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21 pages, 2074 KiB  
Article
Preliminary Analysis of Bilberry NaDES Extracts as Versatile Active Ingredients of Natural Dermocosmetic Products: In Vitro Evaluation of Anti-Tyrosinase, Anti-Hyaluronidase, Anti-Collagenase, and UV Protective Properties
by Milica Martinović, Ivana Nešić, Ana Žugić and Vanja M. Tadić
Plants 2025, 14(15), 2374; https://doi.org/10.3390/plants14152374 - 1 Aug 2025
Viewed by 199
Abstract
Bilberry (Vaccinium myrtillus L.) fruits represent the recognized wellspring of bioactive compounds with various documented bioactivities. Although bilberry leaves are often treated as industrial by-products, they also represent a valuable source of phytochemicals with potential dermocosmetic applications. In this study, extracts of [...] Read more.
Bilberry (Vaccinium myrtillus L.) fruits represent the recognized wellspring of bioactive compounds with various documented bioactivities. Although bilberry leaves are often treated as industrial by-products, they also represent a valuable source of phytochemicals with potential dermocosmetic applications. In this study, extracts of bilberry fruits and leaves were prepared using both conventional solvents (water and 50% ethanol) and natural deep eutectic solvents (NaDES) as green, biodegradable alternatives. The aim of this study was to examine the UV protective activity and inhibitory potential of those extracts against some enzymes (tyrosinase, hyaluronidase, collagenase) that are important in terms of skin conditioning and skin aging. The results of in vitro tests have shown the superiority of NaDES extracts compared to conventional extracts regarding all tested bioactivities. In addition, bilberry leaves extracts were more potent compared to fruit extracts in all cases. The most potent extract was bilberry leaf extract made with malic acid–glycerol, which exhibited strong anti-tyrosinase (IC50 = 3.52 ± 0.26 mg/mL), anti-hyaluronidase (IC50 = 3.23 ± 0.30 mg/mL), and anti-collagenase (IC50 = 1.84 ± 0.50 mg/mL) activities. The correlation analysis revealed correlation between UV protective and anti-tyrosinase, UV protective and anti-collagenase as well as between anti-hyaluronidase and anti-collagenase activity. UV protection and anti-tyrosinase activity correlated significantly with chlorogenic acid and hyperoside contents in extracts. The extracts with the best activities also demonstrated a good safety profile in a 24 h in vivo study on human volunteers. Full article
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25 pages, 3993 KiB  
Article
Green Chemistry and Multivariate Optimization in the Extraction of Phenolic Compounds: The Potential of NaDES in Alternative Raw Materials for Expanded Extrudates
by Mateus Alves Araújo, Bianca Rodrigues Morais, João Pedro da Silva Santos, Larissa Karla de Jesus, Kaliston Aurélio Lomba, Gustavo Costa do Nascimento, Marcus Alvarenga Soares, Nathalia de Andrade Neves, Irene Andressa, Maria Teresa Pedrosa Silva Clerici and Marcio Schmiele
Methods Protoc. 2025, 8(4), 82; https://doi.org/10.3390/mps8040082 - 23 Jul 2025
Viewed by 360
Abstract
Phenolic compounds are secondary metabolites widely distributed among plants, with bioactive properties, especially antioxidant activity. The search for sustainable extraction methods has driven the use of natural deep eutectic solvents (NaDESs), formed by combinations of natural compounds, such as organic acids, sugars, alcohols, [...] Read more.
Phenolic compounds are secondary metabolites widely distributed among plants, with bioactive properties, especially antioxidant activity. The search for sustainable extraction methods has driven the use of natural deep eutectic solvents (NaDESs), formed by combinations of natural compounds, such as organic acids, sugars, alcohols, and amino acids. This study optimized NaDES (sorbitol, citric acid, and glycine) efficiency and compared it to that of 70% methanol solution in extracting total soluble phenolic compounds (TSPCs) from six flours matrices—corn, buckwheat, biofortified orange sweet potato, red lentil, Sudan grass, and chickpea—before and after thermoplastic extrusion cooking. Quantification was performed using the Folin–Ciocalteu method, with statistical analysis at the 10% significance level. In general, the methanolic extracts showed higher TSPC levels in the raw materials, whereas the levels were higher in NaDESs for legumes. After extrusion, a reduction in the TSPC levels was observed, except in the sweet potato. Multivariate analysis (PLS-DA and heatmap) distinguished the raw and extruded samples, revealing structural and chemical changes from thermal processing. The AGREE scores were 0.7 (NaDES) and 0.54 (methanol), favoring NaDES. The BAGI score (75.0) confirmed the method’s robustness and suitability for sustainable analytical applications. Full article
(This article belongs to the Collection Green Chemistry)
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21 pages, 2632 KiB  
Article
Natural Deep Eutectic Solvent-Based Extraction of Malva sylvestris L.: Phytochemical Content, Antioxidant and Antimicrobial Potential
by Neli Memdueva, Milena Tzanova, Zvezdelina Yaneva, Nikolina Rusenova, Neli Grozeva and Toncho Dinev
Separations 2025, 12(7), 187; https://doi.org/10.3390/separations12070187 - 20 Jul 2025
Viewed by 322
Abstract
Malva sylvestris L. is a herbaceous plant, distributed worldwide, rich in biological active compounds, and known for its health benefits. In this study, extracts from different parts (leaves, flowers, and roots) of this plant were prepared using green classic (70% ethanol) and natural [...] Read more.
Malva sylvestris L. is a herbaceous plant, distributed worldwide, rich in biological active compounds, and known for its health benefits. In this study, extracts from different parts (leaves, flowers, and roots) of this plant were prepared using green classic (70% ethanol) and natural deep eutectic solvents (NADESs) based on choline chloride and acetic acid (NADES1) or glycerol (NADES2). Their antioxidant, antibacterial (against B. cereus, S, aureus, E. coli, and P. aeruginosa), and antifungal activity (against P. chrysogenum, F. oxysporum, A. parasiticus, A. flavus, A. niger A. carbonarius, and A. ochraceus) were compared. Ethanolic extracts were characterized with the highest total contents of phenols, flavonoids, and condensed tannins. Ethanolic and NADES flower extracts were the richest in the antioxidants tested. Alkaloids were extracted in low quantities. The experimentally determined antioxidant potential of the extracts proved the highest DPPH scavenging activity of ethanolic extracts and the lowest of NADES1 extracts. The ABTS scavenging capacity of NADES1 and ethanolic extracts displayed comparable results, while NADES2 extracts were characterized as having the highest FRAP activity. NADES1 extracts manifested pronounced antibacterial activity, partially due to the low pH of the pure solvent, as well as inconsistent antifungal activity—from moderate to a complete lack of activity. A strong positive correlation was reported between the DPPH radical scavenging capacity and phenolic compound content. Future detailed investigations on the mechanism of the antimicrobial activity of NADES1 extracts are necessary to clarify the observed phenomenon of the decreased antifungal potential of NADES1 extracts compared to the pure solvent NADES1. Full article
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14 pages, 586 KiB  
Article
NaDES-Based Extracts by Microwave Activation from Laurus nobilis L. Leaves: Sustainable Multifunctional Ingredients for Potential Cosmetic and Pharmaceutical Applications
by Debora Caviglia, Eleonora Russo, Anna Maria Schito, Francesco Saverio Robustelli della Cuna, Elena Grignani, Nicola Lionetti and Carla Villa
Molecules 2025, 30(14), 3006; https://doi.org/10.3390/molecules30143006 - 17 Jul 2025
Viewed by 342
Abstract
Laurus nobilis L. is a widely cultivated plant, used for ornamental purposes, as a high-value spice crop, and in the flavor and fragrance industry. In natural medicine, it is well-known for its many beneficial properties (due to a broad spectrum of biologically active [...] Read more.
Laurus nobilis L. is a widely cultivated plant, used for ornamental purposes, as a high-value spice crop, and in the flavor and fragrance industry. In natural medicine, it is well-known for its many beneficial properties (due to a broad spectrum of biologically active compounds) and used for the treatment of different disorders. In this study, natural deep eutectic solvents (NaDESs), coupled with microwave activation, were studied and applied for a green extraction of L. nobilis leaves. The main objective was to obtain a sustainable and multifunctional cosmetic and pharmaceutical ingredient (the NaDES-based extract itself), exploiting both the intrinsic cosmetic functionalities of NaDES components and the biological properties of laurel bioactive compounds. The most promising candidate was obtained from a eutectic system containing betaine, glycerol, and lactic acid. The evaluation of this NaDES-based complex reveals a considerable number of phenolic compounds (around 11.57 mg of gallic acid equivalents for a gram of fresh leaves) and a notable antioxidant activity (80.1% with respect to Trolox), with values quite constant over a period of six months. The complex exhibits effective antimicrobial activity against different Gram-positive (S. aureus and S. epidermidis) and Gram-negative (E. coli and P. aeruginosa) bacterial strains, with concentrations ranging from 3.8 to 7.5 mg/mL. Furthermore, the extract presents a pleasant fragrance, attributable to the selective extraction of different volatile aromatic compounds, as confirmed by GC-MS analysis. Full article
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15 pages, 990 KiB  
Article
Towards a Green and Sustainable Valorization of Salix amplexicaulis: Integrating Natural Deep Eutectic Solvents and Microwave-Assisted Extraction for Enhanced Recovery of Phenolic Compounds
by Milica Vidić, Nevena Grujić-Letić, Branislava Teofilović and Emilia Gligorić
Sustainability 2025, 17(14), 6347; https://doi.org/10.3390/su17146347 - 10 Jul 2025
Viewed by 309
Abstract
Combining advanced extraction technologies with non-pollutant solvents represents a sustainable approach toward valorizing medicinal plants and aligns with the principles of green chemistry. This study aimed to evaluate the efficiency of microwave-assisted extraction (MAE) combined with natural deep eutectic solvents (NADES) to extract [...] Read more.
Combining advanced extraction technologies with non-pollutant solvents represents a sustainable approach toward valorizing medicinal plants and aligns with the principles of green chemistry. This study aimed to evaluate the efficiency of microwave-assisted extraction (MAE) combined with natural deep eutectic solvents (NADES) to extract bioactive compounds from the underexplored leaves and bark of Salix amplexicaulis Bory & Chaub. Additionally, the potential of NADES as sustainable alternatives to conventional solvents was assessed through a comparative evaluation of MAE-NADES with MAE–water and traditional ethanol maceration. NADES based on lactic acid–glycerol, lactic acid–glucose, glycerol–glucose, and glycerol–urea were synthesized by heating and stirring. Willow extracts were characterized by HPLC-DAD, resulting in the identification and quantification of seven phenolic acids and four flavonoids. Lactic acid–glucose (5:1)-based NADES extracted the highest number of phenolics in the greatest amount from the bark and leaves of S. amplexicaulis. MAE-NADES offers a fast, cost-effective preparation, high extraction efficiency, and environmentally friendly properties, opening new perspectives on the valorization of S. amplexicaulis in the pharmaceutical field. Furthermore, NADES provide a promising alternative to water and toxic organic solvents for extracting bioactives. Full article
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20 pages, 1663 KiB  
Article
Microwave–Ultrasound-Assisted Extraction Coupled with Natural Deep Eutectic Solvent Enables High-Yield, Low-Solvent Recovery of Curcumin from Curcuma longa L.
by Muhammad Sahlan, Desy Rosarina, Hasna Farida Ratna Suminar, Yoga Diatama Pohan, Ibnu Maulana Hidayatullah, Dimas Rafi Narawangsa, Dwini Normayulisa Putri, Eka Sari, Meka Saima Perdani, Yudha Gusti Wibowo and Heri Hermansyah
Pharmaceutics 2025, 17(7), 818; https://doi.org/10.3390/pharmaceutics17070818 - 24 Jun 2025
Viewed by 443
Abstract
Background/Objectives: Solvent-intensive methods are traditionally required to extract curcumin, a potent bioactive compound from Curcuma longa, raising environmental and safety concerns. Methods: This study introduces an efficient and scalable extraction approach using microwave–ultrasound-assisted extraction (MUAE) combined with a natural deep [...] Read more.
Background/Objectives: Solvent-intensive methods are traditionally required to extract curcumin, a potent bioactive compound from Curcuma longa, raising environmental and safety concerns. Methods: This study introduces an efficient and scalable extraction approach using microwave–ultrasound-assisted extraction (MUAE) combined with a natural deep eutectic solvent (NADES) composed of choline chloride and lactic acid. Process parameters, including solvent water content (20–30% v/v) and solid loading (4–8% w/v), were optimized using response surface methodology (RSM) to enhance curcumin yield. Results: Under optimal conditions (20% water content and 8% solid loading), the MUAE method achieved a curcumin content of 40.72 ± 1.21 mg/g, representing a 14.36% improvement over conventional ultrasound-assisted extraction (UAE), while reducing solvent usage by 50%. The quadratic model demonstrated excellent predictive capability, with an R2 value of 0.98. In addition, anti-solvent precipitation using water increased curcuminoid purity from 0.31% to 20.54%, with a recovery rate of 21.49%. Conclusions: Mechanistic analysis revealed that microwave-induced cell disruption, ultrasound cavitation, and the modulation of NADES viscosity contributed synergistically to the enhanced extraction performance. This study is the first to combine MUAE with NADES for optimized curcumin extraction, delivering both high yield and reduced solvent consumption. The proposed method offers a sustainable and industrially relevant alternative for curcumin recovery in the food, nutraceutical, and pharmaceutical sectors. Full article
(This article belongs to the Section Pharmaceutical Technology, Manufacturing and Devices)
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20 pages, 2721 KiB  
Article
Natural Deep Eutectic Solvents (NADESs) for the Extraction of Bioactive Compounds from Quinoa (Chenopodium quinoa Willd.) Leaves: A Semi-Quantitative Analysis Using High Performance Thin-Layer Chromatography
by Verónica Taco, Dennys Almachi, Pablo Bonilla, Ixchel Gijón-Arreortúa, Samira Benali, Jean-Marie Raquez, Pierre Duez and Amandine Nachtergael
Molecules 2025, 30(12), 2620; https://doi.org/10.3390/molecules30122620 - 17 Jun 2025
Viewed by 416
Abstract
Natural deep eutectic solvents (NADESs) have emerged as a promising eco-friendly alternative to petrochemicals for extracting plant metabolites. Considering that the demand for sustainable “green” ingredients for industrial applications is growing, those solvents are purported to develop extracts with interesting phytochemical fingerprints and [...] Read more.
Natural deep eutectic solvents (NADESs) have emerged as a promising eco-friendly alternative to petrochemicals for extracting plant metabolites. Considering that the demand for sustainable “green” ingredients for industrial applications is growing, those solvents are purported to develop extracts with interesting phytochemical fingerprints and biological activities. Given the interest in flavonoids from Chenopodium quinoa Willd. leaves, an efficient “green” extraction method was developed by investigating eight NADESs with defined molar ratios, i.e., malic acid-choline chloride (chcl)-water (w) (1:1:2, N1), chcl-glucose-w (5:2:5, N2), proline-malic acid-w (1:1:3, N3), glucose-fructose-sucrose-w (1:1:1:11, N4), 1,2-propanediol-chcl-w (1:1:1, N5), lactic acid-glucose-w (5:1:3, N6), glycerol-chcl-w (2:1:1, N7), and xylitol-chcl-w (1:2:3, N8). Rheological measurements of all NADESs confirmed their pseudoplastic behaviors. To improve the extraction processes, differential scanning calorimetry (DSC) allowed us to determine the maximum amount of water that could be added to the most stable NADES (N1, N2, N3, and N4; 17.5%, 20%, 10%, and 10% w/w, respectively) to lower their viscosities without disturbing their eutectic environments. The phytochemical compositions of NADES extracts were analyzed using high-performance thin-layer chromatography (HPTLC), and their free radical scavenging and α-amylase inhibitory properties were assessed using HPTLC-bioautography. N2, diluted with 20% of water, and N7 presented the best potential for replacing methanol for an eco-friendly extraction of flavonoids, radical scavengers, and α-amylase inhibitors from quinoa leaves. Their biological properties, combined with a good understanding of both thermal behavior and viscosity, make the obtained quinoa leaf NADES extracts good candidates for direct incorporation in nutraceutical formulations. Full article
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22 pages, 2249 KiB  
Article
Impedimetric DNA Sensor Based on a Composite of Electrochemically Reduced Graphene Oxide and Polyproflavine Electropolymerized from Natural Deep Eutectic Solvent for Anthracycline Medications Determination
by Anastasia Goida, Tatiana Krasnova, Rezeda Shamagsumova, Vladimir Evtugyn, Anatoly Saveliev and Anna Porfireva
Biosensors 2025, 15(6), 385; https://doi.org/10.3390/bios15060385 - 14 Jun 2025
Viewed by 1114
Abstract
A novel nanocomposite based on electrochemically reduced graphene oxide (ERGO) and electropolymerized polyproflavine (PPFL) was obtained within a “one-pot” synthesis from natural deep eutectic solvent (NADES). NADES consisted of citric acid, glucose, and water in a molar ratio of 1:1:6. The synthesis was [...] Read more.
A novel nanocomposite based on electrochemically reduced graphene oxide (ERGO) and electropolymerized polyproflavine (PPFL) was obtained within a “one-pot” synthesis from natural deep eutectic solvent (NADES). NADES consisted of citric acid, glucose, and water in a molar ratio of 1:1:6. The synthesis was carried out in potentiostatic mode by consequent potential application in cathodic and anodic areas. The composite was applied to develop the impedimetric DNA sensor for anthracycline determination. The sensor has provided linear range from 10 nM to 0.1 mM for doxorubicin, from 1 pM to 10 nM for epirubicin, and from 10 pM to 10 nM for idarubicin, with the limit of detection 3 nM, 1 pM, and 5 pM, respectively. The concentrations of doxorubicin below 10 nM did not have any other influence on epirubicin and idarubicin determination despite their molecular structure similarity. The sensor developed was used for the determination of anticancer medications, such as doxorubicin, epirubicin, and idarubicin, in their standard solutions, pharmaceuticals, artificial, and human urine samples. It is worth noting that the additions of mannitol and lactose, which are the stabilizers of the pharmaceuticals, exhibited an interfering effect on the sensor response. Full article
(This article belongs to the Special Issue Application of Nanocomposites for Biosensors)
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19 pages, 533 KiB  
Review
Extraction of Phenolic Compounds from Agro-Industrial By-Products Using Natural Deep Eutectic Solvents: A Review of Green and Advanced Techniques
by Fernanda de Sousa Bezerra and Maria Gabriela Bello Koblitz
Separations 2025, 12(6), 150; https://doi.org/10.3390/separations12060150 - 3 Jun 2025
Cited by 1 | Viewed by 838
Abstract
As sustainability gains prominence, the circular economy has encouraged the valorization of agri-food by-products, which are rich in phenolic compounds known for their antioxidant and anti-inflammatory properties. Conventional extraction methods commonly employ organic solvents, which contradict green chemistry principles. Natural deep eutectic solvents [...] Read more.
As sustainability gains prominence, the circular economy has encouraged the valorization of agri-food by-products, which are rich in phenolic compounds known for their antioxidant and anti-inflammatory properties. Conventional extraction methods commonly employ organic solvents, which contradict green chemistry principles. Natural deep eutectic solvents (NaDESs) have emerged as environmentally friendly alternatives for recovering bioactive compounds from food waste. This review investigated recent studies (2020–2024) on ultrasound (UAE), microwave (MAE), and pressurized liquid extraction (PLE) using NaDESs to extract phenolic compounds from agri-food by-products. A total of 116 publications were initially identified, of which 19 met the inclusion criteria. UAE combined with NaDESs proved effective, particularly for fruit and oilseed residues. MAE achieved good yields for phenolic acids and flavonoids but showed limitations on high temperatures. PLE, though less explored, demonstrated promising results when optimized for temperature, pressure, and NaDES composition. The combination of NaDESs with assisted extraction techniques enhanced yield, selectivity, and environmental performance compared to conventional approaches. These findings highlight a greener and more efficient strategy for phenolic recovery within a biorefinery framework. Ultimately, this approach contributes to the sustainable management and valorization of agri-food by-products, supporting circular economy principles and the development of cleaner extraction technologies for functional ingredients. Full article
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20 pages, 2180 KiB  
Article
Effective Liquid–Liquid Extraction for the Recovery of Grape Pomace Polyphenols from Natural Deep Eutectic Solvents (NaDES)
by Alessandro Frontini, Giulio Tarentini, Carmine Negro, Andrea Luvisi, Massimiliano Apollonio and Luigi De Bellis
Separations 2025, 12(6), 148; https://doi.org/10.3390/separations12060148 - 2 Jun 2025
Viewed by 632
Abstract
Natural deep eutectic solvents (NaDESs) are emerging solvents for their yield when used for extraction of different molecules, including polyphenols. NaDESs are a cutting-edge technology that offers numerous advantages, including cheap cost, safety, effectiveness and environmental friendliness. However, due to NaDES’ high boiling [...] Read more.
Natural deep eutectic solvents (NaDESs) are emerging solvents for their yield when used for extraction of different molecules, including polyphenols. NaDESs are a cutting-edge technology that offers numerous advantages, including cheap cost, safety, effectiveness and environmental friendliness. However, due to NaDES’ high boiling point, the recovery and separation of compounds after the extraction is the bottleneck of the process. In this work, two affordable methods were tested for the recovery of phenolic compounds from three binary NaDESs (composed of choline chloride mixed separately with lactic acid, tartaric acid or glycerol as hydrogen bond donors): the antisolvent and the liquid–liquid extraction methods. The former was assessed by diluting the extracts with different aliquots of water, employed as antisolvent, which was ineffective. For the liquid–liquid extraction method, ethyl acetate (EtOAc), acetonitrile (ACN), 2-chlorobutane (2-CB) and 2-methyltetrahydrofuran (2-MeTHF) were compared. Except for ACN, all solvents were perfectly immiscible with the three NaDESs, forming biphasic systems that were analyzed by colorimetric assays and HPLC/MS. 2-MeTHF applied on a 10-fold water dilution of the NaDES extract reached recovery percentages higher than 90% for most of the non-anthocyanin phenols and good recovery (up to 80%) for some anthocyanins. 2-MeTHF appears to be the first known solvent capable of extracting anthocyanins from NaDESs. Finally, a two-step liquid–liquid extraction performed firstly with EtOAc and subsequently with 2-MeTHF is proposed for the separation of different phenolic fractions. Full article
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20 pages, 1095 KiB  
Article
Sustainable Extraction of Prospective Cosmetic Ingredients from Colombian Marine Macroalgae Using Natural Deep Eutectic Solvents
by Verónica María Tamayo-Rincón, Jhonny Colorado-Ríos, Didier Johan Alvarez-Bustamante, Vanessa Urrea-Victoria, Diana Margarita Márquez-Fernández, Constain H. Salamanca, Stefano Dall’Acqua, Leonardo Castellanos-Hernandez and Alejandro Martínez-Martínez
Mar. Drugs 2025, 23(6), 239; https://doi.org/10.3390/md23060239 - 30 May 2025
Viewed by 663
Abstract
This study presents the results obtained from extracting and quantifying cosmetically valuable metabolites such as phenolic compounds and mycosporine-like amino acids (MAAs) from 12 samples of marine macroalgae collected in the Colombian Caribbean Sea. Natural deep eutectic solvents (NADESs) were prepared, physicochemically tested [...] Read more.
This study presents the results obtained from extracting and quantifying cosmetically valuable metabolites such as phenolic compounds and mycosporine-like amino acids (MAAs) from 12 samples of marine macroalgae collected in the Colombian Caribbean Sea. Natural deep eutectic solvents (NADESs) were prepared, physicochemically tested (viscosity, surface tension, pH, and conductivity), and then compared with water as the reference solvent to quantify phenolic compounds using the Folin–Ciocalteau test. With a simple extraction assay with water and ultrasound followed by ultraviolet spectral scanning the presence of MAAs was easily determined in several of the analysed samples, and then they were identified by HPLC-DAD. Hydrochloric acid solution at 5% extracted a higher content of phenolic compounds than NADES and water. The NADES that showed the highest phenolic compound extraction yield was a mixture of betaine, glucose, and water with 1:1:5 molar ratio. Sargassum cf. ramifolium and Sargassum fluitans showed the highest contents of phenolic compounds extracted with NADES, with 29.2 and 21.9 mg GAE/g DW, respectively. The results show that NADESs are an interesting alternative for the more efficient extraction of cosmetically valuable compounds such as phenolic compounds and mycosporine-type amino acids from marine macroalgae. Full article
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20 pages, 476 KiB  
Article
Combining Carboxylic-Acid-Based Deep Eutectic Solvents and High Temperatures Enhances Phenolic Acid Extraction from Grape Pomace
by Francesca Lorenzo, Marialaura Frisina, Sonia Bonacci, Monica Nardi, Manuela Oliverio and Antonio Procopio
Antioxidants 2025, 14(6), 643; https://doi.org/10.3390/antiox14060643 - 27 May 2025
Viewed by 496
Abstract
Phenolic acids are contained in grape pomace, mostly in a conjugate form, and can be a natural source of building blocks if they are efficiently hydrolyzed and extracted from the natural matrix. In this study, a comparative study based on the spectrophotometric evaluation [...] Read more.
Phenolic acids are contained in grape pomace, mostly in a conjugate form, and can be a natural source of building blocks if they are efficiently hydrolyzed and extracted from the natural matrix. In this study, a comparative study based on the spectrophotometric evaluation of total phenolic content, hydroxycinnamic acid content, and anthocyanin content was performed on different carboxylic-acid-based NADES with different heating sources. Moreover, a quali–quantitative characterization of the bioactive molecules extracted was performed using UHPLC-ESI-HRMS. We found that the nature of the acidic component of the DES was crucial in selecting the family of molecules to be extracted; ChCl/oxalic acid 1:1 NADES, when combined with MAE at 100 °C, is the best medium for the in situ hydrolysis and extraction of phenolic acids from grape pomace. The ORAC test performed on natural extracts with and without NADES revealed a role for NADES components in antioxidant activity against the ROS of extracted bioactive phenols. Full article
(This article belongs to the Section Natural and Synthetic Antioxidants)
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25 pages, 1620 KiB  
Article
Laccase-Catalyzed Polymerized Natural Bioactives for Enhanced Mushroom Tyrosinase Inhibition
by Diana Costa, Diana Rocha, Joana Santos, Jennifer Noro, Artur Ribeiro and Carla Silva
Catalysts 2025, 15(5), 481; https://doi.org/10.3390/catal15050481 - 14 May 2025
Viewed by 1338
Abstract
Skin hyperpigmentation disorders, such as melasma, are linked to excessive melanin production, primarily regulated by the enzyme tyrosinase (TYR). While current inhibitors like kojic acid (KA) are effective, they often cause adverse side effects, driving the search for safer andnatural alternatives. This study [...] Read more.
Skin hyperpigmentation disorders, such as melasma, are linked to excessive melanin production, primarily regulated by the enzyme tyrosinase (TYR). While current inhibitors like kojic acid (KA) are effective, they often cause adverse side effects, driving the search for safer andnatural alternatives. This study evaluated the TYR inhibitory potential of bioactive-rich extracts from acorn, cocoa, cork, and eucalyptus, extracted using hydroethanolic (HE) and natural deep eutectic solvents (NADES), and explored the enhancement of their bioactivity through laccase-assisted polymerization. NADES significantly improved extraction yields and preserved bioactive compounds, with cocoa extracts showing the highest TYR inhibition. Laccase-mediated polymerization further enhanced TYR inhibitory activity, particularly of NADES extracts, suggesting a more effective and sustainable approach for skincare applications. The results highlight the potential of combining green chemistry principles with enzymatic catalysis to develop eco-friendly and efficient treatments for hyperpigmentation disorders, offering a promising alternative to conventional methods. Full article
(This article belongs to the Special Issue The Design of Protein-Based Catalysts)
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26 pages, 4026 KiB  
Article
Enhanced Extraction of Bioactive Compounds from Red Grape Pomace: Optimizing Ultrasound-Assisted Extraction with Ethanol and NaDES as Solvents
by Nicoleta Balan, Silviu Măntăilă, Gabriela Râpeanu and Nicoleta Stănciuc
Antioxidants 2025, 14(5), 526; https://doi.org/10.3390/antiox14050526 - 27 Apr 2025
Viewed by 1066
Abstract
This study aims to investigate two types of solvents, ethanol and natural deep eutectic solvent (NaDES), using the ultrasound-assisted extraction techniques, in order to analyze their efficiency and ability to extract polyphenolic compounds from red grape pomace. The optimization and validation of the [...] Read more.
This study aims to investigate two types of solvents, ethanol and natural deep eutectic solvent (NaDES), using the ultrasound-assisted extraction techniques, in order to analyze their efficiency and ability to extract polyphenolic compounds from red grape pomace. The optimization and validation of the most feasible extraction conditions leading to maximization of the dependent variables (total anthocyanins, polyphenols, flavonoids and antioxidant activity), were carried out using response surface methodology with a central composite design. For ethanol extraction, the validated optimal conditions were at 35 °C for 22.5 min and a concentration of 70% ethanol. The values obtained under these conditions were 105.32 mg cyanindin-3-glucoside (C3G)/g DW, 465.81 mg gallic acid equivalents (GAE)/100 g DW, 15.3 mg catechin equivalents (CE)/100 g DW and 1414.15 mMol Trolox/g DW, respectively. Concerning the extraction using NaDES, consisting of a 1:2:1 molar mixture of choline chloride, lactic acid and water, the optimal conditions that led to a profile consisting in 57.58 mg C3G/g DW, 414.04 mg GAE/100 g DW, 15.8 mg CE/100 g DW and 7.28 mMol Trolox/g DW, respectively, were at 60 °C for 60 min and a solvent volume of 10 mL. Two different chromatographic profiles were obtained, with 12 polyphenolic compounds identified in ethanolic extracts and only 5 in NaDES, respectively. The in vitro digestion study revealed the high bioaccessibility of polyphenols in the gastric environment, with a drastic decrease in simulated intestinal fluid. The results are valuable in terms of identifying the best extraction conditions for polyphenols using alternative, non-toxic, ecofriendly solvents. Full article
(This article belongs to the Special Issue Green Extraction of Antioxidant from Natural Source)
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21 pages, 2769 KiB  
Article
Utilizing Natural Deep Eutectic Solvents (NADESs) for Sustainable Phytonutrient Recovery: Optimization and Multi-Matrix Extraction of Bioactive Compounds
by Ainur Makarova, Ceylin Özten and Bartłomiej Zieniuk
Appl. Sci. 2025, 15(9), 4843; https://doi.org/10.3390/app15094843 - 27 Apr 2025
Viewed by 665
Abstract
Bioactive phytochemicals, such as polyphenols, play vital roles in human health, but conventional extraction methods rely on hazardous solvents. This study establishes natural deep eutectic solvents (NADESs) as versatile and environmentally friendly alternatives for recovering a variety of bioactive compounds from plant materials. [...] Read more.
Bioactive phytochemicals, such as polyphenols, play vital roles in human health, but conventional extraction methods rely on hazardous solvents. This study establishes natural deep eutectic solvents (NADESs) as versatile and environmentally friendly alternatives for recovering a variety of bioactive compounds from plant materials. Five choline chloride-based NADESs were evaluated for their effectiveness in extracting betalains (from beetroot), carotenoids (from carrot and sweet potato), anthocyanins (from chokeberry pomace and red onion), and polyphenols (from Lonicera japonica flowers, hop cones, rowan berries, and spent coffee grounds). Notably, NADES2 outperformed water in betalain recovery (179.86 mg of betanin/100 g of beetroot), while NADES4 (choline chloride-urea, 1:2 molar ratio) matched the polyphenol extraction efficiency of ethanol. Using L. japonica flowers as a model for optimization, Response Surface Methodology (RSM) identified the solvent ratio and temperature as critical extraction parameters, using high ratios (12:1–15:1 v/w) and moderate heat (55–75 °C) to maximize recovery. NADES4 emerged as a high-performing solvent, achieving a total phenolic content (TPC) of 75.94 mg chlorogenic acid/g and antioxidant activity of 451.00 µmol Trolox/g under the following conditions: 60% aqueous dilution, 15:1 solvent ratio, and 80 °C, 30 min. These findings highlight NADESs as a green, tunable solvent system for phytochemical extraction across plant species, offering enhanced efficiency, reduced environmental impact, and alignment with sustainable practices. Full article
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