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A special issue of Processes (ISSN 2227-9717). This special issue belongs to the section "Separation Processes".

Deadline for manuscript submissions: 10 August 2026 | Viewed by 9234

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Dr. Iván Costa-Trigo

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Guest Editor

Unidade de Bioenergia e Biorrefinarias, LNEG—Laboratório Nacional de Energia e Geologia, Estrada do Paço do Lumiar, 22, 1649-038 Lisboa, Portugal
Interests: green and sustainable pretreatments; extraction of bioactive compounds; fermentative processes; high value-added compounds; catalytic conversion; enzymes production and application

Dr. Luís C. Duarte

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Guest Editor

Unidade de Bioenergia e Biorrefinarias, LNEG—Laboratório Nacional de Energia e Geologia, Estrada do Paço do Lumiar, 22, 1649-038 Lisboa, Portugal
Interests: oligosaccharides; biomass pretreatments; biofuels; phenolics; algae biorefinery; bioactive compounds
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Special Issue Information

Dear Colleagues,

Nowadays, the use of conventional solvents remains a concern due to their environmental damage and potential health risks to humans. In this regard, one of the Green Chemistry principles focuses on the search and development of green solvents, which exhibit interesting features such as low toxicity, biodegradability, low environmental impact, and/or recyclability. Therefore, it is crucial to promote investigations that address sustainable processes for extracting and separating pivotal molecules using green solvents (deep eutectic solvents, ionic liquids, supercritical solvents, low- and high-pressure solvents). All these technologies provide us with knowledge about how they can be efficiently implemented in a biorefinery, offering great value to society in terms of sustainability and the production of safe products.

This Special Issue on “Advances in Green Extraction and Separation Processes” will encompass novel articles or reviews that are in concordance with Green Chemistry principles and commitment to the sustainable processes aims to extract and separate value-added molecules.

Topics include, but are not limited to:

Novel design and implementation of DES mixtures and ionic liquids
Supercritical CO₂ technology
Subcritical water, pressure hot water, steam explosion, or organosolv.
Adsorption–desorption processes
Membranes technologies
Advances in enzyme formulation and application

Thank you, and I hope you will consider participating in this Special Issue.

Sincerely,

Dr. Iván Costa-Trigo
Dr. Luís C. Duarte
Guest Editors

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 250 words) can be sent to the Editorial Office for assessment.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Processes is an international peer-reviewed open access semimonthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2400 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

deep eutectic solvents/ionic liquids
enzymatic conversion
bioactive compounds extraction
supercritical extraction
membranes
adsorption–desorption processes
waste streams valorization

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Published Papers (10 papers)

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Research

26 pages, 1754 KB

Open AccessArticle

Sustainable Valorization of Spent Coffee Grounds: Phenolic Compound Extraction Using Hydrophobic Eutectic Solvents

by Cristiane Nunes da Silva, Talita Rego Prado, Filipe Smith Buarque and Bernardo Dias Ribeiro

Processes 2026, 14(7), 1109; https://doi.org/10.3390/pr14071109 - 30 Mar 2026

Viewed by 519

Abstract

Spent coffee grounds (SCG) are the main by-product generated by the coffee industry, with an estimated annual production of approximately 7 million tons. Although commonly treated as waste, SCG constitute a valuable source of phenolic compounds, particularly chlorogenic acid, which has been associated with antimicrobial, antioxidant, antimutagenic, anti-inflammatory, and cardioprotective properties. These bioactive compounds are of interest as functional ingredients for food, cosmetic, and pharmaceutical applications. However, their recovery by conventional extraction methods often depends on volatile, flammable, or toxic organic solvents. In this context, hydrophobic eutectic solvents (HES) have emerged as a greener and more sustainable alternative. In the present study, phenolic compounds were extracted from SCG using HES combined with microwave-assisted extraction (MAE). Sixteen terpene-based HES formulated with fatty acids and fatty alcohols were evaluated. Among them, camphor:dodecanoic acid and borneol:dodecanoic acid gave the highest total phenolic contents. Process optimization showed that the borneol:dodecanoic acid system, under 12% water content, a 1:10 solid-to-liquid ratio, 57 °C, and 120 min, reached 80.94 ± 4.44 mg GAE g⁻¹ by MAE. HPLC analysis revealed chlorogenic, caffeic, and ferulic acids as the main phenolic compounds, while the extracts also displayed high antioxidant activity. Overall, these findings demonstrate that HES-MAE is a promising and sustainable strategy for the recovery of value-added phenolics from SCG. Full article

(This article belongs to the Special Issue Advances in Green Extraction and Separation Processes)

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19 pages, 1243 KB

Open AccessArticle

Sustainable Bacterial Cellulose Production from Avocado Seed Waste Using a Green Biorefinery Approach

by Gabriela Barraza-Jáuregui, Yolanda Luciana Abanto Sánchez, Angie Rojas, José Carlos Alcántara, Daniel Antonio Medina Bocanegra, Hernán Alvarado-Quintana, Alberto Flores-Pérez, Fernando Javier Hurtado Butrón, Carlos Sopán-Benaute, María Guadalupe Morán-Aguilar and Fabiola Vilaseca

Processes 2026, 14(3), 543; https://doi.org/10.3390/pr14030543 - 4 Feb 2026

Cited by 2 | Viewed by 788

Abstract

In this study, avocado seed (AS) waste was used as a feedstock for bacterial cellulose (BC) production. Global avocado consumption continues to rise due to its recognised health benefits, resulting in substantial amounts of waste generated by the avocado processing industry. This work proposes the efficient utilisation of avocado seed residues—rich in fermentable sugars—to enhance the economic viability of BC production while supporting responsible agro-industrial waste management. Hydrolysed avocado seeds were incorporated into a modified Hestrin–Schramm (MHS) medium for BC production using Komagataeibacter xylinus as the bacterial strain. The BC membranes obtained from the modified medium (BC-MHS) exhibited higher production (1.93 g/L) and productivity (0.19 g/L·day) compared with those produced in the standard HS medium (BC-HS). The morphology and nanofibre diameter (11–85 nm) of the resulting BC were not significantly affected; however, BC-MHS showed higher crystallinity (~78%) and a higher degradation temperature (~357 °C) than BC-HS. Conversely, the modified medium slightly reduced the mechanical performance of the BC in terms of elongation at break, tensile strength, and Young’s modulus. Overall, avocado seed waste was successfully transformed into a value-added material, demonstrating its potential for agro-industrial waste valorisation through scalable and sustainable biorefinery processes. Full article

(This article belongs to the Special Issue Advances in Green Extraction and Separation Processes)

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20 pages, 4309 KB

Open AccessArticle

Characterization and Optimization of the Ultrasound-Assisted Extraction Process of an Unexplored Amazonian Drupe (Chondrodendron tomentosum): A Novel Source of Anthocyanins and Phenolic Compounds

by Disbexy Huaman-Huaman, Segundo G. Chavez, Laydy Mena-Chacon, José Marcelo-Peña, Hans Minchán-Velayarce and Ralph Rivera-Botonares

Processes 2026, 14(2), 357; https://doi.org/10.3390/pr14020357 - 20 Jan 2026

Viewed by 613

Abstract

This study presents the first comprehensive physicochemical and bioactive characterization of the fruit of Chondrodendron tomentosum Ruiz & Pav. (Menispermaceae). Biometric and physicochemical parameters were characterized across three fruit ripening stages (green, turning, ripe). Additionally, proximate composition was determined in ripe fruits, and methanol concentration (25–75%), ultrasonic amplitude (30–70%), and time (1–15 min) were optimized using response surface methodology with a Box–Behnken design. During ripening, weight increased by +47.7% (3.89 to 5.74 g; p < 0.0001), TSS by +26.1% (7.00 to 8.83 °Brix), pH decreased by 32.0% (6.28 to 4.27), and acidity increased by 276% (0.25 to 0.94%). The quadratic models demonstrated high predictive accuracy (R² > 96.5%; p < 0.004). Optimal conditions (57% methanol, 70% amplitude, and 15 min) maximized total anthocyanin content (120.71 ± 1.89 mg cyanidin-3-glucoside/L), total phenols (672.46 ± 5.84 mg GAE/100 g), and DPPH radical scavenging capacity (5857.55 ± 60.20 µmol Trolox/100 g) in ripe fruits. Unripe fruits do not contain anthocyanins, reaching 46.01 mg C3G/L in turning fruits and 120.71 mg/L in ripe fruits (162% higher than turning fruits). Principal component analysis (90.6% variance) revealed synchronized co-accumulation of anthocyanins and phenols, enhanced by vacuolar acidification. These results suggest ripe C. tomentosum fruits as a potential source for natural colorants, nutraceuticals, and functional foods, pending prior development of green, human-safe extraction processes. Full article

(This article belongs to the Special Issue Advances in Green Extraction and Separation Processes)

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21 pages, 19614 KB

Open AccessArticle

Hydrothermal–Membrane Valorization of Coffee Pulp for Xylooligosaccharide Production

by James Villar, Iris Paola Roncal Huaman, Delicia L. Bazán, Ruly Teran Hilares and Rita de Cássia Lacerda Brambilla Rodrigues

Processes 2026, 14(1), 153; https://doi.org/10.3390/pr14010153 - 2 Jan 2026

Viewed by 1023

Abstract

Wet coffee pulp residues (WCPRs) are typically underutilized, and their accumulation increases alongside coffee production, generating significant environmental impacts. This study proposes a sustainable valorization approach through hydrothermal treatment followed by membrane filtration for the production of xylooligosaccharides (XOSs). Extractive-free WCPR contained 35.4% structural carbohydrates (20.4% cellulose and 15.0% hemicellulose) and 27.0% lignin. Hydrothermal treatments (180 °C, 3 °C min⁻¹, 15–60 min) were performed with and without citric acid as an organic catalyst. The acid-assisted treatment (T4) enhanced hemicellulose depolymerization and xylose release (16 g·kg⁻¹ dry biomass), whereas milder, non-acidic conditions (T3) promoted the selective formation and recovery of short-chain XOS, reaching cumulative biomass-normalized yields of up to 14 g·kg⁻¹ of xylobiose (X2) and 9 g·kg⁻¹ of xylotriose (X3). Subsequent membrane processing (UF–DF–NF) enabled progressive purification and enrichment of XOS fractions. Diafiltration was identified as the main step governing XOS enrichment, whereas nanofiltration primarily refined separation by directing monomeric sugars to the permeate rather than substantially increasing XOS yields. Additionally, Multiple Factor Analysis (MFA) integrated process and compositional variables, explaining 79.6% of the total variance. Dimension 1 represented process intensity and xylose transport, while Dimension 2 reflected molecular-weight-driven XOS fractionation. The acid-assisted process (T4) exhibited a distinct multivariate signature, characterized by enhanced carbohydrate mobilization and improved XOS recovery with reduced dependence on dilution. Overall, coupling hydrothermal pretreatment with membrane fractionation proved to be an efficient, and environmentally friendly strategy for coffee by-product valorization, consistent with hemicellulose-first biorefinery models and the principles of the circular bioeconomy. Full article

(This article belongs to the Special Issue Advances in Green Extraction and Separation Processes)

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17 pages, 1227 KB

Open AccessFeature PaperEditor’s ChoiceArticle

Enhancing the Biorefinery of Chestnut Burrs, Part II: Influence of Pretreatment with Choline Chloride–Urea-Diluted Deep Eutectic Solvent on Enzymatic Hydrolysis

by Iván Costa-Trigo, María Guadalupe Morán-Aguilar, Nelson Pérez Guerra, Ricardo Pinheiro de Souza Oliveira and José Manuel Domínguez

Processes 2025, 13(12), 4090; https://doi.org/10.3390/pr13124090 - 18 Dec 2025

Viewed by 854

Abstract

Agro-industrial chestnut waste derived from chestnut processing is usually discharged without further use. However, these residues are attractive due to their high-value composition, rich in sugars and lignin. Among these residues, chestnut burrs (CB) represent a promising feedstock for biorefinery applications aimed at maximizing the valorization of their main constituents. In this study, we propose an environmentally friendly approach based on deep eutectic solvents (DES) formed by choline chloride and urea (ChCl/U) (1:2, mol/mol) for the selective deconstruction of lignocellulosic architecture, followed by enzymatic hydrolysis to release second-generation (2G) fermentable sugars. Pretreatments were applied to raw CB, washed CB (W-CB), and the obtained solid fraction after prehydrolysis (PreH). Structural and morphological modifications, as well as crystallinity induced by DES pretreatment, were characterized using attenuated total reflectance Fourier-transform infrared spectroscopy (ATR-FTIR), field emission scanning electron microscopy (FE-SEM), and X-ray diffraction (XRD). Remarkable results in terms of effectiveness and environmental friendliness on saccharification yields were achieved for PreH subjected to DES treatment for 8 h, reaching approximately 60% glucan and 74% xylan conversion under the lower enzyme loading (23 FPU/g) and liquid-to-solid ratio (LSR) of 20:1 studied. This performance significantly reduces DES pretreatment time from 16 h to 8 h at mild conditions (100 °C), lowers the LSR for enzymatic hydrolysis from 30:1 to 20:1, and decreases enzyme loading from 63.5 FPU/g to 23 FPU/g, therefore improving process efficiency and sustainability. Full article

(This article belongs to the Special Issue Advances in Green Extraction and Separation Processes)

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18 pages, 1872 KB

Open AccessArticle

Kinetics and Thermodynamics of Ultrasound-Assisted Extraction of Taxanes from Taxus chinensis by Natural Deep Eutectic Solvents

by Ying Guo, Wenna Song, Lingyu Hu, Runbo Liu, Izni Atikah Abd Hamid and Jiaxin Quan

Processes 2025, 13(12), 4074; https://doi.org/10.3390/pr13124074 - 17 Dec 2025

Cited by 4 | Viewed by 795

Abstract

This study aimed to enhance the extraction efficiency and elucidate the mechanism of ultrasound-assisted extraction (UAE) of taxanes from Taxus chinensis by natural deep eutectic solvents (NADES). The processes of kinetics and thermodynamics were systematically investigated. These extractions adhered to a pseudo-second-order kinetic model (R² > 0.972), with intraparticle diffusion identified as the dominant mechanism. Key parameters such as temperature, ultrasonic power, and solid/liquid ratio significantly improved the effective diffusion coefficient (D_e) and mass transfer coefficient (K_T), reaching values of 6.21 × 10⁻⁹ m²/s and 4.14 × 10⁻³ m/s, respectively. A high Biot number (B_i > 59.21) confirmed that internal diffusion is the rate-determining step. Thermodynamic analysis indicated that the process is endothermic (ΔH > 0), irreversible (ΔS > 0), and spontaneous (ΔG < 0). These results elucidate the underlying mechanisms of UAE and establish a foundational framework for its industrial-scale implementation. Full article

(This article belongs to the Special Issue Advances in Green Extraction and Separation Processes)

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18 pages, 5592 KB

Open AccessFeature PaperEditor’s ChoiceArticle

Development and Optimization of Green Extraction Process of Greek Mountain Tea (Sideritis scardica)

by Maria-Anna Karadendrou, Anna Karantoni, Ioanna Pitterou, Kyriaki Safari, Georgios Stavropoulos, Andromachi Tzani and Anastasia Detsi

Processes 2025, 13(12), 3945; https://doi.org/10.3390/pr13123945 - 6 Dec 2025

Viewed by 1016

Abstract

Medicinal and aromatic plants continue to attract attention as rich sources of natural bioactive compounds with potential health benefits. Among them, Greek mountain tea (Sideritis scardica) is widely recognized for its high content of phytochemicals, which have been associated with various biological activities. In this study, Natural Deep Eutectic Solvents (NADESs) were investigated as a sustainable and efficient alternative to conventional solvents for the extraction of such compounds, aiming to the development of a more efficient extraction process. Six task-specific designed NADESs were prepared and evaluated for their extraction efficiency, based on the Total Phenolic Content (TPC) and Total Flavonoid Content (TFC) of the extract. The most promising NADES, comprising betaine and 1,3-propandeiol, was selected for process optimization using a Box–Behnken design and key extraction parameters were systematically examined to maximize TPC and TFC. The extract obtained under the proposed conditions (S/L = 20 mg/g, 240 min, 40% water as cosolvent) exhibited a TPC and TFC value of 49.2 mg_GAE/g and 45.9 mg_CAE/g, respectively, approximately two times higher than the values of a hydroethanolic extract, obtained under the same conditions (TPC = 26.6 mg_GAE/g, TF = 19.9 mg_CAE/g). The optimum extract was further analyzed using HPLC-DAD to determine its phytochemical profile and was compared with the conventional hydroethanolic extract, revealing the role of the selected media on the extracted compounds. Full article

(This article belongs to the Special Issue Advances in Green Extraction and Separation Processes)

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14 pages, 625 KB

Open AccessArticle

Ultrasound-Assisted Extraction to Recover Antioxidant Compounds: A Comparative Analysis of Green Solvents for the Sustainable Valorization of Olive Leaves

by Nils Leander Huamán-Castilla, Salome Mamani-Pari, Dayana Ramos Allcca, María Fernanda Quispe Angulo, Gregorio Arroyo and Nilton Cesar León-Calvo

Processes 2025, 13(12), 3856; https://doi.org/10.3390/pr13123856 - 28 Nov 2025

Viewed by 819

Abstract

The olive industry produces large quantities of olive leaves, an agro-industrial byproduct without commercial value and with significant environmental disposal challenges. However, olive leaves are a rich source of antioxidant compounds known for their diverse biological properties. This highlights the need for green processes that utilize environmentally friendly solvents. Thus, this research aimed to evaluate the effectiveness of two different solvents: ethanol (at concentrations of 0%, 15%, and 30%) and glycerol (also at 0%, 15%, and 30%), combined with moderate temperatures (50 °C and 70 °C) using ultrasound-assisted extraction (20 kHz and 60% amplitude for 30 min) to recover antioxidant compounds from olive leaves. Our results showed that 30% glycerol at 70 °C was more effective at recovering polyphenols (14.85 ± 0.09 mg GAE g⁻¹ dw) compared to ethanol (12.26 ± 0.13 mg GAE g⁻¹ dw) under the same conditions. Additionally, the antioxidant capacity, measured using DPPH and ORAC assays, yielded higher results with 30% glycerol, showing values of 2.65 ± 0.16 mg mL⁻¹ and 684.65 ± 20.79 µmol TE g⁻¹ dw, respectively. The polyphenol profile quantified different families of polyphenols like phenolic acids, flavanols, flavonols, stilbenes, and secoiridoids. However, oleuropein, a secoiridoid, was the most predominant polyphenol found in the extracts (1122.52 ± 33.72 μg g⁻¹ dw). Interestingly, the use of 30% ethanol at 70 °C reduced the glucose and fructose content by 48% and 84%, respectively. Therefore, glycerol emerges as an efficient green solvent for the extraction of antioxidant compounds. These findings support the valorization of this agricultural residue by recovering its valuable components, contributing to food sustainability and a circular economy. Full article

(This article belongs to the Special Issue Advances in Green Extraction and Separation Processes)

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18 pages, 1011 KB

Open AccessFeature PaperEditor’s ChoiceArticle

Optimization of Green Extraction of Antioxidant Compounds from Blackthorn Pomace (Prunus spinosa L.) Using Natural Deep Eutectic Solvents (NADES)

by Sara Hourani, Jelena Vukosavljević, Nemanja Teslić, Ružica Ždero Pavlović, Boris M. Popović and Branimir Pavlić

Processes 2025, 13(11), 3737; https://doi.org/10.3390/pr13113737 - 19 Nov 2025

Cited by 3 | Viewed by 1152

Abstract

Blackthorn (Prunus spinosa L.) is a wild, understudied plant rich in bioactive compounds such as polyphenols with designated antioxidant potential. The main objective of this research was to optimize ultrasound-assisted extraction of blackthorn pomace using natural deep eutectic solvents (NADES). To obtain the highest yield of polyphenols and improved in vitro antioxidant activity, response surface methodology (RSM) and central composite experimental design were used. The screening step of the study included ten different NADESs using a one-factor-at-a-time approach. Two NADES mixtures (N12, containing proline and lactic acid in a molar ratio of 1:2, and N14, containing choline chloride and glycerol in a molar ratio of 1:1) were chosen for the second step of the study, which aimed to select the most influential process parameters. A fractional factorial 2⁵⁻¹ design was used, varying five different parameters at two levels: extraction time (30 and 60 min), extraction temperature (40 and 50 °C), and liquid-to-solid ratio (10 and 20 mL/g), water content in NADES (15 and 20%), and NADES type (N12 and N14). After the second step, N12 containing 20% water was chosen as the most potent solvent for the optimization study. For the final step, the other three parameters were varied on three levels, and thus optimal conditions were obtained (extraction time 90 min, extraction temperature 65 °C, and liquid-to-solid ratio 22.65 mL/g). Blackthorn juice was also tested in the first step, as well as under optimal conditions established for pomace, in order to evaluate whether these conditions are suitable for juice and to determine the percentage of improvement in extraction efficiency. Full article

(This article belongs to the Special Issue Advances in Green Extraction and Separation Processes)

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13 pages, 766 KB

Open AccessFeature PaperEditor’s ChoiceArticle

Sunflower Seed Oil Enriched with Phenolic Compounds from Barbatimão Bark

by Janiani de Oliveira Cavitioli, Izabelle Alves de Castro França, Djéssica Tatiane Raspe, Natália Stevanato, Vitor Augusto dos Santos Garcia, Beatriz Cervejeira Bolanho Barros and Camila da Silva

Processes 2025, 13(11), 3534; https://doi.org/10.3390/pr13113534 - 4 Nov 2025

Cited by 1 | Viewed by 935

Abstract

This study aimed to use sunflower seeds (SSs) and barbatimão bark (BB) to obtain an oil enriched with phenolic compounds. For this purpose, simultaneous extractions were carried out using different proportions of SSs and BB. Subsequently, the effects of temperature and extraction time were determined. The resulting oils were evaluated for composition and physicochemical properties. BB addition decreased the mass yield by 27% to 56% but increased the total phenolic content by 5 to 13 times. The best SS/BB ratio (3:2.5) was selected for further experiments. Increasing the extraction temperature from 30 to 60 °C and the extraction time from 15 to 60 min led to a 10% increase in oil yield and enhanced the contents of phenolic acids and flavonoids by 1.1 to 10 times. Gallic, quinic, and trans-cinnamic acids were the main phenolics in enriched oils, which exhibited higher antioxidant activity via the DPPH^•, FRAP, and ABTS^•+ methods. Linoleic and oleic acids were identified as the major fatty acids in the tested oils. Enriched oils showed greater thermal stability than their unenriched counterpart. The application of phenolic-enriched oil at concentrations of up to 400 µg/mL did not exert cytotoxic effects on human keratinocyte HaCaT cells. Full article

(This article belongs to the Special Issue Advances in Green Extraction and Separation Processes)

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