Search

In the olive oil industry, a pit fraction is collected from olive pomace and split into a clean pit fraction and a residual olive skin-rich fraction, which does not an industrial application. Therefore, in this work, microwave-assisted extraction (MAE) was applied to obtain high-value triterpene acids (maslinic acid and oleanolic acid) from this biomass using the renewable solvent ethanol. The response surface methodology was used to gain a deeper understanding of how the solvent (ethanol–water, 50–100% v/v), time (4–30 min), and temperature (50–120 °C) affect the extraction performance, as well as the energy required for the process. The effect of milling was also studied and the solid-to-liquid ratio was also evaluated, and overall, a good compromise was found at 10% (w/v) using the raw sample (unmilled biomass). The optimised conditions were applied to residual olive skin sourced from various industries, yielding up to 5.1 g/100 g and 2.2 g/100 g dry biomass for maslinic acid and oleanolic acid, respectively. In conclusion, the residual olive skin is a promising natural source of these triterpene acids, which can be extracted using MAE, releasing extracted solids rich in polymeric carbohydrates and lignin that can be valorised under a holistic biorefinery process. [ABSTRACT FROM AUTHOR]

In the olive oil industry, a pit fraction is collected from olive pomace and split into a clean pit fraction and a residual olive skin-rich fraction, which does not an industrial application. Therefore, in this work, microwave-assisted extraction (MAE) was applied to obtain high-value triterpene acids (maslinic acid and oleanolic acid) from this biomass using the renewable solvent ethanol. The response surface methodology was used to gain a deeper understanding of how the solvent (ethanol–water, 50–100% v/v), time (4–30 min), and temperature (50–120 °C) affect the extraction performance, as well as the energy required for the process. The effect of milling was also studied and the solid-to-liquid ratio was also evaluated, and overall, a good compromise was found at 10% (w/v) using the raw sample (unmilled biomass). The optimised conditions were applied to residual olive skin sourced from various industries, yielding up to 5.1 g/100 g and 2.2 g/100 g dry biomass for maslinic acid and oleanolic acid, respectively. In conclusion, the residual olive skin is a promising natural source of these triterpene acids, which can be extracted using MAE, releasing extracted solids rich in polymeric carbohydrates and lignin that can be valorised under a holistic biorefinery process.

The present study aimed to evaluate the efficacy of natural deep eutectic solvents (NADESs) on the extraction of phytochemicals from eight Algerian date fruit cultivars (Phoenix dactylifera L.). In this study, lactic acid/sucrose-based NADESs were used as an alternative to conventional chemical solvents using the ultrasound-assisted extraction (UAE) method. The obtained extracts were assessed for the determination of bioactive compound contents, phenolic composition, antioxidant activity, and enzyme inhibitory potential. The results showed a considerable variation in phytochemical compositions and related activities between cultivars, where the greatest contents of total phenolics (1288.7 mg GAE/100 g), total flavonoids (53.8 mg QE/100 g), proanthocyanidins (179.5 mg CE/g), and total triterpenoids (12.88 mg OAE/100 g) were detected in the fruits of the Ourous cultivar. The same cultivar displayed the highest antioxidant capacity against DPPH• free radical (595 mg AAE/100 g), ABTS•+ cation radical (839 mg TE/100 g), and ferric reducing antioxidant potential (704 mg AAE/100 g). All extracts manifested moderate antioxidant activities tested by phosphomolybdenum, NO•, and linoleic acid lipid peroxidation assays. These extracts also exhibited interesting levels of in vitro enzyme inhibition; the Ourous cultivar gave the best inhibitory activity against α-amylase and acetylcholinesterase with 45 and 37%, respectively. HPLC-DAD-MS detected a total of five compounds, with phenolic acids and flavonoids being the main phenolics identified in the extract. The phenolic composition exhibited significant variability among cultivars. Notably, the highest amounts were revealed in the Tazizaout cultivar, with the predominance of gallic acid. The results confirmed that the combination of UAE and NADESs provides a novel and important alternative to chemical solvents for sustainable and environmentally friendly extraction and can represent a good alternative in food and pharmaceutical industry applications. [ABSTRACT FROM AUTHOR]

Given today's increasingly intensive agriculture, one key problem area considers the valorization and reuse of wastes from food and agricultural production with minimal impact on the environment. Due to its physicochemical characteristics, biochar (BC) derived from grapevine pruning residue has shown considerable potential for use as an adsorbent. High-value phytochemicals found in abundance in the olive leaf (OL) can be employed in many different industrial sectors. The potential application of BC in the removal of specific polyphenolic components from OL extracts has been investigated in the present study. Water, as the most available and greenest of solvents, was investigated as to its use in the extraction of polyphenols, which was carried out by comparing maceration, ultrasound-assisted extraction, and microwave-assisted extraction, considering different temperatures and solid-to-liquid (s/l) ratios. The BC adsorption capacity of selected polyphenols was fitted with both the Langmuir and Freundlich isotherm models. The Freundlich model fitted better relative to OL polyphenols adsorption. Oleuropein was the most abundant compound identified in the extracts, obtaining the highest Kf value (20.4 (mg/g) × (L/g)n) and R2 coefficient (0.9715) in the adsorption on the biochar's surface. The optimum conditions in the dosage experiment suggest the use of 0.5 g of BC using 3 g/L extracts, with an exception for oleuropein and hydroxytyrosol, for which the highest biochar dose (2.5 g) performed better. Considering the compounds' concentrations and the BC dose, BC from grapevine pruning residues demonstrated a potential use in the uptake of specific polyphenols from olive leaves, making it a promising adsorbent for such applications. [ABSTRACT FROM AUTHOR]

The mangosteen (Garcinia mangostana L.) pericarp is known to be rich in potent bioactive phytochemical compounds such as xanthones, which possess pharmacologically important antioxidant activity and beneficial cardiometabolic properties. Mangosteen pericarp is typically classified as unavoidable food waste and discarded, despite being rich in bioactive phytochemical compounds that therefore present an exciting opportunity for valorization. Thus, this study aims to extract phytochemical compounds from mangosteen pericarp using pressurized hot water extraction (PHWE) and determine its biological effects in endothelial cells using RNA sequencing. Liquid chromatography with MS/MS (LC/MSMS) and UV detection (LC/UV) was subsequently used to identify three key phytochemical compounds extracted from the mangosteen pericarp: α-Mangostin, γ-Mangostin, and Gartanin. Within the tested range of extraction temperatures by PHWE, our results demonstrated that an extraction temperature of 120 °C yielded the highest concentrations of α-Mangostin, γ-Mangostin, and Gartanin with a concomitant improvement in antioxidant capacity compared to other extraction temperatures. Using global transcriptomic profiling and bioinformatic analysis, the treatment of endothelial cells with mangosteen pericarp extracts (120 °C PHWE) for 48 h caused 408 genes to be differentially expressed. Furthermore, our results demonstrated that key biological processes related to "steroid biosynthesis and metabolism", likely involving the activation of the AMPK signaling pathway, were upregulated by mangosteen pericarp extract treatment. In conclusion, our study suggests a green extraction method to valorize phytochemical compounds from mangosteen pericarp as a natural product with potential beneficial effects on cardiometabolic health. [ABSTRACT FROM AUTHOR]

Pomegranate (Punica granatum L.) is well known for its high content of bioactives, including polyphenols, flavonoids, and tannins, which have been shown to exhibit a wide range of biological activities, such as antioxidant, antimicrobial, and anticancer effects. It is worth noting that the majority of these molecules are found in the peels, which are usually disposed of after processing, causing a significant amount of waste, amounting to more than 3.6 million t/y. This work investigates microwave-assisted extraction (MAE) in water for the recovery of antioxidants from pomegranate peels (PP), including the optimisation of temperature and extraction times. The total phenolic, anthocyanin, flavonoid, and tannin contents of the recovered extracts were determined, as well as their antioxidant activities, which were found to be 356.35 mgGAE/gExtr, 303.97 µgCy3G/gExtr, 37.28 mgQE/gExtr, 56.48 mgGAE/gExtr, and 5.72 mmolTE/gExtr, respectively (according to the adopted reference). All results were compared with those obtained using a conventional protocol. In addition, the potential for water recycling by means of downstream nanofiltration in optimised MAE was investigated, leading to overall water reuse of approx. 75%. Power consumption (20.92 W/mgGAE) and common green metrics, Reaction Mass Efficiency (RME), E-Factor, and the Process Mass Intensiti/efficiency (PMI, PME), were considered in evaluating the proposed PP valorisation strategy. Finally, the biological activities of the main products were assessed. The antimicrobial properties of the PP extracts against three Gram-positive and three Gram-negative bacteria and their antiproliferative activity towards human cancer cells were tested. S. aureus bacteria was the most susceptible to the PP extracts. All tested products displayed antiproliferative activity against HeLa cells when higher concentrations were tested, with D-PP/NF (obtained from dried PP and sequential nanofiltration) being the most effective. This result was also confirmed via clonogenic analysis, which generally indicated the possible anti-cancer activity of pomegranate peel extracts obtained using this green approach. [ABSTRACT FROM AUTHOR]

Hydrodynamic cavitation (HC), as an effective, efficient, and scalable extraction technique for natural products, could enable the affordable production of valuable antioxidant extracts from plant resources. For the first time, whole pomegranate (Punica granatum L.) fruits, rich in bioactive phytochemicals endowed with anti-cancer properties, were extracted in water using HC. Aqueous fractions sequentially collected during the process (M1–M5) were lyophilized (L), filtered (A), or used as such, i.e., crude (C), and analyzed for their biochemical profile and in vitro antioxidant power. The fractions M3 and M4 from the L and C series showed the highest antiradical activity and phytochemical content. While the lyophilized form is preferable for application purposes, sample L-M3, which was produced faster and with lower energy consumption than M4, was used to assess the potential antiproliferative effect on human breast cancer line (AU565-PAR) and peripheral blood mononuclear (PBMC) cells from healthy donors. In a pilot study, cell growth, death, and redox state were assessed, showing that L-M3 significantly reduced tumor cell proliferation and intracellular oxygen reactive species. No effect on PBMCs was detected. Thus, the antioxidant phytocomplex extracted from pomegranate quickly (15 min), at room temperature (30 °C), and efficiently showed potential anticancer activity without harming healthy cells. [ABSTRACT FROM AUTHOR]

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. [ABSTRACT FROM AUTHOR]

Agri-food industries generate a large amount of waste that offers great revalorization opportunities within the circular economy framework. In recent years, new methodologies for the extraction of compounds with more eco-friendly solvents have been developed, such as the case of natural deep eutectic solvents (NADES). In this study, a methodology for extracting phenolic compounds from olive tree leaves using NADES has been optimized. The conditions established as the optimal rely on a solvent composed of choline chloride and glycerol at a molar ratio of 1:5 with 30% water. The extraction was carried out at 80 °C for 2 h with constant agitation. The extracts obtained have been analyzed by high-performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) in MRM mode. The comparison with conventional ethanol/water extraction has shown that NADES, a more environmentally friendly alternative, has improved extraction efficiency. The main polyphenols identified in the NADES extract were Luteolin-7-O-glucoside, Oleuropein, 3-Hydroxytyrosol, Rutin, and Luteolin at the concentrations of 262, 173, 129, 34, and 29 mg kg−1 fresh weight, respectively. [ABSTRACT FROM AUTHOR]

The present study aimed to evaluate the efficacy of natural deep eutectic solvents (NADESs) on the extraction of phytochemicals from eight Algerian date fruit cultivars (Phoenix dactylifera L.). In this study, lactic acid/sucrose-based NADESs were used as an alternative to conventional chemical solvents using the ultrasound-assisted extraction (UAE) method. The obtained extracts were assessed for the determination of bioactive compound contents, phenolic composition, antioxidant activity, and enzyme inhibitory potential. The results showed a considerable variation in phytochemical compositions and related activities between cultivars, where the greatest contents of total phenolics (1288.7 mg GAE/100 g), total flavonoids (53.8 mg QE/100 g), proanthocyanidins (179.5 mg CE/g), and total triterpenoids (12.88 mg OAE/100 g) were detected in the fruits of the Ourous cultivar. The same cultivar displayed the highest antioxidant capacity against DPPH• free radical (595 mg AAE/100 g), ABTS•+ cation radical (839 mg TE/100 g), and ferric reducing antioxidant potential (704 mg AAE/100 g). All extracts manifested moderate antioxidant activities tested by phosphomolybdenum, NO•, and linoleic acid lipid peroxidation assays. These extracts also exhibited interesting levels of in vitro enzyme inhibition; the Ourous cultivar gave the best inhibitory activity against α-amylase and acetylcholinesterase with 45 and 37%, respectively. HPLC-DAD-MS detected a total of five compounds, with phenolic acids and flavonoids being the main phenolics identified in the extract. The phenolic composition exhibited significant variability among cultivars. Notably, the highest amounts were revealed in the Tazizaout cultivar, with the predominance of gallic acid. The results confirmed that the combination of UAE and NADESs provides a novel and important alternative to chemical solvents for sustainable and environmentally friendly extraction and can represent a good alternative in food and pharmaceutical industry applications.

Given today’s increasingly intensive agriculture, one key problem area considers the valorization and reuse of wastes from food and agricultural production with minimal impact on the environment. Due to its physicochemical characteristics, biochar (BC) derived from grapevine pruning residue has shown considerable potential for use as an adsorbent. High-value phytochemicals found in abundance in the olive leaf (OL) can be employed in many different industrial sectors. The potential application of BC in the removal of specific polyphenolic components from OL extracts has been investigated in the present study. Water, as the most available and greenest of solvents, was investigated as to its use in the extraction of polyphenols, which was carried out by comparing maceration, ultrasound-assisted extraction, and microwave-assisted extraction, considering different temperatures and solid-to-liquid (s/l) ratios. The BC adsorption capacity of selected polyphenols was fitted with both the Langmuir and Freundlich isotherm models. The Freundlich model fitted better relative to OL polyphenols adsorption. Oleuropein was the most abundant compound identified in the extracts, obtaining the highest Kf value (20.4 (mg/g) × (L/g)n) and R2 coefficient (0.9715) in the adsorption on the biochar’s surface. The optimum conditions in the dosage experiment suggest the use of 0.5 g of BC using 3 g/L extracts, with an exception for oleuropein and hydroxytyrosol, for which the highest biochar dose (2.5 g) performed better. Considering the compounds’ concentrations and the BC dose, BC from grapevine pruning residues demonstrated a potential use in the uptake of specific polyphenols from olive leaves, making it a promising adsorbent for such applications.

The mangosteen (Garcinia mangostana L.) pericarp is known to be rich in potent bioactive phytochemical compounds such as xanthones, which possess pharmacologically important antioxidant activity and beneficial cardiometabolic properties. Mangosteen pericarp is typically classified as unavoidable food waste and discarded, despite being rich in bioactive phytochemical compounds that therefore present an exciting opportunity for valorization. Thus, this study aims to extract phytochemical compounds from mangosteen pericarp using pressurized hot water extraction (PHWE) and determine its biological effects in endothelial cells using RNA sequencing. Liquid chromatography with MS/MS (LC/MSMS) and UV detection (LC/UV) was subsequently used to identify three key phytochemical compounds extracted from the mangosteen pericarp: α-Mangostin, γ-Mangostin, and Gartanin. Within the tested range of extraction temperatures by PHWE, our results demonstrated that an extraction temperature of 120 °C yielded the highest concentrations of α-Mangostin, γ-Mangostin, and Gartanin with a concomitant improvement in antioxidant capacity compared to other extraction temperatures. Using global transcriptomic profiling and bioinformatic analysis, the treatment of endothelial cells with mangosteen pericarp extracts (120 °C PHWE) for 48 h caused 408 genes to be differentially expressed. Furthermore, our results demonstrated that key biological processes related to “steroid biosynthesis and metabolism”, likely involving the activation of the AMPK signaling pathway, were upregulated by mangosteen pericarp extract treatment. In conclusion, our study suggests a green extraction method to valorize phytochemical compounds from mangosteen pericarp as a natural product with potential beneficial effects on cardiometabolic health.

The aim of this study was to investigate the effect of the use of green solvents, natural deep eutectic solvents (NaDES), in comparison with conventional solvents on the extraction of free unbound phenolic compounds and the antioxidant activity of extracts of dried bilberry fruit, bilberry leaves and green tea leaves. After preparation of the extracts via ultrasound-assisted extraction using NaDES and conventional solvents (water and ethanol), spectrophotometric determination of total phenolic and flavonoid content, HPLC analysis of extracted polyphenols and antioxidant determination using FRAP, DPPH and ABTS assays were conducted. The results showed that NaDES have a great potential as agents for the extraction of phenolic compounds with potent antioxidant activity; the highest values of phenolic content and antioxidant activity were detected in the samples obtained by extraction using the NaDES combination betaine + urea. The bilberry leaves exhibited the highest flavonoid content among all extracts and turned out to be more active than bilberry fruits, to which they are often just a by-product during processing. The most active extract of all was the betaine-urea green tea leaves extract. Further research into the most active NaDES extracts should be performed. [ABSTRACT FROM AUTHOR]

Pomegranate (Punica granatum L.) is well known for its high content of bioactives, including polyphenols, flavonoids, and tannins, which have been shown to exhibit a wide range of biological activities, such as antioxidant, antimicrobial, and anticancer effects. It is worth noting that the majority of these molecules are found in the peels, which are usually disposed of after processing, causing a significant amount of waste, amounting to more than 3.6 million t/y. This work investigates microwave-assisted extraction (MAE) in water for the recovery of antioxidants from pomegranate peels (PP), including the optimisation of temperature and extraction times. The total phenolic, anthocyanin, flavonoid, and tannin contents of the recovered extracts were determined, as well as their antioxidant activities, which were found to be 356.35 mgGAE/gExtr, 303.97 µgCy3G/gExtr, 37.28 mgQE/gExtr, 56.48 mgGAE/gExtr, and 5.72 mmolTE/gExtr, respectively (according to the adopted reference). All results were compared with those obtained using a conventional protocol. In addition, the potential for water recycling by means of downstream nanofiltration in optimised MAE was investigated, leading to overall water reuse of approx. 75%. Power consumption (20.92 W/mgGAE) and common green metrics, Reaction Mass Efficiency (RME), E-Factor, and the Process Mass Intensiti/efficiency (PMI, PME), were considered in evaluating the proposed PP valorisation strategy. Finally, the biological activities of the main products were assessed. The antimicrobial properties of the PP extracts against three Gram-positive and three Gram-negative bacteria and their antiproliferative activity towards human cancer cells were tested. S. aureus bacteria was the most susceptible to the PP extracts. All tested products displayed antiproliferative activity against HeLa cells when higher concentrations were tested, with D-PP/NF (obtained from dried PP and sequential nanofiltration) being the most effective. This result was also confirmed via clonogenic analysis, which generally indicated the possible anti-cancer activity of pomegranate peel extracts obtained using this green approach.

Hydrodynamic cavitation (HC), as an effective, efficient, and scalable extraction technique for natural products, could enable the affordable production of valuable antioxidant extracts from plant resources. For the first time, whole pomegranate (Punica granatum L.) fruits, rich in bioactive phytochemicals endowed with anti-cancer properties, were extracted in water using HC. Aqueous fractions sequentially collected during the process (M1–M5) were lyophilized (L), filtered (A), or used as such, i.e., crude (C), and analyzed for their biochemical profile and in vitro antioxidant power. The fractions M3 and M4 from the L and C series showed the highest antiradical activity and phytochemical content. While the lyophilized form is preferable for application purposes, sample L-M3, which was produced faster and with lower energy consumption than M4, was used to assess the potential antiproliferative effect on human breast cancer line (AU565-PAR) and peripheral blood mononuclear (PBMC) cells from healthy donors. In a pilot study, cell growth, death, and redox state were assessed, showing that L-M3 significantly reduced tumor cell proliferation and intracellular oxygen reactive species. No effect on PBMCs was detected. Thus, the antioxidant phytocomplex extracted from pomegranate quickly (15 min), at room temperature (30 °C), and efficiently showed potential anticancer activity without harming healthy cells.

Antioxidant compounds with health benefits can be found in food processing residues, such as grape pomace. In this study, antioxidants were identified and quantified in an extract obtained from Graciano red grape pomace via a green process. The antioxidant activity of the extract was assessed by the DPPH and FRAP tests, and the phenolic content by the Folin–Ciocalteu test. Furthermore, nanotechnologies were employed to produce a safe and effective formulation that would exploit the antioxidant potential of the extract for skin applications. Anthocyanins, flavan-3-ols and flavanols were the main constituents of the grape pomace extract. Phospholipid vesicles, namely liposomes, were prepared and characterized. Cryo-TEM images showed that the extract-loaded liposomes were predominantly spherical/elongated, small, unilamellar vesicles. Light scattering results revealed that the liposomes were small (~100 nm), homogeneously dispersed, and stable during storage. The non-toxicity of the liposomal formulation was demonstrated in vitro in skin cells, suggesting its possible safe use. These findings indicate that an extract with antioxidant properties can be obtained from food processing residues, and a liposomal formulation can be developed to exploit its bioactive value, resulting in a promising healthy product. [ABSTRACT FROM AUTHOR]

Agri-food industries generate a large amount of waste that offers great revalorization opportunities within the circular economy framework. In recent years, new methodologies for the extraction of compounds with more eco-friendly solvents have been developed, such as the case of natural deep eutectic solvents (NADES). In this study, a methodology for extracting phenolic compounds from olive tree leaves using NADES has been optimized. The conditions established as the optimal rely on a solvent composed of choline chloride and glycerol at a molar ratio of 1:5 with 30% water. The extraction was carried out at 80 °C for 2 h with constant agitation. The extracts obtained have been analyzed by high-performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) in MRM mode. The comparison with conventional ethanol/water extraction has shown that NADES, a more environmentally friendly alternative, has improved extraction efficiency. The main polyphenols identified in the NADES extract were Luteolin-7-O-glucoside, Oleuropein, 3-Hydroxytyrosol, Rutin, and Luteolin at the concentrations of 262, 173, 129, 34, and 29 mg kg−1 fresh weight, respectively.

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. [ABSTRACT FROM AUTHOR]

The aim of this study was to investigate the effect of the use of green solvents, natural deep eutectic solvents (NaDES), in comparison with conventional solvents on the extraction of free unbound phenolic compounds and the antioxidant activity of extracts of dried bilberry fruit, bilberry leaves and green tea leaves. After preparation of the extracts via ultrasound-assisted extraction using NaDES and conventional solvents (water and ethanol), spectrophotometric determination of total phenolic and flavonoid content, HPLC analysis of extracted polyphenols and antioxidant determination using FRAP, DPPH and ABTS assays were conducted. The results showed that NaDES have a great potential as agents for the extraction of phenolic compounds with potent antioxidant activity; the highest values of phenolic content and antioxidant activity were detected in the samples obtained by extraction using the NaDES combination betaine + urea. The bilberry leaves exhibited the highest flavonoid content among all extracts and turned out to be more active than bilberry fruits, to which they are often just a by-product during processing. The most active extract of all was the betaine-urea green tea leaves extract. Further research into the most active NaDES extracts should be performed.

Antioxidant compounds with health benefits can be found in food processing residues, such as grape pomace. In this study, antioxidants were identified and quantified in an extract obtained from Graciano red grape pomace via a green process. The antioxidant activity of the extract was assessed by the DPPH and FRAP tests, and the phenolic content by the Folin–Ciocalteu test. Furthermore, nanotechnologies were employed to produce a safe and effective formulation that would exploit the antioxidant potential of the extract for skin applications. Anthocyanins, flavan-3-ols and flavanols were the main constituents of the grape pomace extract. Phospholipid vesicles, namely liposomes, were prepared and characterized. Cryo-TEM images showed that the extract-loaded liposomes were predominantly spherical/elongated, small, unilamellar vesicles. Light scattering results revealed that the liposomes were small (~100 nm), homogeneously dispersed, and stable during storage. The non-toxicity of the liposomal formulation was demonstrated in vitro in skin cells, suggesting its possible safe use. These findings indicate that an extract with antioxidant properties can be obtained from food processing residues, and a liposomal formulation can be developed to exploit its bioactive value, resulting in a promising healthy product.

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.

The increasing production of tropical fruits followed by their processing results in tons of waste, such as skins or seeds. However, these by-products have been reported to be rich in bioactive compounds (BACs) with excellent properties of interest in the cosmeceutical industry: antioxidant, anti-aging, anti-inflammatory, antimicrobial and photoprotective properties. This review summarizes the tropical fruits most produced worldwide, their bioactive composition and the most important and studied therapeutic properties that their by-products can contribute to skin health, as well as the different approaches for obtaining these compounds using techniques by conventional (Soxhlet, liquid-liquid extraction or maceration) and non-conventional extractions (supercritical fluid extraction (SFE), ultrasound-assisted extraction (UAE), microwave-assisted extraction (MAE), pressurized liquid extraction (PLE) and two-phase aqueous system), followed by their identification by HPLC-MS or GC-MS analysis. Moreover, this work encompasses several studies that may prove the effects of seeds and skins from tropical fruits against oxidative stress, hyperpigmentation, acne, aging or UV radiation. Therefore, the investigation of functional components present in tropical fruit by-products under a circular bioeconomy model could be of great interest for the cosmeceutical industry and a very promising option for obtaining new cosmeceutical formulations.

Olive-derived biomasses contain bioactive compounds with health promoting effects as well as antioxidant and sweet-tasting properties. However, their sequential extraction has not been attained. In the present study, firstly antioxidants and mannitol were extracted from exhausted olive pomace (EOP) by an eco-friendly method, ultrasound-assisted water extraction (UAWE). The amplitude (20–80%), extraction time (2–18 min) and solid loading (2–15%, w/v) were evaluated according to a Box–Behnken experimental design. Using the response surface methodology, the optimal conditions for extraction were obtained: 80% amplitude, 11.5% solid loading and 16 min. It enabled the multi-response optimization of the total phenolic content (TPC) (40.04 mg/g EOP), hydroxytyrosol content (6.42 mg/g EOP), mannitol content (50.92 mg/g EOP) and antioxidant activity (ferric reducing power or FRAP, 50.95 mg/g EOP; ABTS, 100.64 mg/g EOP). Moreover, the phenolic profile of the extracts was determined by liquid chromatography-UV and mass spectrometry, identifying hydroxytyrosol as the main phenolic compound and other minor derivatives could be characterized. Scanning electron microscopy was used to analyze the morphological changes produced in the cellular structure of EOP after UAWE. In addition, the chemical composition of the extracted EOP solid was characterized for further valorization. Then, a second extraction step was performed in order to extract bioactive triterpenes from the latter solid. The triterpenes content in the extract was determined and the effect of the previous UAWE step on the triterpenes extraction was evaluated. In this case, the use of ultrasound enhanced the extraction of maslinic acid and oleanolic acid from pelletized EOP with no milling requirement. Overall, UAWE can be applied to obtain antioxidant compounds and mannitol as first extraction step from pelletized EOP while supporting the subsequent recovery of triterpenic acids.

Cold plasma is a new technology of promising potential to use as a part of technological extraction lines constructed to implement green chemistry solutions or simply to reduce resources in solvent-based extraction lines. The present study was undertaken to verify the effect of nitrogen cold plasma pre-treatment conducted for 8 min (20 kHz) on the content of antioxidants, antioxidant activity, the profile of volatile compounds, microbial count, pH and color measured in herb extracts (12 herbs: Echinacea purpurea; Salvia officinalis; Urtica dioica; Polygonum aviculare; Vaccinium myrtillus; Taraxacum officinale; Hypericum perforatum; Achillea millefolium; Sanguisorba officinalis; Leonurus cardiaca; Ballota nigra; Andrographis paniculata) obtained with its usage. The surface morphology of extracted herbs was examined as well. Herbs used for extraction were ground and suspended in water before cold plasma treatment, which is a novel approach not studied before. Most plasma-treated extracts were characterized by a higher content of polyphenols (11 out of 12). Content of flavonoids and anthocyanins increased in four extracts and in the case of anthocyanins was significantly higher in comparison to control (up to 77%). The antioxidant activity measured at least by one method (ABTS, DPPH, FRAP) was also higher in nine plasma-treated solutions. Moreover, plasma decreased total aerobic bacteria, affected the color and increased pH of the extracts. The surface structure of the plant material after the extraction process was significantly damaged, which probably led to a higher extraction yield of bioactive compounds and in consequence to the higher antioxidant activity of extracts obtained with the cold plasma treatment.

Nowadays, the food industry is heavily involved in searching for green sources of valuable compounds, to be employed as potential food ingredients, to cater to the evolving consumers’ requirements for health-beneficial food ingredients. In this frame, agri-food by-products represent a low-cost source of natural bioactive compounds, including antioxidants. However, to effectively recover these intracellular compounds, it is necessary to reduce the mass transfer resistances represented by the cellular envelope, within which they are localized, to enhance their extractability. To this purpose, emerging extraction technologies, have been proposed, including Supercritical Fluid Extraction, Microwave-Assisted Extraction, Ultrasound-Assisted Extraction, High-Pressure Homogenization, Pulsed Electric Fields, High Voltage Electrical Discharges. These technologies demonstrated to be a sustainable alternative to conventional extraction, showing the potential to increase the extraction yield, decrease the extraction time and solvent consumption. Additionally, in green extraction processes, also the contribution of solvent selection, as well as environmental and economic aspects, represent a key factor. Therefore, this review focused on critically analyzing the main findings on the synergistic effect of low environmental impact technologies and green solvents towards the green extraction of antioxidants from food by-products, by discussing the main associated advantages and drawbacks, and the criteria of selection for process sustainability.

Currently, there is increased interest in finding appropriate food-grade green extraction systems capable of extracting these bioactive compounds from dietary mushrooms for applications in various food, pharmacological, or nutraceutical formulations. Herein, we evaluated a modified Swiss water process (SWP) method using alkaline and acidic pH at low and high temperature under pressurized conditions as a suitable green food grade solvent to obtained extracts enriched with myco-nutrients (dietary phenolics, total antioxidants (TAA), vitamins, and minerals) from Chaga. Ultra-high performance liquid chromatography coupled to high resolution accurate mass tandem mass spectrometry (UHPLC-HRAMS-MS/MS) was used to assess the phenolic compounds and vitamin levels in the extracts, while inductively coupled plasma mass spectrometry (ICP-MS) was used to determine the mineral contents. Over 20 phenolic compounds were quantitatively evaluated in the extracts and the highest total phenolic content (TPC) and total antioxidant activity (TAA) was observed at pH 11.5 at 100 °C. The most abundant phenolic compounds present in Chaga extracts included phenolic acids such as protocatechuic acid 4-glucoside (0.7–1.08 µg/mL), syringic acid (0.62–1.18 µg/mL), and myricetin (0.68–1.3 µg/mL). Vitamins are being reported for the first time in Chaga. Not only, a strong correlation was found for TPC with TAA (r-0.8,

A green ultrasound-assisted extraction (UAE) method using glycerol/water mixtures for extraction of licorice (Glycyrrhiza glabra) bioactive constituents was developed in this study. The response surface method, according to the Box-Behnken design, was employed to optimize the extraction parameters: glycerol concentration (X1), temperature (X2), and the amount of herbal drug used in the production (X3). The responses were content of total phenols (TP), TP extraction efficiency (TPy) and the content of licorice characteristic constituents, glabridin (Gla) and isoliquiritigenin (Iso). Response surface analysis predicted the optimal extraction conditions for maximized amounts of TP, Tpy, Gla, and Iso. The extracts were prepared using the calculated conditions. The analysis of the selected constituents confirmed the validity of the model. Furthermore, biological activity of the extracts was tested. The results demonstrate that UAE using glycerol is a fast and efficient method for preparation of extracts with excellent radical scavenging, Fe2+ chelating and antioxidant activity. Furthermore, the observed notable tyrosinase and elastase inhibitory activity of the extracts, as well as their anti-inflammatory activity, indicate the anti-aging properties of the investigated extracts. The fact that the extracts were prepared using the safe, cosmetically active solvent, glycerol, makes them suitable for direct use in specialized cosmeceutical formulations.

The increasing production of tropical fruits followed by their processing results in tons of waste, such as skins or seeds. However, these by-products have been reported to be rich in bioactive compounds (BACs) with excellent properties of interest in the cosmeceutical industry: antioxidant, anti-aging, anti-inflammatory, antimicrobial and photoprotective properties. This review summarizes the tropical fruits most produced worldwide, their bioactive composition and the most important and studied therapeutic properties that their by-products can contribute to skin health, as well as the different approaches for obtaining these compounds using techniques by conventional (Soxhlet, liquid-liquid extraction or maceration) and non-conventional extractions (supercritical fluid extraction (SFE), ultrasound-assisted extraction (UAE), microwave-assisted extraction (MAE), pressurized liquid extraction (PLE) and two-phase aqueous system), followed by their identification by HPLC-MS or GC-MS analysis. Moreover, this work encompasses several studies that may prove the effects of seeds and skins from tropical fruits against oxidative stress, hyperpigmentation, acne, aging or UV radiation. Therefore, the investigation of functional components present in tropical fruit by-products under a circular bioeconomy model could be of great interest for the cosmeceutical industry and a very promising option for obtaining new cosmeceutical formulations. [ABSTRACT FROM AUTHOR]

Olive-derived biomasses contain bioactive compounds with health promoting effects as well as antioxidant and sweet-tasting properties. However, their sequential extraction has not been attained. In the present study, firstly antioxidants and mannitol were extracted from exhausted olive pomace (EOP) by an eco-friendly method, ultrasound-assisted water extraction (UAWE). The amplitude (20–80%), extraction time (2–18 min) and solid loading (2–15%, w/v) were evaluated according to a Box–Behnken experimental design. Using the response surface methodology, the optimal conditions for extraction were obtained: 80% amplitude, 11.5% solid loading and 16 min. It enabled the multi-response optimization of the total phenolic content (TPC) (40.04 mg/g EOP), hydroxytyrosol content (6.42 mg/g EOP), mannitol content (50.92 mg/g EOP) and antioxidant activity (ferric reducing power or FRAP, 50.95 mg/g EOP; ABTS, 100.64 mg/g EOP). Moreover, the phenolic profile of the extracts was determined by liquid chromatography-UV and mass spectrometry, identifying hydroxytyrosol as the main phenolic compound and other minor derivatives could be characterized. Scanning electron microscopy was used to analyze the morphological changes produced in the cellular structure of EOP after UAWE. In addition, the chemical composition of the extracted EOP solid was characterized for further valorization. Then, a second extraction step was performed in order to extract bioactive triterpenes from the latter solid. The triterpenes content in the extract was determined and the effect of the previous UAWE step on the triterpenes extraction was evaluated. In this case, the use of ultrasound enhanced the extraction of maslinic acid and oleanolic acid from pelletized EOP with no milling requirement. Overall, UAWE can be applied to obtain antioxidant compounds and mannitol as first extraction step from pelletized EOP while supporting the subsequent recovery of triterpenic acids. [ABSTRACT FROM AUTHOR]

Cold plasma is a new technology of promising potential to use as a part of technological extraction lines constructed to implement green chemistry solutions or simply to reduce resources in solvent-based extraction lines. The present study was undertaken to verify the effect of nitrogen cold plasma pre-treatment conducted for 8 min (20 kHz) on the content of antioxidants, antioxidant activity, the profile of volatile compounds, microbial count, pH and color measured in herb extracts (12 herbs: Echinacea purpurea; Salvia officinalis; Urtica dioica; Polygonum aviculare; Vaccinium myrtillus; Taraxacum officinale; Hypericum perforatum; Achillea millefolium; Sanguisorba officinalis; Leonurus cardiaca; Ballota nigra; Andrographis paniculata) obtained with its usage. The surface morphology of extracted herbs was examined as well. Herbs used for extraction were ground and suspended in water before cold plasma treatment, which is a novel approach not studied before. Most plasma-treated extracts were characterized by a higher content of polyphenols (11 out of 12). Content of flavonoids and anthocyanins increased in four extracts and in the case of anthocyanins was significantly higher in comparison to control (up to 77%). The antioxidant activity measured at least by one method (ABTS, DPPH, FRAP) was also higher in nine plasma-treated solutions. Moreover, plasma decreased total aerobic bacteria, affected the color and increased pH of the extracts. The surface structure of the plant material after the extraction process was significantly damaged, which probably led to a higher extraction yield of bioactive compounds and in consequence to the higher antioxidant activity of extracts obtained with the cold plasma treatment. [ABSTRACT FROM AUTHOR]

Nowadays, the food industry is heavily involved in searching for green sources of valuable compounds, to be employed as potential food ingredients, to cater to the evolving consumers' requirements for health-beneficial food ingredients. In this frame, agri-food by-products represent a low-cost source of natural bioactive compounds, including antioxidants. However, to effectively recover these intracellular compounds, it is necessary to reduce the mass transfer resistances represented by the cellular envelope, within which they are localized, to enhance their extractability. To this purpose, emerging extraction technologies, have been proposed, including Supercritical Fluid Extraction, Microwave-Assisted Extraction, Ultrasound-Assisted Extraction, High-Pressure Homogenization, Pulsed Electric Fields, High Voltage Electrical Discharges. These technologies demonstrated to be a sustainable alternative to conventional extraction, showing the potential to increase the extraction yield, decrease the extraction time and solvent consumption. Additionally, in green extraction processes, also the contribution of solvent selection, as well as environmental and economic aspects, represent a key factor. Therefore, this review focused on critically analyzing the main findings on the synergistic effect of low environmental impact technologies and green solvents towards the green extraction of antioxidants from food by-products, by discussing the main associated advantages and drawbacks, and the criteria of selection for process sustainability. [ABSTRACT FROM AUTHOR]

Currently, there is increased interest in finding appropriate food-grade green extraction systems capable of extracting these bioactive compounds from dietary mushrooms for applications in various food, pharmacological, or nutraceutical formulations. Herein, we evaluated a modified Swiss water process (SWP) method using alkaline and acidic pH at low and high temperature under pressurized conditions as a suitable green food grade solvent to obtained extracts enriched with myco-nutrients (dietary phenolics, total antioxidants (TAA), vitamins, and minerals) from Chaga. Ultra-high performance liquid chromatography coupled to high resolution accurate mass tandem mass spectrometry (UHPLC-HRAMS-MS/MS) was used to assess the phenolic compounds and vitamin levels in the extracts, while inductively coupled plasma mass spectrometry (ICP-MS) was used to determine the mineral contents. Over 20 phenolic compounds were quantitatively evaluated in the extracts and the highest total phenolic content (TPC) and total antioxidant activity (TAA) was observed at pH 11.5 at 100 °C. The most abundant phenolic compounds present in Chaga extracts included phenolic acids such as protocatechuic acid 4-glucoside (0.7–1.08 µg/mL), syringic acid (0.62–1.18 µg/mL), and myricetin (0.68–1.3 µg/mL). Vitamins are being reported for the first time in Chaga. Not only, a strong correlation was found for TPC with TAA (r-0.8, <0.0001), but also, with individual phenolics (i.e., Salicylic acid), lipophilic antioxidant activity (LAA), and total antioxidant minerals (TAM). pH 2.5 at 100 °C treatment shows superior effects in extracting the B vitamins whereas pH 2.5 at 60 and 100 °C treatments were outstanding for extraction of total fat-soluble vitamins. Vitamin E content was the highest for the fat-soluble vitamins in the Chaga extract under acidic pH (2.5) and high temp. (100 °C) and ranges between 50 to 175 µg/100 g Chaga. Antioxidant minerals ranged from 85.94 µg/g (pH7 at 100 °C) to 113.86 µg/g DW (pH2.5 at 100 °C). High temperature 100 °C and a pH of 2.5 or 9.5. The treatment of pH 11.5 at 100 °C was the most useful for recovering phenolics and antioxidants from Chaga including several phenolic compounds reported for the first time in Chaga. SWP is being proposed herein for the first time as a novel, green food-grade solvent system for the extraction of myco-nutrients from Chaga and have potential applications as a suitable approach to extract nutrients from other matrices. Chaga extracts enriched with bioactive myconutrients and antioxidants may be suitable for further use or applications in the food and nutraceutical industries. [ABSTRACT FROM AUTHOR]

The use of grape stems for the extraction of bioactive compounds to be used in the pharmaceutical, food, and cosmetic industries is a promising objective. The aim of this work is to determine the influence of the different extraction conditions (temperature, ethanol concentration, and ratio of sample/solvent) on phenolic composition and antioxidant capacity of Mazuelo stem extracts. In general, the ethanol concentration of the extraction solvent was the factor that had the greatest influence on the extraction of different bioactive compounds. The greatest content of total phenolic compounds and the highest antioxidant activity of the extracts were obtained with 50% ethanol and at 40 °C. The most abundant compound found in the different extracts obtained from Mazuelo grape stem was (+)-catechin, but appreciable concentrations of gallic acid, a quercetin derivative, and stilbenes (trans-resveratrol and trans-ε-viniferin) were also extracted. Quercetin and malvidin-3-glucoside showed the highest correlation with the antioxidant capacity of the extracts, while stilbenes did not present such relation. The maximum concentration of gallic acid was extracted with water but the extraction of most of the compounds was maximum on using 50% ethanol. Consequently, the selection of the extraction method to be used will depend on the particular compound to be extracted in greatest quantity. [ABSTRACT FROM AUTHOR]

A green ultrasound-assisted extraction (UAE) method using glycerol/water mixtures for extraction of licorice (Glycyrrhiza glabra) bioactive constituents was developed in this study. The response surface method, according to the Box-Behnken design, was employed to optimize the extraction parameters: glycerol concentration (X1), temperature (X2), and the amount of herbal drug used in the production (X3). The responses were content of total phenols (TP), TP extraction efficiency (TPy) and the content of licorice characteristic constituents, glabridin (Gla) and isoliquiritigenin (Iso). Response surface analysis predicted the optimal extraction conditions for maximized amounts of TP, Tpy, Gla, and Iso. The extracts were prepared using the calculated conditions. The analysis of the selected constituents confirmed the validity of the model. Furthermore, biological activity of the extracts was tested. The results demonstrate that UAE using glycerol is a fast and efficient method for preparation of extracts with excellent radical scavenging, Fe2+ chelating and antioxidant activity. Furthermore, the observed notable tyrosinase and elastase inhibitory activity of the extracts, as well as their anti-inflammatory activity, indicate the anti-aging properties of the investigated extracts. The fact that the extracts were prepared using the safe, cosmetically active solvent, glycerol, makes them suitable for direct use in specialized cosmeceutical formulations. [ABSTRACT FROM AUTHOR]