Search Results (90)

Furfural is a fascinating bio-based platform molecule that can be converted into useful cyclic compounds, among others. In this work, the hydrogenative rearrangement-dehydration of furfural towards cyclopentanone using a commercially available Pt/C catalyst was investigated in terms of its reaction performance to assess its feasibility as an industrial process. However, acquiring an acceptable cyclopentanone yield proved very difficult, and the reaction was constrained by unforeseen parameters, such as the relative liquid volume in the reactor and the substrate concentration. Most strikingly, the sacrificial formation of furanoic oligomers that precipitated onto the catalyst’s surface was a troublesome key factor that mediated the product’s selectivity versus the carbon mass balance. By applying a biphasic water–toluene solvent system, the yield of cyclopentanone was somewhat improved to a middling 59%, while tentatively positive distributions of reaction components over these solvent phases were observed, which could be advantageous for anticipated down-stream processing. Overall, the sheer difficulty of controlling this one-pot cascade transformation towards a satisfactory product output under rather unfavorable reaction parameters renders it unsuitable for industrial process development, and a multi-step procedure for this chemical transformation might be considered instead. Full article

Background: This study developed and characterized a novel drug delivery system (DDS) for potential use in oral surgery, combining poly(lactic-co-glycolic acid) (PLGA) microspheres loaded with chlorhexidine (MS-CHX) and a polyethylene glycol (PEG)-based hydrogel containing dexketoprofen (HG-DXT). Methods: MS-CHX was synthesized using a double emulsion evaporation method, while HG-DXT was formulated from a PEG blend. The components were combined in a 2:1 ratio to create the MS-CHX/HG-DXT DDS. Characterization techniques included differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and energy-dispersive X-ray spectroscopy (EDS). Antibacterial activity was evaluated using disk diffusion assays against E. faecalis, E. coli, S. aureus, and C. albicans. Biocompatibility was assessed with MTS, and drug release was measured via high-performance liquid chromatography (HPLC) in vitro. Results: CHX-loaded microspheres showed spherical morphology, stability above 37 °C, and antimicrobial efficacy. HG-DXT demonstrated good biocompatibility (80% of cell viability) and stable physicochemical properties (stability at 50-day storage). The DDS exhibited a biphasic release: an initial burst of dexketoprofen for analgesia, followed by sustained release of chlorhexidine for antimicrobial protection. Conclusions: This novel dual-action DDS showed promising characteristics and a favorable release profile, supporting its potential as a therapeutic alternative for post-operative pain and infection control in oral surgical procedures. Full article

The increasing demand for lithium-ion batteries (LIBs) and their limited lifespan emphasize the urgent need for sustainable recycling strategies. This study investigates the application of tetrabutylphosphonium-based ionic liquids (ILs) as alternative leaching agents for recovering critical metals, Li(I), Co(II), Ni(II), and Mn(II), from spent NMC cathode materials. Initial screening experiments evaluated the leaching efficiencies of nine tetrabutylphosphonium-based ILs for Co(II), Ni(II), Mn(II), and Li(I), revealing distinct metal dissolution behaviors. Three ILs containing HSO₄⁻, EDTA²⁻, and DTPA³⁻ anions exhibited the highest leaching performance and were selected for further optimization. Key leaching parameters, including IL and acid concentrations, temperature, time, and solid-to-liquid ratio, were systematically adjusted, achieving leaching efficiencies exceeding 90%. Among the tested systems, [TBP][HSO₄] enabled near-complete metal dissolution (~100%) even at room temperature. Furthermore, an aqueous biphasic system (ABS) was investigated utilizing [TBP][HSO₄] in combination with ammonium sulfate, enabling the complete extraction of all metals into the salt-rich phase while leaving the IL phase metal-free and potentially suitable for reuse, indicating the feasibility of integrating leaching and extraction into a continuous, interconnected process. This approach represents a promising step forward in LIB recycling, highlighting the potential for sustainable and efficient integration of leaching and extraction within established hydrometallurgical frameworks. Full article

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

Gels are semi-solid colloidal systems characterized by three-dimensional networks capable of retaining up to 99% of liquid while exhibiting both solid-like and liquid-like properties. A novel biphasic system, the bigel, consists of hydrogel and oleogel, enabling the encapsulation of hydrophilic and lipophilic compounds. Their structure and functionality are influenced by the distribution of gel phases (e.g., oleogel-in-hydrogel or hydrogel-in-oleogel). This study aims to review current trends in polysaccharide-based bigels derived from seeds, vegetable oils and waxes, highlighting their biocompatibility, sustainability and potential food applications. A bibliometric analysis of 157 documents using VOSviewer identified four key thematic clusters: structured materials, delivery systems, pharmaceutical applications, and physicochemical characterization. Principal component analysis revealed strong correlations between terms, while also highlighting emerging areas such as 3D printing. This analysis demonstrated that seed-derived polysaccharides, including chia seed mucilage and guar gum, improve bigel structure and rheological properties, offering sustainable plant-based alternatives. Additionally, innovations such as extrusion-based 3D printing, functional food design, controlled drug release, bioactive compound delivery, and fat replacement are helping to support the further development of these systems. Finally, bibliometric tools remain instrumental in identifying research gaps and guiding future directions in this field. Full article

Electrospray mass spectrometry off-line profiling monitored the recovery of targeted indole alkaloids from a fortified crude extract of Catharanthus roseus (790 mg) using semi-preparative high-performance countercurrent chromatography (HPCCC) fractionation. Visualization of selected single-ion traces projected the HPCCC molecular weight elution profile. Experimental partition-ratio values K_D and peak widths for detected metabolites were determined. Structural characterization of metabolites and co-elution effects were monitored in the scan range m/z 100–2000. In this study, the biphasic solvent system containing n-hexane–n-butanol–water with 0.5% ion-pair reagent trifluoro-acetic acid [1:1:2, v/v/v] was used based on partition ratio K_D-value liquid chromatography–electrospray ionization–mass spectrometry (LC-ESI-MS) analysis prediction. The monitoring of target ions resulted in the isolation of six major concentrated indole alkaloids (akuammicine, catharanthine, perivine, vindoline, vindorosine, and 19R-vindolinine), which were fully elucidated by 1D and 2D nuclear magnetic resonance (NMR) spectroscopy. Full article

In this study, an efficient and eco-friendly method was developed for continuous liquid–liquid extraction of lutein from microalgae Chlorella vulgaris. By employing a limonene-based biphasic liquid system, high-purity lutein was successfully obtained from the crude extract in a single run via centrifugal partition chromatography (CPC). Evaluation and optimization results demonstrated that limonene could effectively serve as a replacement for n-hexane as the solvent system for lutein extraction, exhibiting natural renewability and minimal environmental impact. Furthermore, the elution–extrusion operation mode was employed to fully exploit the liquid nature of the stationary phase in the extraction process, allowing for continuous sampling and separation without interruption. This proposed protocol offers a sustainable and environmentally friendly alternative for extracting valuable ingredients from microalgae biomass, demonstrating its potential as a scalable solution for producing lutein-enriched ingredients applicable to functional foods and nutraceuticals. Full article

Polyphenylene sulfide (PPS)-based separators have garnered significant attention as high-performance components for next-generation lithium-ion batteries (LIBs), driven by their exceptional thermal stability (>260 °C), chemical inertness, and mechanical durability. This review comprehensively examines advances in PPS separator design, focusing on two structurally distinct categories: porous separators engineered via wet-chemical methods (e.g., melt-blown spinning, electrospinning, thermally induced phase separation) and nonporous solid-state separators fabricated through solvent-free dry-film processes. Porous variants, typified by submicron pore architectures (<1 μm), enable electrolyte-mediated ion transport with ionic conductivities up to >1 mS·cm⁻¹ at >55% porosity, while their nonporous counterparts leverage crystalline sulfur-atom alignment and trace electrolyte infiltration to establish solid–liquid biphasic conduction pathways, achieving ion transference numbers >0.8 and homogenized lithium flux. Dry-processed solid-state PPS separators demonstrate unparalleled thermal dimensional stability (<2% shrinkage at 280 °C) and mitigate dendrite propagation through uniform electric field distribution, as evidenced by COMSOL simulations showing stable Li deposition under Cu particle contamination. Despite these advancements, challenges persist in reconciling thickness constraints (<25 μm) with mechanical robustness, scaling solvent-free manufacturing, and reducing costs. Innovations in ultra-thin formats (<20 μm) with self-healing polymer networks, coupled with compatibility extensions to sodium/zinc-ion systems, are identified as critical pathways for advancing PPS separators. By addressing these challenges, PPS-based architectures hold transformative potential for enabling high-energy-density (>500 Wh·kg⁻¹), intrinsically safe energy storage systems, particularly in applications demanding extreme operational reliability such as electric vehicles and grid-scale storage. Full article

Beauveria bassiana PfBb is a new strain with high host specificity to the target pest Phauda flammans. We conducted a series of experiments to optimize the biphasic fermentation system of B. bassiana PfBb by screening the medium compositions and fermentation environmental conditions in both liquid and solid fermentations. In the liquid fermentation, glucose and yeast extract with a C:N ratio of 17:1 were the optimal carbon and nitrogen sources, respectively, for B. bassiana PfBb mycelium growth and blastospore production, and liquid fermentation with an inoculation concentration of 1 × 10⁸/mL and an inoculum content of 50 mL conidial suspension, at 180 rpm/min rotation speed, pH 7 and 26 °C, favored mycelium growth. However, additional trace elements did not significantly improve liquid fermentation. In the solid fermentation, wheat bran and chaff at a ratio of 8:2 were identified as the best substrates that facilitated B. bassiana PfBb sporulation and conidial germination, and optimal substrates with 20% inoculum content, 50% water content, and 3-day fermentation in darkness had the highest conidia yield. The resulting conidia, stored at −20, 4, and 20 °C for one year, did not significantly change the water content, and with prolonged storage duration, conidial germination was significantly higher at −20 and 4 °C. Moreover, conidia stored at 4 °C for one year maintained its validity and virulence, which were toxic to all instar larvae of P. flammans. Our results provide essential support for the commercial production of B. bassiana PfBb-based biopesticides. Full article

The chemical industry faces major challenges despite recent progress in the transition to more environmentally friendly processes. Sustainable industrial chemistry relies on the optimization of protocols and downstream processes such as extraction, purification, and drying. Process intensification, which includes non-conventional techniques and continuous manufacturing, has emerged as a key strategy to improve efficiency and environmental impact. Technologies such as ultrasound, microwaves, mechanochemistry, and reactive extrusion offer improved performance but face scalability and proprietary barriers. Flow chemistry offers additional benefits, including smaller reactors, lower energy consumption (from 40 to 90%), and increased safety through continuous, automated reactions. However, implementing these methods requires overcoming engineering, economic, and regulatory hurdles. Biphasic catalysis and sonochemical activation in liquid–liquid systems are promising approaches for scalable reactions under mild conditions. The pharmaceutical industry, a major source of waste, has shown resistance due to high validation costs and complex regulations. Fortunately, international regulatory institutions have introduced programs to facilitate the introduction of advanced technologies. Future perspectives emphasize the integration of modular, intensified processes with digitalization and smart manufacturing. Collaborative, transdisciplinary research will be crucial for accelerating commercialization and addressing sustainability challenges in chemical production. Full article

Nanoemulsions (NEs) are submicron-sized heterogeneous biphasic liquid systems stabilized by surfactants. They are physically transparent or translucent, optically isotropic, and kinetically stable, with droplet sizes ranging from 20 to 500 nm. Their unique properties, such as high surface area, small droplet size, enhanced bioavailability, excellent physical stability, and rapid digestibility, make them ideal for encapsulating various active substances. This review focuses on recent advancements, future prospects, and challenges in the field of NEs, particularly in oral, parenteral, and ophthalmic delivery. It also discusses recent clinical trials and patents. Different types of in vitro and in vivo NE characterization techniques are summarized. High-energy and low-energy preparation methods are briefly described with diagrams. Formulation considerations and commonly used excipients for oral, ocular, and ophthalmic drug delivery are presented. The review emphasizes the need for new functional excipients to improve the permeation of large molecular weight unstable proteins, oligonucleotides, and hydrophilic drugs to advance drug delivery rapidly. Full article

This work unfolds functionalized ABSs composed of FILs ([C₂C₁Im][C₄F₉SO₃] and [${\mathrm{N}}_{1112\left(\mathrm{OH}\right)}$][C₄F₉SO₃]), mere fluoro-containing ILs ([C₂C₁Im][CF₃SO₃] and [C₄C₁Im][CF₃SO₃]), known globular protein stabilizers (sucrose and [${\mathrm{N}}_{1112\left(\mathrm{OH}\right)}$][C₄F₉SO₃]), low-molecular-weight carbohydrate (glucose), and even high-charge density salt (K₃PO₄). The ternary phase diagrams were determined, stressing that FILs highly increased the ability for ABS formation. The functionalized ABSs (FILs vs. mere fluoro-containing ILs) were used to extract lysozyme (Lys). The ABSs’ biphasic regions were screened in terms of protein biocompatibility, analyzing the impact of ABS phase-forming components in Lys by UV-VIS spectrophotometry, CD spectroscopy, fluorescence spectroscopy, DSC, and enzyme assay. Lys partition behavior was characterized in terms of extraction efficiency (% EE). The structure, stability, and function of Lys were maintained or improved throughout the extraction step, as evaluated by CD spectroscopy, DSC, enzyme assay, and SDS-PAGE. Overall, FIL-based ABSs are more versatile and amenable to being tuned by the adequate choice of the phase-forming components and selecting the enriched phase. Binding studies between Lys and ABS phase-forming components were attained by MST, demonstrating the strong interaction between Lys and FILs aggregates. Two of the FIL-based ABSs (30 %wt [C₂C₁Im][C₄F₉SO₃] + 2 %wt K₃PO₄ and 30 %wt [C₂C₁Im][C₄F₉SO₃] + 25 %wt sucrose) allowed the simultaneous purification of Lys and BSA in a single ABS extraction step with high yield (extraction efficiency up to 100%) for both proteins. The purity of both recovered proteins was validated by SDS-PAGE analysis. Even with a high-charge density salt, the FIL-based ABSs developed in this work seem more amenable to be tuned. Lys and BSA were purified through selective partition to opposite phases in a single FIL-based ABS extraction step. FIL-based ABSs are proposed as an improved extraction step for proteins, based on their biocompatibility, customizable properties, and selectivity. Full article

Polyphenols are natural compounds with enhanced antioxidant properties. They are present in relatively high concentrations in fruit/vegetable by-products. Therefore, there is a need for the development of efficient and cost-effective methods for the separation and purification of these valuable compounds. Traditional extraction with organic solvents needs to be switched to novel methods that are more efficient, with reduced extraction times and low consumption of organic solvents. Aiming at developing sustainable processes for the separation and purification of phenolic compounds, we used three model compounds, namely resveratrol, quercetin, and gallic acid, to investigate ionic liquid-based aqueous biphasic systems (IL-ABSs) formed by cholinium-based IL in combination with polypropylene glycol with a molecular mass of 400 g/mol (PPG400). The ABS composition in the two-phase region was selected according to a previously determined phase diagram. Extraction studies indicated the preferential partition of resveratrol and quercetin toward the hydrophobic PPG-rich phase that is mainly dominated by its hydrophobic nature and the strong salting-out effect of ILs. On the other hand, due to its considerably hydrophilic nature, gallic acid preferentially migrates toward the IL phase. The achieved results from grape stem extract demonstrated high extraction efficiencies of cholinium dihydrogen phosphate (~99% for resveratrol for the PPG phase and 78% for gallic acid for the IL phase), with considerable selectivity, demonstrating promising outcomes for potential applications. Full article

Interferon alpha-2b (IFN-$\alpha$2b) is an essential cytokine widely used in the treatment of chronic hepatitis C and hairy cell leukemia, and serum albumin is the most abundant plasma protein with numerous physiological functions. Effective single-step aqueous biphasic system (ABS) extraction for the simultaneous purification of IFN-$\alpha$2b and BSA (serum albumin protein) was developed in this work. Effects of the ionic liquid (IL)-based ABS functionalization, fluorinated ILs (FILs; [C${}_2$C${}_1$Im][C${}_4$F${}_9$SO${}_3$] and [N${}_{1112\left(\mathrm{OH}\right)}$][C${}_4$F${}_9$SO${}_3$]) vs. mere fluoro-containing IL ([C${}_4$C${}_1$Im][CF${}_3$SO${}_3$]), in combination with sucrose or [N${}_{1112\left(\mathrm{OH}\right)}$][H${}_2$PO${}_4$] (well-known globular protein stabilizers), or high-charge-density salt K${}_3$PO${}_4$ were investigated. The effects of phase pH, phase water content (%wt), phase composition (%wt), and phase volume ratio were investigated. The phase pH was found to have a significant effect on IFN-$\alpha$2b and BSA partition. Experimental results show that simultaneous single-step purification was achieved with a high yield (extraction efficiency up to 100%) for both proteins and a purification factor of IFN-$\alpha$2b high in the enriched IFN-$\alpha$2b phase (up to 23.22) and low in the BSA-enriched phase (down to 0.00). SDS-PAGE analysis confirmed the purity of both recovered proteins. The stability and structure of IFN-$\alpha$2b and BSA were preserved or even improved (FIL-rich phase) during the purification step, as evaluated by CD spectroscopy and DSC. Binding studies of IFN-$\alpha$2b and BSA with the ABS phase-forming components were assessed by MST, showing the strong interaction between FILs aggregates and both proteins. In view of their biocompatibility, customizable properties, and selectivity, FIL-based ABSs are suggested as an improved purification step that could facilitate the development of biologics. Full article