Search Results (27)

The olive oil industry generates by-products like olive leaves and pomace, which are rich in bioactive compounds, especially polyphenols. This study applied a circular economy approach to valorize these residues using green ultrasound-assisted extraction (UAE) with GRAS solvents. Key parameters (solvent composition, ultrasound amplitude, and specific energy) were optimized via Response Surface Methodology (RSM) to enhance polyphenol recovery and yield. Ethanol concentration proved to be the most influential factor. Optimal conditions for olive pomace were 100% ethanol, 46 μm amplitude, and 25 J∙mL⁻¹ specific energy, while olive leaves required 72% ethanol with similar ultrasound settings. Under these conditions, extracts were prepared and analyzed using HPLC-ESI-QTOF-MS and DPPH assays. The optimized UAE process achieved yields of 15–20% in less than 5 min and under mild conditions. Optimal extracts showed high oleuropein content (6 mg/g in leaves, 5 mg/g in pomace), lower hydroxytyrosol levels, and minimal oxidized derivatives, suggesting reduced degradation compared to conventional methods. These findings demonstrate UAE’s effectiveness in recovering valuable phenolics from olive by-products, supporting sustainable and efficient resource use. Full article

Citrus peel, a significant by-product of fruit processing, represents a rich source of carotenoids with strong antioxidant and health-promoting properties. The present study evaluated two green extraction techniques, cloud point extraction (CPE) and supramolecular solvent (SUPRAS)-based extraction, for carotenoids recovered from citron, orange, and tangerine peels. Whereas SUPRAS methods rely on a supramolecular solvent made of water, ethanol, and octanoic acid, CPE methods use surfactants and water, and both show a high potential to extract lipophilic components. CPE demonstrated superior efficiency in extracting total carotenoids and enhancing antioxidant activity, with orange peel extracts showing the highest concentrations. CPE and SUPRAS extracts were subsequently encapsulated using freeze-drying with chickpea protein isolate, achieving high encapsulation efficiencies (82.40–88.97%). The use of encapsulation technology is an effective strategy to protect carotenoids from environmental stressors. Color, morphological, and FTIR analyses confirmed the successful encapsulation and retention of carotenoids. Environmental impact was assessed using the EcoScale tool, revealing excellent sustainability for CPE (92 points) and satisfactory performance for SUPRAS-based extraction (70 points). The use of Generally Recognized As Safe (GRAS) solvents and plant-derived encapsulation materials makes this method highly suitable for clean-label product development across the food, cosmetic, and nutraceutical industries. In summary, the results point to a practical and sustainable approach to citrus waste valorization into valuable, health-promoting ingredients—supporting both circular economy goals and eco-friendly innovation. Full article

Hawm Gra Dang Ngah rice (HDNR) is a red rice variety cultivated in Thailand’s southern border region, yet its biological properties have not been extensively studied. This study investigates the effects of HDNR extracts on bioactive constituents, spectral fingerprints, and antioxidant capacities. We evaluated the inhibitory effects of aqueous (HDNR-W) and ethanolic (HDNR-E) extracts on monoamine oxidase (MAO), α-glucosidase, and HMG-CoA reductase activities, as well as their cytotoxicity in normal and cancer cells. The results demonstrated that HDNR-E contained significantly higher concentrations of phenolic compounds, flavonoids, and anthocyanins compared to HDNR-W. In contrast, HDNR-W exhibited greater amino acid content than HDNR-E. FT-IR analysis revealed solvent-specific interactions that influenced compound solubility, highlighting distinct extraction efficiencies. Antioxidant assays showed HDNR-E to be markedly more potent, with superior performance in DPPH, ABTS, metal chelation, and FRAP assays, as evidenced by its lower IC₅₀ values relative to HDNR-W. Furthermore, HDNR-E displayed significantly stronger inhibitory activity against both MAO and α-glucosidase compared to HDNR-W. Conversely, HDNR-W demonstrated greater inhibitory efficacy toward HMG-CoA reductase than HDNR-E. Furthermore, HDNR-E exhibited significant antiproliferative effects against A549 lung cancer and MCF-7 breast cancer cells without affecting normal cells. These results highlight the potential of HDNR-E as a valuable source of bioactive compounds and underscore the importance of solvent selection in enhancing the health benefits of rice extracts. Full article

The brown seaweed Saccharina latissima is an abundant, although yet underutilized, source of natural bioactive compounds commonly found in western regions. In recent years, brown algae have garnered attention as promising sources of polyphenols, particularly phlorotannins. The recovery of these relevant components by eco-friendly and energy-efficient methods with solvents GRAS (Generally recognized as safe) contributes to minimizing environmental impact, and promotes sustainability. Pressurized liquid extraction (PLE) and microwave-assisted extraction (MAE) optimized by Box–Behnken design (BBD) were explored for this purpose. The methods were evaluated considering the process yield and the quality of the recovered extracts by phenolic and phlorotannin levels, and their antioxidant capacity was assessed by DPPH and ABTS assays. The optimized MAE techniques (80 °C, 2% EtOH/Water at 40 mL g⁻¹) and PLE2 (80 °C with water) showed the highest extract yields, with increases of 65.76% and 37.36%, respectively, compared to CRE. PLE2 also achieved higher TPC and antioxidant capacity (ABTS) values by 61.88% and 80.39%, respectively. MAE (optimized) increased TPC and ABTS by 53.90% and 36.42%, respectively. Regression analysis of MAE confirmed the accuracy of the models in assessing interaction parameters (adjustment p < 0.05 and adequacy R² > 0.86). Therefore, the study presents eco-efficient approaches for recovering phenolic compounds and antioxidants from brown algae, contributing to the valorization of these resources in the industry and enhancing their application. Full article

Food waste has a significant social impact but can be revalued as a source of bioactive compounds, such as condensed tannins. This abundant biomass, corresponding to a polymeric antioxidant, must be depolymerized to become bioavailable. Previous studies have investigated polymer degradation into oligomers using high temperatures and expensive nucleophiles, often under conditions unsuitable for food applications. In the present investigation, it is proposed that the depolymerization of condensed tannins can occur under food-grade conditions using a Generally Recognized as Safe (GRAS) solvent by optimizing the reaction’s heating method with microwave assistance and using gallic acid as a nucleophile. Thermal studies indicate that the degradation of total polyphenols content follows first-order kinetics and occurs above 80 °C in microwave. Depolymerization follows second-order kinetics, yielding epicatechin as the primary product with zero-order formation kinetics. The optimized factors were 80% v/v ethanol, 10 mg/mL polymeric tannins, and 5.88 mg/mL gallic acid. Under these conditions, the reaction efficiency was 99.9%, the mean particle diameter was 5.7 nm, the total polyphenols content was 297.3 ± 15.9 EAG mg/g, and the inhibition of ABTS●+ and DPPH● radicals was 93.5 ± 0.9% and 88.2 ± 1.5%, respectively. These results are promising for future scaling processes. Full article

Cocoa and coffee are two of the world’s most important crops. Therefore, their by-products are generated in large quantities. This work proposes a simple method for the valorization of these residues by obtaining phenolic compounds and melanoidins by solid–liquid extraction using different hydroalcoholic solutions as extracting solvents (0, 25, 50, 75, 100% ethanol). Extracts of both by-products presented the highest antioxidant capacity and total phenolic and melanoidin content when using 50–75% ethanol in the solvent. Among all the extracts, those obtained from spent coffee grounds at 75% ethanol showed the highest concentrations of total phenolic compounds (13.5 ± 1.3 mmol gallic acid equivalents/g dry matter) and melanoidins (244.4 ± 20.1 mg/g dry matter). Moreover, the sun protection factor values of the coffee extracts obtained with 50 and 75% of ethanol as extraction solvent (7.8 ± 0.9 and 8.5 ± 0.7, respectively) showed their potential for use in the cosmetic sector. The most important phenolic compounds identified in the coffee by-products extracts were phenolic acids, and most of them were found in higher concentration in extracts obtained with lower percentages of ethanol (0–25%). Protocatechuic acid was the most abundant phenolic in cocoa extracts, with concentrations ranging from 18.49 ± 2.29 to 235.35 ± 5.55 µg/g dry matter, followed by 4-hydroxybenzoic acid, (-)-epicatechin and (+)-catechin. Esculetin was found in both coffee and cocoa extracts, which had not been reported to date in these residues. In summary, the use of 75% ethanol as an extraction solvent seems a good strategy to obtain extracts rich in phenolic compounds from food by-products rich in melanoidins, such as coffee and cocoa by-products. The high antioxidant potential of these extracts makes them of great interest for the cosmetic and nutraceutical industries. Full article

New environmentally friendly methods for extracting vegetable oils are in development, with a focus on pressurized liquid extraction (PLE) in an intermittent process. Ethanol, a renewable and generally recognized as safe (GRAS) solvent, is gaining prominence in this process. It is crucial for these methods to maintain the physicochemical characteristics of the extracted oils and be economically viable on a large scale. Using SuperPro Design software v 8.5, a simulation of PLE scaled up to industrial levels was conducted. Measurements of oils extracted with pressurized hexane and ethanol showed minimal density variations, with slightly higher viscosity for ethanol-extracted oil. Accelerated oxidative degradation revealed a longer induction period for hexane-extracted oil, indicating that ethanol-extracted oil degrades more easily. The antioxidant activity of the oil extracted with hexane was lower than that with ethanol. In the differential scanning calorimetry analysis, the oils extracted with hexane and ethanol presented onset melting point temperatures of −43.2 and −36.1 °C, respectively. The economic assessment considered 16 scenarios, showing a return on investment ranging from 9.0 to 133.5% in the first year and payback times from 0.7 to 11.1 years. Scenario 8, involving two 5000 L extractors, ethanol recycling, and an annual production of 3,325,300 L of soybean oil at USD 1.25/L, demonstrated the best return on investment (133.5%) in less than one year. Overall, this study suggests that industrial-scale soybean oil extraction via PLE in an intermittent process can be more cost-effective than conventional methods, making implementation feasible. Full article

Orange and coffee grounds by-products, rich in phenolic bioactive compounds, can be used in the food industry as antioxidants, colorants, flavorings and additives, mainly because they are solvents that are easy to prepare, have a lower cost, are thermally stable, biodegradable, renewable, and are considered GRAS (Generally Recognized as Safe). Deep eutectic solvents, which are sustainable and have lower melting points, are effective for extracting these compounds. This study aimed to evaluate the use of deep eutectic solvents (DES) in extracting Total Phenolic Compounds (TPC), from orange by-products and spent coffee grounds. DES formed by citric acid: mannitol (CM-DES), and lactic acid: glucose (LG-DES), were evaluated by varying the following parameters: water content (10–50%), solid–liquid ratio (1:5–1:50 w/w) and temperature (40–50 °C). DES citric acid: mannitol presented the best efficiency in the extraction of TPC under the conditions of 10% water, 80 °C, and solid–liquid ratio 1:10 (w/w) for the orange by-products (1782.92 ± 4.50 mg GAE/L) and 1:15 (w/w) for spent coffee grounds (1620.71 ± 3.72 mg GAE/L). The highest antioxidant activity was observed in the extraction with CM-DES for both by-products in the three methods evaluated: Ferric Reducing Antioxidant Power (FRAP) (1.087 ± 0.004 and 1.071 ± 0.006 mol ascorbic acid/L), DPPH radical scavenging activity (2,2-difenil-1-picrilhidrazil—DPPH) (0.233 ± 0.003 and 0.234 ± 0.001 mol Trolox equivalent/L), and radical cation scavenging activity ABTS (2,2-azino-bis (3-ethyl-benzothiazoline-6-sulfonic acid—ABTS) (0.284 ± 7.16 and 0.319 ± 0.002 mol Trolox equivalent/L). Therefore, DES with citric acid: mannitol is a promising alternative to conventional solvents to recover phenolic compounds in agro-industrial by-products, such as orange by-products and SCG. Full article

In wheat and barley, Fusarium head blight is mainly caused by Fusarium graminearum, and its control is based on the agricultural practices of not leaving crop residues in the field, growing phytopathogenic fungi-resistant varieties, biological control, and chemical treatment, including using fungicides. Here, we investigated the antifungal and antimycotoxigenic activities of Massoia essential oil (MEO) and C10 Massoia lactone (C10) on Fusarium graminearum KACC 41047. Because DMSO, which was used as a solvent in this study, exhibited antifungal activity at 5% in a fungal growth medium, it was used in the antifungal and antimycotoxigenic experiments at 0.05%. Three assays were used to investigate the antifungal activities of MEO and C10, which exhibited potent antifungal activity in the agar dilution assay, with complete fungal growth inhibition at 100 mg/L. At 5–50 mg/L, MEO and C10 suppressed deoxynivalenol and 15-acetyl-deoxynivalenol production by >50% by downregulating the Tri10 gene, which expresses trichodiene synthase. MEO and C10 might be potent antifungal agents for F. graminearum control with less toxicological concerns because they are GRAS chemicals. Full article

Electrospun/sprayed fiber films and nanoparticles were broadly studied as encapsulation techniques for bioactive compounds. Nevertheless, many of them involved using non-volatile toxic solvents or non-biodegradable polymers that were not suitable for oral consumption, thus rather limiting their application. In this research, a novel electrospun lipid–polymer composite (ELPC) was fabricated with whole generally recognized as safe (GRAS) materials including gelatin, medium chain triglyceride (MCT) and lecithin. A water-insoluble bioactive compound, tetrahydrocurcumin (TC), was encapsulated in the ELPC to enhance its delivery. Confocal laser scanning microscopy (CLSM) was utilized to examine the morphology of this ELPC and found that it was in a status between electrospun fibers and electrosprayed particles. It was able to form self-assembled emulsions (droplets visualized by CLSM) to deliver active compounds. In addition, this gelatin-based ELPC self-assembled emulsion was able to form a special emulsion gel. CLSM observation of this gel displayed that the lipophilic contents of the ELPC were encapsulated within the cluster of the hydrophilic gelatin gel network. The FTIR spectrum of the TC-loaded ELPC did not show the fingerprint pattern of crystalline TC, while it displayed the aliphatic hydrocarbon stretches from MCT and lecithin. The dissolution experiment demonstrated a relatively linear release profile of TC from the ELPC. The lipid digestion assay displayed a rapid digestion of triglycerides in the first 3–6 min, with a high extent of lipolysis. A Caco-2 intestinal monolayer transport study was performed. The ELPC delivered more TC in the upward direction than downwards. MTT study results did not report cytotoxicity for both pure TC and the ELPC-encapsulated TC under 15 μg/mL. Caco-2 cellular uptake was visualized by CLSM and semi-quantified to estimate the accumulation rate of TC in the cells over time. Full article

Beans are an essential source of nutritional components such as plant proteins, minerals and dietary fiber, as well as of antioxidants such as phenolic compounds. Phenolic compounds are praised for their biological activities and possible benefits on human health. Since no official methods are available for phenolic compound extraction, the optimization of extraction parameters via Response Surface Methodology (RSM) has become a commonly used methodological approach for reliable determinations. This study aimed to apply RSM to optimize the ultrasound-assisted extraction procedure of phenolic compounds, including anthocyanins, from black beans. A Generally Recognized As Safe solvent (ethanol) was used. Solvent concentration, extraction time, and solvent/sample ratio were optimized to maximize two responses: Total Anthocyanin Content (TAC) and Total Phenolic Content (TPC). An ethanol concentration of 64%, 30 min extraction time, and a 50 mL/g solvent/sample ratio were identified as the optimal extraction conditions. The TAC was 71.45 ± 1.96 mg cyanidin-3-O-glucoside equivalents 100 g⁻¹ dm, and the TPC was 60.14 ± 0.89 mg gallic acid equivalents 100 g⁻¹ dm. Among the pigmented phenolic compounds, cyanidin-3-O-glucoside and peonidin-3-O-glucoside were identified in the extracts. Regarding phenolic acids, caffeic, sinapic, and t-ferulic acids were detected. Full article

Chitosan is a fibrous compound derived from chitin, which is the second most abundant natural polysaccharide and is produced by crustaceans, including crabs, shrimps, and lobsters. Chitosan has all of the important medicinal properties, including biocompatibility, biodegradability, and hydrophilicity, and it is relatively nontoxic and cationic in nature. Chitosan nanoparticles are particularly useful due to their small size, providing a large surface-to-volume ratio, and physicochemical properties that may differ from that of their bulk counterparts; thus, chitosan nanoparticles (CNPs) are widely used in biomedical applications and, particularly, as contrast agents for medical imaging and as vehicles for drug and gene delivery into tumors. Because CNPs are formed from a natural biopolymer, they can readily be functionalized with drugs, RNA, DNA, and other molecules to target a desired result in vivo. Furthermore, chitosan is approved by the United States Food and Drug Administration as being Generally Recognized as Safe (GRAS). This paper reviews the structural characteristics and various synthesis methods used to produce chitosan nanoparticles and nanostructures, such as ionic gelation, microemulsion, polyelectrolyte complexing, emulsification solvent diffusion, and the reverse micellar method. Various characterization techniques and analyses are also discussed. In addition, we review drug delivery applications of chitosan nanoparticles, including for ocular, oral, pulmonary, nasal, and vaginal methodologies, and applications in cancer therapy and tissue engineering. Full article

Elderberry, which is well known for its richness in anthocyanin, is attracting attention in the bioindustry as a functional material with high antioxidant capacity. The aim of this study is to optimize extraction conditions to more effectively recover anthocyanins from elderberry. In a fundamental experiment to determine the suitable solvent, various GRAS reagents, such as acetone, ethanol, ethyl acetate, hexane, and isopropyl alcohol, were used, and total phenol and anthocyanin contents were detected as 9.0 mg/g-biomass and 5.1 mg/g-biomass, respectively, only in the extraction using ethanol. Therefore, ethanol was selected as the extraction solvent, and an experimental design was performed to derive a response surface model with temperature, time, and EtOH concentration as the main variables. The optimal conditions for maximal anthocyanin recovery were determined to be 20.0 °C, 15.0 min, and 40.9% ethanol, and the total anthocyanin content was 21.0 mg/g-biomass. In addition, the total phenol and flavonoid contents were detected as 67.4 mg/g-biomass and 43.8 mg/g-biomass, respectively. The very simple and economical extraction conditions suggested in this study contributed to improving the utilization potential of anthocyanin, a useful antioxidant derived from elderberry. Full article

This study aims to contribute to those valorization approaches for the recovery process of high-value-added substances in environmentally friendly ways. In this study, one of the most consumed juice products was selected for providing waste byproducts (peel). Sour cherry peels were subjected to automatic solvent extraction using a GRAS solvent (aqueous 80% ethanol, v/v). Then, encapsulation for the preservation of the related extract was performed by ionic gelation in alginate beads. The process conditions (gelling medium concentration, wall material concentration, and hardening time) were optimized by a Box–Behnken design (statistical experimental design approach). An almost 80% encapsulation efficiency was achieved under the proposed method (7.8% CaCI₂, 1.3% alginate, and 26 min). The inhibition effect of the produced capsules against DPPH (2,2-diphenyl-1-picrylhydrazil) radicals also shows that the current products might represent potential alternative natural antioxidants for food formulations. The morphological properties were also measured. Full article

The use of seaweed as a source of bioactive extracts has received increased attention from the market in recent years—particularly for nutraceutical applications. In this context, this study evaluated the nutraceutical application of seaweed biomass and extracts from three seaweeds from Portugal: Ulva sp., Laminaria ochroleuca, and Chondrus crispus. For each of the said seaweeds, four different extracts were obtained using GRAS solvents—acetone (A), ethanol (E), ethanol–water (1:1) (EW), and one polysaccharide-rich extract (P) using water and further precipitation with ethanol. The bioactive potential of the extracts was assessed in terms of antioxidant capacity (ABTS^•+, DPPH^•, ^•NO, O₂^•− scavenging, and ORAC-FL assay) and anti-inflammatory capacity (COX inhibition and human red blood cell membrane stabilisation). Furthermore, the biochemical profile was determined for the raw biomass and extracts to better comprehend their possible applications as nutraceuticals. The results show that all extracts have antioxidant potential. Five extracts (L. ochroleuca E, EW, and P and Ulva sp. E and P) showed anti-inflammatory capacity. Overall, L. ochroleuca EW extract exhibited the most promising potential as both an antioxidant and anti-inflammatory and is an interesting candidate nutraceutical ingredient. Full article