyphenols was obtained after extraction with scCO2 and water, while the lowest concentration was found in extracts obtained with scCO2. The highest concentration of polyphenols (p &lt, 0.05) was obtained in an extract from P. nigra (b) (502.62 &plusmn, 9.86 mg GAE/g dry matter (d.m.)) after extraction with scCO2 and water, whereas the lowest polyphenol concentration was observed in an scCO2 extract from S. purpurea (b) (6.02 &plusmn, 0.13 mg GAE/g d.m.). The flavonoids were effectively separated by extraction with scCO2 (0.88&ndash, 18.37 mg QE/g d.m.). A positive linear relationship between the antioxidant activity determined by DPPH and ABTS assays and the concentration of polyphenols was demonstrated, R2 = 0.8377 and R2 = 0.9568, respectively. It is most probable that the concentration of flavonoids, rather than the concentration of polyphenols, determines the chelating activity of Fe2+. The Fe2+-chelating activity of scCO2 extracts ranged from 75.11% (EC50 = 5.41 mg/cm3, S. purpurea, b + w) to 99.43% (EC50 = 0.85 mg/cm3, P. nigra, b + w). The lowest chelating activity was demonstrated by the extracts obtained with scCO2 and water (maximum 26.36%, S. purpurea, b + w). In extracts obtained with scCO2 and water, p-hydroxybenzoic acid (210&ndash, 428 &micro, g/g), p-coumaric acid (56&ndash, 281 &micro, g/g), saligenin (142&ndash, 300 &micro, g/g) and salicortin (16&ndash, 164 &micro, g/g) were the dominant polyphenols. All of these chemical compounds occurred mainly in the free form. The S. purpurea, S. viminalis and P. nigra biomass proved to be an attractive source of biologically active compounds for various possible applications in food, drugs or cosmetics. These compounds could be extracted using an environmentally friendly method with scCO2 and water as a co-solvent.

Aqueous solutions of ionic liquids (ILs) with surface active properties were used as extraction solvents, taking advantage of their impressive solvation properties, in a green microwave-assisted solid-liquid extraction method (IL-MA-SLE) for the extraction of flavonoids from passion fruit and mango leaves. The extraction method was combined with high-performance liquid chromatography and photodiode-array detection (HPLC-PDA) and optimized by response surface methodology using the Box-Behnken experimental design. Under optimum conditions, the extraction efficiency of six structurally different IL-based surfactants was evaluated. Thus, imidazolium-, guanidinium- and pyridinium-type ILs with different tailorable characteristics, such as side chain length and multicationic core, were assessed. The decylguanidinium chloride ([C10Gu+][Cl&ndash, ]) IL-based surfactant was selected as key material given its superior performance and its low cytotoxicity, for the determination of flavonoids of several samples of Passiflora sp. and Mangifera sp. leaves from the Canary Islands, and using as target analytes: rutin, quercetin and apigenin. The analysis of 50 mg of plant material only required 525 &micro, L of the low cytotoxic IL-based surfactant solution at 930 mM, 10.5 min of microwave irradiation at 30 &deg, C and 50 W, which involves a simpler, faster, more efficient and greener method in comparison with other strategies reported in the literature for obtaining bioactive compounds profiles from plants.

The objective of this study was to evaluate the potential of green solvents for extractions of bioactive compounds (BACs) and essential oils from wild thyme (Thymus serpyllum L.) using theoretical and experimental procedures. Theoretical prediction was assessed by Hansen solubility parameters (HSPs) and conductor-like screening model for realistic solvents (COSMO-RS), to predict the most suitable solvents for extraction of BACs. An experimental procedure was performed by nonthermal technology high voltage electrical discharge (HVED) and it was compared with modified conventional extraction (CE). Obtained extracts were analyzed for chemical and physical changes during the treatment. Theoretical results for solution of BACs in ethanol and water, as green solvents, were confirmed by experimental results, while more accurate data was given by COSMO-RS assessment than HSPs. Results confirmed high potential of HVED for extraction of BACs and volatile compounds from wild thyme, in average, 2.03 times higher yield of extraction in terms of total phenolic content was found compared to CE. The main phenolic compound found in wild thyme extracts was rosmarinic acid, while the predominant volatile compound was carvacrol. Obtained extracts are considered safe and high-quality source reach in BACs that could be further used in functional food production.

This paper proposes a new sustainable and simple strategy for the micro-scale extraction of phenolic compounds from grapevine leaves with analytical purpose. The method is based on a microwave-assisted solid-liquid extraction approach (MA-SLE), using an aqueous solution of an ionic liquid (IL)-based surfactant as extraction phase. The method does not require organic solvents, nor any clean-up step, apart from filtration prior to the injection in the analytical system. Two IL-based surfactants were evaluated, and the method was optimized by using experimental designs, resulting in the use of small amounts of sample (100 mg) and extraction phase (2.25 mL), low concentrations of the selected 1-hexadecyl-3-butyl imidazolium bromide IL (0.1 mM), and 30 min of extraction time. The proposed methodology was applied for the determination of the polyphenolic pattern of six different varieties of Vitis vinifera leaves from the Canary Islands, using high-performance liquid chromatography and photodiode array detection for the quantification of the compounds. The proposed MA-SLE approach was greener, simpler, and more effective than other methods, while the results from the analysis of the leaves samples demonstrate that these by-products can be exploited as a source of natural compounds for many applications.

Natural deep eutectic solvents (NaDESs) are recently developed green solvent alternatives to conventional fossil solvents. The present work systematically screened 22 different NaDESs for the ultrasonic-assisted extraction of bioactive components from Salvia miltiorrhiza (SM), a widely used traditional Chinese medical plant. The suitable solvent and extraction condition were optimized in a two-round screening. In comparison with fossil solvents, NaDESs, especially L-proline-lactic acid (L-Pro-Lac) showed significant advantages in the extraction of salvianolic acid B (SAB), tanshinone IIA (TIIA) and cryptotanshinone (CYT). The optimized yields of the three targeting compounds were 42.05, 1.485 and 0.839 mg/g, respectively. The present method was also applied to the pretreatment of SM samples from different geographic origins. The 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging activities of NaDES extracts were determined in the study to prove the feasibility of NaDES in bioactive component extraction. The application of NaDESs in the extraction of both hydrophilic and hydrophobic small molecules from SM is proved to be a green and efficient method for pretreatment of herbal materials.

The aim of this work is the evaluation of a green extraction technology to exploit winery waste byproducts. Specifically, a solid&ndash, liquid extraction technology (Naviglio Extractor&reg, ) was used to obtain polyphenolic antioxidants from the Cagnulari grape marc. The extract was then chemically characterized by spectrophotometric analysis, high-performance liquid chromatography, and mass spectrometry, revealing a total polyphenol content of 4.00 g/L &plusmn, 0.05, and the presence of anthocyanins, one of the most representative groups among the total polyphenols in grapes. To investigate potential biological activities of the extract, its ability to counteract hydrogen peroxide-induced oxidative stress and cell death was assessed in primary human endothelial cells. The 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) test, used to assess potential extract cytotoxicity, failed to show any deleterious effect on cultured cells. Fluorescence measurements, attained with the intracellular reactive oxygen species (ROS) probe 2&prime, 7&prime, dichlorodihydrofluorescein diacetate (H2DCF-DA), revealed a strong antioxidant potential of the marc extract on the used cells, as indicated by the inhibition of the hydrogen peroxide-induced ROS generation and the counteraction of the oxidative-induced cell death. Our results indicate the Naviglio extraction, as a green technology process, can be used to exploit wine waste to obtain antioxidants which can be used to produce enriched foods and nutraceuticals high in antioxidants.