Search Results (149)

The development of sustainable and efficient sample-preparation strategies remains a key challenge in analytical workflows for plant-derived bioactive compounds. In this study, choline chloride (ChCl)-based natural deep eutectic solvents (NADES) were systematically investigated as green extraction media and combined with chemical and enzyme assays to identify the bioactive effect of phenolic compounds from Bellevalia dubia, an understudied Mediterranean plant. A design of experiments approach was applied to evaluate the influence of hydrogen bond donors (lactic, malic, and citric acid) and their molar ratios on extraction performance. Among the tested systems, the ChCl–malic acid (MA) mixture at a molar ratio of 1:2.5 (precisely 1:2.47) was identified as the best overall solution according to the desirability approach, which integrated both phytochemical and enzyme-inhibitory responses. This system also showed strong enzyme-inhibitory effects compared to conventional extractants (water and 80% methanol). To identify the extract composition, a suspect screening workflow was applied based on ultra-high-performance liquid chromatography hybrid quadrupole Orbitrap mass spectrometry (UHPLC–q-Orbitrap-MS). Twenty-one compounds were detected and annotated, mainly belonging to the flavonoid class. Principal component analysis (PCA) showed that ChCl-MA extracts were discriminated, particularly at molar ratio 1:2.5, from the rest, indicating a distinct chemical and bioactivity profile. PCA further suggested a possible association of the ChCl-MA 1:2.5 system with vitexin and AChE inhibition, which requires further investigation. Overall, the proposed NADES-based approach offers a tunable, promising, and potentially more sustainable alternative for the extraction of bioactive compounds from plant-based sources. Full article

The transition from predatory extractive economies to high-technology systems centered on the standing forest paradigm represents a defining sustainability challenge for the Global South. This integrative review establishes a novel socio-technical and technological architecture, conceptualized as Amazonian Nanobioeconomy 5.0, by critically synthesizing the convergence of the Amazonian lipid pharmacopeia, Natural Deep Eutectic Solvents (NaDESs), and Artificial Intelligence/Machine Learning (AI/ML) optimization. We critically evaluate how data-driven green nanomanufacturing can overcome the empirical trial-and-error bottlenecks and severe chemical variability inherent to native biodiversity oils and butters. The integration of predictive algorithms—such as tree-based models and Bayesian optimization—with eco-friendly extraction media enables the rational design of solid lipid nanoparticles (SLNs) and Nanostructured Lipid Carriers (NLCs) while accelerating their translation across the biotechnological “Valley of Death”. Under the Safe-and-Sustainable-by-Design (SSbD) framework, this convergence offers a composition-dependent green alternative to harmful petrochemical volatile organic compounds, fosters circular biorefineries, and minimizes the global environmental footprint of advanced nanopharmaceuticals and cosmeceuticals. Finally, we articulate how this digital and green deep-tech infrastructure must be non-negotiably tethered to strict territorial governance, fair benefit-sharing, and epistemic justice to prevent data colonialism and foster a truly just planetary transition. Full article

Citrus aurantium L. by-products are a valuable source of bioactive compounds with potential industrial applications. This study evaluated the use of natural deep eutectic solvents (NADESs), formulated with choline chloride as the hydrogen bond acceptor (HBA) and fructose as the hydrogen bond donor (HBD), combined with ultrasound-assisted extraction to optimize the recovery of flavonoids from Citrus aurantium L. industrial by-products. A central composite design (CCD) was employed to optimize total flavonoid content (TFC). The molar ratio (MR; 1 and 2 mol of HBD per mol of HBA) and the percentage of added water (AW; 40 and 60%) were optimized. In addition to TFC, total phenolic content (TPC), total ascorbic acid (TAA), antioxidant capacity (Ax) and phenolic profiles were also evaluated. The optimal extraction conditions, as obtained by Response Surface Methodology (RSM) for TFC, corresponded to an HBD molar ratio of 1.33 per 1 mol of HBA and 47.48% added water, resulting in an optimal value of 1576.63 ± 4.9 mg quercetin equivalents (QE)/100 g dry mass (DM). Maximum values of 4276.94 ± 25.4 mg gallic acid equivalents (GAE)/100 g DM for TPC, 2077.66 ± 21.3 mg/100 g DM for TAA and 88.09 ± 0.1% inhibition for Ax were also obtained. The optimal NADES was characterized by density, viscosity, pH, Fourier-transform infrared (FTIR) and Raman spectroscopy. Additionally, phenolic profiling revealed high concentrations of hesperidin (2747.1 mg/100 g DM), naringenin (1251.93 mg/100 g DM), and quercetin + luteolin (660.65 mg/100 g DM). Full article

Jarosite residues generated during zinc hydrometallurgy may retain valuable metals such as silver within complex and poorly accessible mineral phases. In this study, hydrated reline, a choline chloride–urea natural deep eutectic solvent (NADES), was evaluated as an alternative leaching medium for silver recovery from an industrial jarosite residue. Reline/water mixtures containing 10, 20, and 30 wt.% water (RE9010, RE8020, and RE7030, respectively) were investigated to determine the influence of solvent hydration and temperature (25–80 °C) on silver extraction. Mineralogical characterization by XRD, SEM–EDS, and automated TIMA analysis revealed a heterogeneous residue in which silver-bearing phases are associated with complex mineral assemblages, potentially limiting their accessibility during leaching. Among the evaluated systems, RE9010 consistently exhibited the highest silver recovery, increasing from 12.83% at 25 °C to 24.10% at 80 °C. Successive leaching cycles further increased the cumulative silver recovery to 34.7% for RE9010. FTIR analysis showed that the characteristic spectral features of reline were preserved after the addition of up to 30 wt.% water. Kinetic analysis indicated that diffusion-based models provided the best description of the leaching behavior, with the Zhuravlev–Lesokhin–Templeman model showing the best overall fit. An apparent activation energy of 18.4 kJ mol⁻¹ was obtained, supporting the contribution of mass-transfer and diffusion phenomena to the overall process. These results demonstrate that controlled hydration and moderate heating can improve the leaching performance of reline while preserving its characteristic interactions, highlighting its potential as an alternative solvent for silver recovery from complex metallurgical residues. Full article

Edible Natural Deep Eutectic Solvents (NADES) offer a route to ready-to-use extracts without solvent removal. This study examined how rational formulation design influences physicochemical properties, extraction performance, energy efficiency, thermal behavior, and cytocompatibility during bioactive recovery from Nigella sativa seeds. Twelve formulations spanning malic acid–polyol, citric acid–polyol, binary polyol, and ternary acid–polyol families were evaluated under standardized ultrasound-assisted conditions and compared with ethanolic ultrasound-assisted extraction, Soxhlet extraction, and cold-pressed oils. Selected NADES formulations outperformed the conventional systems. E1 (malic acid:glycerol:water) achieved the highest total phenolic content and lowest specific energy consumption (40.00 kJ mg⁻¹ GAE), below the Soxhlet benchmark (55.17 kJ mg⁻¹ GAE), whereas E9 (glycerol:xylitol:water) exhibited the greatest ABTS activity. Neat-NADES apparent pH and viscosity were inversely associated with total phenolic content, while viscosity and density were inversely associated with ABTS activity. ATR-FTIR showed stable, solvent-dominated fingerprints over 15 days, whereas DSC better differentiated neat NADES from their extracts. Most systems remained cytocompatible at 10,000× dilution, while acid–polyol formulations reduced viability at 500×; partial neutralization of N5/E5 restored viability. NADES performance was formulation- and application-dependent, requiring joint optimization of composition, acidity, viscosity, energy efficiency, and biologically compatible concentration. Full article

Textile waste is no longer dominated by simple single-polymer materials. Most post-consumer textiles contain combinations of natural and synthetic fibres, elastane, dyes, coatings, finishes, and other additives, which makes selective recycling considerably more difficult. Deep eutectic solvents (DES) offer a promising route for addressing this complexity because their composition and physicochemical properties can be widely tuned. However, the outcome of DES treatment is often discussed mainly in terms of solvent composition or solvent–polymer affinity, although these factors alone cannot explain why similar DES formulations may lead to different responses in different polymeric or textile systems. In this review, DES-assisted textile recycling is examined from a mechanistic polymer-science perspective. The discussion focuses on how polymer morphology, transport accessibility, supramolecular organization, chemical reactivity, and processing conditions jointly determine whether a material undergoes swelling, molecular dissolution, structural destabilization, or chemical degradation. Particular attention is paid to the distinction between these processes, since changes in sample mass, fibre appearance, or crystallinity do not by themselves prove either true polymer dissolution or chain scission. Evidence from cellulose-based fibres, polyesters, polyamides, polyurethanes, elastane-containing materials, and multicomponent textile systems is used to show how different material outcomes may arise from apparently related DES–polymer interactions. The reviewed studies indicate that selectivity in DES-assisted textile recycling should not be treated as a fixed property of the solvent or of the polymer alone. It is more appropriately understood as the result of a coupled and time-dependent interaction between the DES medium, polymer morphology, textile architecture, and processing conditions. The mechanistic framework proposed here provides a basis for comparing reported DES-based recycling strategies, identifying the experimental evidence needed to support mechanistic claims, and guiding the rational selection of DES composition, process conditions, and recovery pathways for complex textile waste. Full article

Background/Objectives: The pharmacological management of inflammation remains a clinical challenge, driving the demand for advanced topical formulations. This study utilizes a “smart-NADES” (natural deep eutectic solvent) paradigm to develop an innovative anti-inflammatory topical system. The aim was to evaluate the integrated antioxidant potential, alongside the in vitro and in vivo anti-inflammatory activities, of a novel smart-NADES licorice root extract and its hydrogel formulation. Methods: A NADES system composed of D-sorbitol and L-lactic acid (3:1) was employed for licorice root extraction. The antioxidant capacity was assessed using three independent assays and integrated via the Relative Antioxidant Capacity Index (RACI), while phytochemical interactions were quantified using the Chou–Talalai Combination Index (CI). In vitro anti-inflammatory activity was evaluated via protein stabilization capacity, and in vivo efficacy was validated using a formalin-induced paw edema model in mice. Results: The NADES extract contained glycyrrhizic acid levels of 6.3 ± 0.3 mg/g and showed strong antioxidant synergism in the DPPH assay (CI = 0.49 ± 0.07). The extract exhibited potent total antioxidant capacity (IC₅₀ = 11.9 ± 0.6 μg/mL) with a superior RACI score (1.23). In vitro protein stabilization (IC₅₀ = 63 ± 5 μg/mL) was comparable to diclofenac sodium. The 5% hydrogel numerically surpassed the commercial 2% diclofenac Emulgel (67.5% vs. 32.9% inhibition, respectively) at 24 h, although the direct pairwise comparison did not reach statistical significance (p = 0.186). Conclusions: The developed smart-NADES licorice hydrogel represents an effective, green formulation with pronounced topical anti-inflammatory properties, establishing a robust pharmacological rationale for advanced topical drug delivery. Full article

The increasing prevalence of presbyphagia and mild dysphagia among adults over 65 years (International Dysphagia Diet Standardisation Initiative, IDDSI, levels 4–6) has increased the demand for texture-modified foods that ensure safe swallowing while providing added health benefits. This study aimed to develop functional gummy-like systems containing grape pomace extracts obtained by ultrasound-assisted extraction using either a natural deep eutectic solvent (NaDES; choline chloride:citric acid, 1:1) or water, and to evaluate the effects of extraction medium and formulation composition on their physicochemical, textural, and bioactive properties. A simplex-centroid mixture design was used to assess the combined effects of gelatin (4–8%), low-methoxyl pectin (1–3%), and extract concentration (5–10%). NaDES-based formulations exhibited lower water activity and a more homogeneous moisture distribution than aqueous counterparts, indicating improved water structuring within the gel network. Intermediate gelatin–pectin ratios produced cohesive matrices with moderate firmness, consistent with IDDSI levels 5–6. Formulation F5 (6% gelatin, 1% pectin, 7.5% extract) showed the best overall performance, combining favorable textural properties with the highest total polyphenol content and antioxidant activity. These findings support the use of NaDES-extracted grape pomace for developing functional foods suitable for individuals with dysphagia. Full article

Urtica dioica L. (stinging nettle) is a perennial herb with a long ethnomedicinal history and diverse pharmacological potential. This comprehensive review consolidates current knowledge on its phytochemistry, extraction technologies, bioactivities, and molecular mechanisms. However, recent reviews have generally addressed these aspects separately, and an integrated assessment linking green extraction technologies and phytochemical profiles to molecular mechanisms and gene expression modulation is still lacking. U. dioica contains abundant polyphenols (rutin, quercetin, kaempferol, and chlorogenic acid), sterols (β-sitosterol and stigmasterol), vitamins, carotenoids, and the antiviral lectin Urtica dioica agglutinin (UDA). Advances in green extraction technologies, such as ultrasound-assisted extraction, microwave-assisted extraction (MAE), pressurized liquid extraction, and natural deep eutectic solvent (NADES)-based systems, have significantly improved yield, purity, and environmental sustainability compared to conventional maceration and Soxhlet methods. Comprehensive chromatographic and spectroscopic profiling (HPLC, GC–MS, FTIR, NMR, and LC–MS/MS) has established detailed chemical fingerprints linking bioactive constituents to antioxidant, anti-inflammatory, antimicrobial, and antiviral properties. Mechanistic studies reveal that U. dioica exerts its therapeutic effects through modulation of oxidative stress, inhibition of the NF-κB and COX-2 pathways, enhancement of endogenous antioxidant enzymes, and regulation of apoptotic gene expression. Moreover, NADES–MAE extracts demonstrate potential as sustainable, high-efficacy formulations for nutraceutical and cosmetic applications. Despite extensive preclinical evidence, clinical standardization and dosage optimization remain major challenges. This review underscores U. dioica as a multifunctional medicinal plant with significant promise for next-generation phytotherapeutics and molecular nutrition. Full article

Increasing consumer demand for safer and more sustainable food preservation has stimulated interest in natural pigments as multifunctional components in active and intelligent food systems. This review critically summarizes curcumin-, anthocyanin-, and carotenoid-based systems for food preservation and freshness monitoring, focusing on their mechanisms, material strategies, food-matrix-dependent performance, and technological challenges. Curcumin mainly contributes antioxidant, antimicrobial, and photoresponsive functions, especially photodynamic inactivation when supported by suitable carriers. Anthocyanins provide pH- and amine-responsive colorimetric signals for intelligent freshness monitoring, whereas carotenoids primarily protect oxidation-sensitive foods through radical quenching and lipid oxidation inhibition. Recent incorporation of these pigments into biopolymer films, edible coatings, emulsions, nanocarriers, hydrogels, aerogels, cyclodextrin complexes, metal–organic frameworks, and deep eutectic solvent-assisted systems has improved pigment stability, dispersion, barrier performance, and controlled release. However, poor solubility, environmental instability, matrix interference, migration safety, sensory impacts, quantitative calibration, and scalability remain unresolved. Future development should emphasize mechanism-guided formulation, real-food validation, and safe, stable, scalable pigment-based systems tailored to specific deterioration pathways and commercial applications. Full article

Phlorotannins are the characteristic phenolic metabolites of brown seaweeds and represent one of the most chemically diverse, analytically challenging, and industrially promising classes of marine polyphenols. Unlike terrestrial phenolics, phlorotannins are formed from phloroglucinol units and occur as complex mixtures of fucols, phlorethols, fuhalols, fucophlorethols, eckols, and related oligomeric or polymeric structures whose composition varies strongly with species, tissue, season, habitat, extraction protocol, and purification strategy. This review critically examines brown seaweed phlorotannins across five major dimensions: chemical diversity and species-dependent availability; extraction, enrichment, and sustainable solvent strategies, including natural deep eutectic solvents (NADES); analytical challenges and advances in selective quantification, highlighting the non-specific nature of Folin–Ciocalteu assays and the emerging value of selective qNMR-based quantification; and biological relevance to ageing-associated processes such as oxidative stress, inflammation, glycation, metabolic dysfunction, neurodegeneration, and skin ageing. The review further evaluates translational barriers, including poor standardization, uncertain bioavailability, matrix interference, limited compound-specific standards, and insufficient in vivo and clinical validation. Finally, a phlorotannin-first brown seaweed biorefinery framework is proposed, in which the phenolic fraction is recovered early as a high-value stream before sequential valorization of polysaccharides, proteins, pigments, minerals, and residual biomass. This integrated perspective highlights the need to move from crude “total phenolic” descriptions toward chemically defined, functionally validated, and industrially scalable phlorotannin systems. Full article

Deep eutectic solvents (DESs) have emerged as promising green extraction media for natural bioactive compounds, offering tunable physicochemical properties, biocompatibility, and lower toxicity than conventional organic solvents. However, the high viscosity of DESs limits mass transfer efficiency, necessitating integration with auxiliary technologies to overcome this intrinsic constraint. Unlike previous reviews that focus on DESs coupled with a single auxiliary technique, this review for the first time integrates DESs with ultrasound, microwave, enzymatic assistance, and multi-technique hybrid systems into a unified framework, critically comparing their enhancement mechanisms, applicability boundaries, and industrial feasibility. This review systematically examines the non-covalent interactions between DES components and target compounds, including hydrogen bonding, van der Waals forces, and electrostatic interactions, and discusses how these interactions guide the rational selection of hydrogen bond acceptors (HBAs) and donors (HBDs) for specific compound classes. We analyze the distinct mechanisms by which ultrasound, microwave, and enzymatic assistance synergistically enhance DES extraction performance, with particular attention to viscosity reduction, cell wall disruption, and biocatalytic compatibility. Recent advances in the extraction of polyphenols, alkaloids, terpenoids, and polysaccharides are summarized to illustrate the practical application of these principles. Finally, we discuss current challenges in industrial scale-up, including solvent recovery, equipment adaptation for high-viscosity media, and regulatory considerations, and outline future directions toward intelligent solvent design and continuous processing. By integrating molecular-level mechanistic insights with process engineering perspectives, this review provides a comprehensive framework for the optimization and application of DES-based extraction technologies. Full article

Fish processing by-products represent a valuable and sustainable source of collagen for biomedical and functional applications. In the present study, collagen was extracted from the scales of red mullet (Mullus barbatus), gilthead sea bream (Sparus aurata), and European sea bass (Dicentrarchus labrax) using a green extraction approach based on a natural deep eutectic solvent (NADES) system composed of citric acid, xylitol, and water. The extracted collagens were comprehensively characterized by SDS-PAGE, Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and X-ray diffraction (XRD) analyses. The results confirmed the presence of Type I collagen and demonstrated that the characteristic triple-helical structure and molecular organization were preserved throughout the extraction process. To preliminarily evaluate their potential as matrices for incorporating bioactive compounds, collagen matrices were combined with Zingiber officinale (ginger) extract at different ratios. The resulting combinations were evaluated for antioxidant, antimicrobial, and cytocompatibility properties. Antioxidant activity increased significantly with increasing ginger concentration, with the highest radical scavenging activity observed in combinations containing the greatest proportion of ginger extract. Similarly, antimicrobial activity against Escherichia coli and Staphylococcus aureus was enhanced by ginger incorporation, with stronger inhibition observed against the Gram-positive bacterium. Cytocompatibility studies performed on human dermal fibroblast (HDFa) cells revealed that selected collagen–ginger combinations maintained high cell viability and did not induce substantial membrane damage, nuclear abnormalities, apoptosis, or necrosis at appropriate concentrations. Overall, the findings demonstrate that fish scale-derived collagen obtained through a sustainable NADES-based extraction process possesses favorable structural and biological properties and may serve as a potential carrier matrix for plant-derived bioactive compounds. These findings provide preliminary evidence supporting the future development of environmentally friendly functional biomaterials with prospective applications in pharmaceutical, biomedical, and tissue engineering fields. Full article

Rubusoside is the major sweet bioactive compound in Rubus chingii var. suavissimus (S.K.Lee) L.T.Lu, characterized by high sweetness, low caloric value, and favorable safety, with potential applications as a natural sweeteners and in functional foods. However, efficient green extraction technologies and their mechanisms remain insufficiently explored. Here, a microwave-assisted deep eutectic solvent (DES) system was developed for rubusoside recovery. The ternary DES composed of choline chloride, 1,2-propylene glycol, and 1,3-butanediol (1:2:2) showed the best performance and outperformed microwave-assisted water extraction. Response surface methodology identified optimal conditions of 33% moisture content, a liquid–solid ratio of 21 mL/g, 6 min, and 320 W, yielding 7.89 ± 0.25% rubusoside. Fourier-transform infrared spectroscopy, electrostatic potential, atoms-in-molecules theory, and independent gradient modelling based on Hirshfeld partition analyses revealed significant non-covalent interactions between the ternary DES and rubusoside. Scanning electron microscopy showed that DES and microwave treatment synergistically disrupted plant tissues and enhanced mass transfer. LX-28 macroporous resin enabled rubusoside separation, and the recovered DES retained stable performance after five reuse cycles. These results demonstrate a green, efficient, and recyclable strategy driven by cooperative hydrogen bonding and van der Waals interactions between the ternary DES and the rubusoside glycosyl moiety, together with DES–microwave-induced tissue disruption and mass-transfer enhancement. Full article

Proanthocyanidins, a new class of potent antioxidants, are recognized for their strong in vivo activity and occur in high abundance in Lycium ruthenicum. Although the extraction of these compounds from this plant has been extensively investigated, their inherent instability imposes stringent demands on the extraction process. Natural deep eutectic solvents (NADESs) have emerged as attractive alternatives for isolating bioactive constituents from plant materials thanks to their favorable biocompatibility, high extraction efficiency, and environmentally benign nature. Therefore, we have developed an efficient and green NADES-assisted ultrasonic extraction method for recovering proanthocyanidins from Lycium ruthenicum. Among the fourteen NADES formulations screened, the choline chloride–glycerol system (1:5 molar ratio, 30% v/v water) afforded the highest extraction yield. Single-factor experiments, combined with response surface methodology, led to the optimal conditions: solid-to-liquid ratio 1:15 g/mL, ultrasonic power 240 W, temperature 40 °C, and time 30 min. Under these conditions, the proanthocyanidin yield reached 12.19%, markedly outperforming that obtained with conventional methanol extraction. Kinetic analysis indicated that the extraction process conformed to the Logistic model, with coefficients of determination (R²) greater than 0.967 across the entire temperature range studied (20–50 °C). In vitro antioxidant assays further revealed that the extract exhibited significant concentration-dependent scavenging activities against •OH, DPPH•, and ABTS⁺• radicals. The IC₅₀ values of proanthocyanidin extracts for •OH, DPPH•, and ABTS⁺• were 0.029 mg/mL, 0.56 μg/mL, and 0.011 mg/mL, respectively. Overall, these results establish a sustainable NADES-based protocol for the extraction of proanthocyanidins from Lycium ruthenicum, and underscore their promise as natural antioxidants for functional food and pharmaceutical uses. Full article