Search Results (31)

Alkaline treatment is well suited for extracting high-molecular-weight hemicelluloses, specifically hardwoods xylans, which, due to their polymer structure and chemical characteristics, enable the production of films with desirable mechanical, barrier, and optical properties for packaging applications. Despite its relevance, the optimization of antisolvent addition has received little attention in the literature. This study explores the use of eucalyptus industrial residue as feedstock, utilizing a statistical design to determine the optimal extraction conditions for hemicelluloses while minimizing the lignin content in the recovered liquor. The process uses alkali loads that are compatible with those in conventional Kraft pulp mills. Optimal extraction conditions involve a temperature of 105 °C, 16.7% NaOH charge, and 45 min at maximum temperature. The resulting liquor was subjected to ethanol precipitation under varying pH conditions (initial pH, 9, 7, 5, and 2) and different ethanol-to-liquor ratios (1:1 to 4:1). The acidification was performed using hydrochloric, sulfuric, and acetic acids. Ethanol served as the main antisolvent, while isopropyl alcohol and dioxane were tested for comparison. Results show that 2.3 ± 0.2% of xylans (based on oven-dry biomass) could be extracted, minimizing lignin content in the liquor. This value corresponds to the extraction of 15.6% of the xylans present in the raw material. The highest xylan precipitation yield (78%) was obtained at pH 7, using hydrochloric acid for pH adjustment and an ethanol-to-liquor ratio of 1:1. These findings provide valuable insight into optimizing hemicellulose recovery through antisolvent precipitation, contributing to more efficient biomass valorization strategies within lignocellulosic biorefineries. Full article

γ-aminobutyric acid, a critical neurotransmitter, is experiencing an increasing demand in the medical and health fields. Conventional processes for γ-aminobutyric acid purification from fermentation broth encounter significant challenges, such as high ethanol usage, low yield, complex process flow, and environmental pollution. Therefore, a purification process based on crystallization techniques was developed to address the above issues. The process was implemented in two stages: desalination and γ-aminobutyric acid treatment. Na₂SO₄ was effectively removed through a cooling crystallization technique. γ-aminobutyric acid with a purity of 98.66% and a yield of 67.32% was further obtained through a designed “antisolvent-cooling” crystallization process in a 3.2 L system. Moreover, the new process reduced ethanol usage compared to conventional processes, streamlined the purification process flow, and was more environmentally sustainable. Furthermore, we established an industrial-scale model for γ-aminobutyric acid production. Techno-economic analysis indicates that an investment in a plant with an annual capacity of 74.16 tons of γ-aminobutyric acid is projected to achieve payback in 1.98 years. In conclusion, the crystallization-based purification process is poised for industrial-scale γ-aminobutyric acid production due to its high efficiency, economic viability, energy conservation, and environmental compatibility. Full article

Novel AB-Polybenzimidazole (AB-PBI)/TiO₂ nanocomposite membranes have been prepared using a synthetic green chemistry approach. Modified Eaton’s reagent (methansulfonic acid/P₂O₅) was used as both reaction media for microwave-assisted synthesis of AB-PBI and as an efficient dispersant of partially agglomerated titanium dioxide powders. Composite membranes of 80 µm thickness have been prepared by a film casting approach involving subsequent anti-solvent inversion in order to obtain porous composite membranes possessing high sorption capacity. The maximal TiO₂ filler content achieved was 20 wt.% TiO₂ nanoparticles (NPs). Titania particles were green synthesized (using a different content of Mentha Spicata (MS) aqueous extract) by hydrothermal activation (150 °C), followed by thermal treatment at 400 °C. The various methods such as powder X-ray diffraction and Thermogravimetric analyses, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy and Energy-dispersive X-ray spectroscopy, Electronic paramagnetic resonance, Scanning Electron Microscopy and Transmission Electron Microscopy have been used to study the phase and surface composition, structure, morphology, and thermal behavior of the synthesized nanocomposite membranes. The photocatalytic ability of the so-prepared AB-Polybenzimidazole/bio-TiO₂ membranes was studied for decolorization of Reactive Black 5 (RB5) as a model azo dye pollutant under UV light illumination. The polymer membrane in basic form, containing TiO₂ particles, was obtained with a 40 mL quantity of the MS extract, exhibiting the highest decolorization rate (96%) after 180 min of UV irradiation. The so-prepared AB-Polybenzimidazole/TiO₂ samples have a powerful antibacterial effect on E. coli when irradiated by UV light. Full article

This study investigated the valorization of Ilex guayusa leaves by producing a low-caffeine, antioxidant-rich product through the supercritical antisolvent extraction (SAE) process. The objective was to concentrate the antioxidants while selectively reducing the caffeine. The SAE treatments were conducted using an ethanolic extract of guayusa leaves under varying pressure (80 bar–150 bar) and temperature (35–45 °C) conditions to improve the recovery of chlorogenic acid (CGA) and caffeine fractionation. The co-precipitation of antioxidants with polyvinylpyrrolidone (PVP) (ratio 1:1–1:2 mass/mass) as an encapsulant was also studied. The SAE precipitates were analyzed for their recovery yield, CGA and caffeine contents, antioxidant activity, and total phenols. Based on the statistical analysis, the optimal conditions for the SAE were 120 bar and 45 °C. Under these conditions, the CGA concentration increased from 43.02 mg/g extract to 237 mg/g precipitate, while the caffeine was reduced to less than 1% mass. Co-precipitation with PVP improved the recovery yield by more than two times than the SAE alone while maintaining the caffeine content below 1% mass. Additionally, the co-precipitation with PVP facilitated the formation of spherical microparticles, indicating successful encapsulation of the bioactive compounds, with an IC₅₀ of 0.51 ± 0.01 mg/mL for DPPH and 0.18 ± 0.01 mg/mL for ABTS. These results highlight the effectiveness of the SAE co-precipitation process in developing low-caffeine functional ingredients with potential food and pharmaceutical applications. Full article

Copper(I) thiocyanate (CuSCN) is considered an efficient HTL of low cost and with high stability in perovskite solar cells (PSCs). However, the diethyl sulfide solvent used for CuSCN preparation is known to cause damage to the underlying perovskite layer in n-i-p PSCs. Antisolvent treatment of CuSCN during spin-coating can effectively minimize interfacial interactions. However, the effects of antisolvent treatment are not sufficiently understood. In this study, the effects of five different antisolvents were investigated. Scanning electron microscopy and X-ray diffraction analyses showed that the antisolvent treatment improved the crystallinity of the CuSCN layer on the perovskite layer and reduced damage to the perovskite layer. However, X-ray and ultraviolet photoelectron spectroscopy analyses showed that antisolvent treatment did not affect the chemical bonds or electronic structures of CuSCN. As a result, the power conversion efficiency of the PSCs was increased from 14.72% for untreated CuSCN to 15.86% for ethyl-acetate-treated CuSCN. Full article

The solvolysis reaction with ionic liquids is one of the most frequently used methods for producing nanometer-sized cellulose. In this study, the nanocellulose was obtained by reacting microcrystalline cellulose with 1-ethyl-3-methylimidazolium acetate (EmimOAc). The aim of this research was to determine the influence of various antisolvents used in the regeneration of cellulose after treatment with ionic liquid on its properties. The following antisolvents were used in this research: acetone, acetonitrile, water, ethanol and a mixture of acetone and water in a 1:1 v/v ratio. The nanocellulose was characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), dynamic light scattering (DLS), scanning electron microscopy (SEM) and elemental analysis (EA). The results show that the antisolvent used to regenerate cellulose after the solvolysis reaction with EmimOAc affects its properties. Water, ethanol and a mixture of acetone and water successfully removed the used ionic liquid from the cellulose structure, while acetone and acetonitrile were unable to completely remove EmimOAc from the cellulosic material. The results of the XRD analysis indicate that there is a correlation between the ionic liquid content in the regenerated cellulose and its degree of crystallinity. Among the tested solvents, water leads to the effective removal of EmimOAc from the cellulose structure, which is additionally characterized by the smallest particle size and non-formation of agglomerates. Full article

In recent years, concerns about the harmful effects of synthetic UV filters on the environment have highlighted the need for natural sun blockers. Lignin, the most abundant aromatic renewable biopolymer on Earth, is a promising candidate for next-generation sunscreen due to its inherent UV absorbance and its green, biodegradable, and biocompatible properties. Lignin’s limitations, such as its dark color and poor dispersity, can be overcome by reducing particle size to the nanoscale, enhancing UV protection and formulation. In this study, 100–200 nm lignin nanoparticles (LNPs) were prepared from various biomass by-products (hardwood, softwood, and herbaceous material) using an eco-friendly anti-solvent precipitation method. Pure lignin macroparticles (LMPs) were extracted from beech, spruce, and wheat straw using an ethanol–organosolv treatment and compared with sulfur-rich kraft lignin (KL). Sunscreen lotions made from these LMPs and LNPs at various concentrations demonstrated novel UV-shielding properties based on biomass source and particle size. The results showed that transitioning from the macro- to nanoscale increased the sun protection factor (SPF) by at least 2.5 times, with the best results improving the SPF from 7.5 to 42 for wheat straw LMPs and LNPs at 5 wt%. This study underscores lignin’s potential in developing high-quality green sunscreens, aligning with green chemistry principles. Full article

Cesium bismuth iodide perovskite material offers good stability toward ambient conditions and has potential optoelectronic characteristics. However, wide bandgap, absorber surface roughness, and poor surface coverage with pinholes are among the key impediments to its adoption as a photovoltaic absorber material. Herein, bandgap modification and the tailoring of surface morphology have been performed through molar ratio variation and antisolvent treatment, whereby type III antisolvent (toluene) based on Hansen space has been utilized. XRD and Raman spectroscopy analyses confirm the formation of a 0D/2D mixed dimensional structure with improved optoelectronic properties when the molar ratio of CsI/BiI₃ was adjusted from 1.5:1 to 1:1.5. The absorption results and Tauc plot determination show that the fabricated film has a lower bandgap of 1.80 eV. TRPL analysis reveals that the film possesses a very low charge carrier lifetime of 0.94 ns, suggesting deep defects. Toluene improves the charge carrier lifetime to 1.89 ns. The average grain size also increases from 323.26 nm to 444.3 nm upon toluene addition. Additionally, the inclusion of toluene results in a modest improvement in PCE, from 0.23% to 0.33%. Full article

The potential of the supercritical antisolvent micronization (SAS) technique was evaluated for the production of CaO-based particles with a size and a physical structure that could enable high performance for CO₂ capture through the calcium looping process. Two sources of calcium derivative compounds were tested, waste marble powder (WMP) and dolomite. The SAS micronization of the derivate calcium acetate was carried out at 60 °C, 200 bar, a 0.5 mL min⁻¹ flow rate of liquid solution, and 20 mg mL⁻¹ concentration of solute, producing, with a yield of more than 70%, needle-like particles. Moreover, since dolomite presents with a mixture of calcium and magnesium carbonates, the influence of the magnesium fraction in the SAS micronization was also assessed. The micronized mixtures with lower magnesium content (higher calcium fraction) presented needle-like particles similar to WMP. On the other hand, for the higher magnesium fractions, the micronized material was similar to magnesium acetate micronization, presenting sphere-like particles. The use of the micronized material in the Ca-looping processes, considering 10 carbonation-calcination cycles under mild and realistic conditions, showed that under mild conditions, the micronized WMP improved CaO conversion. After 10 cycles the micronization, WMP presented a conversion 1.8 times greater than the unprocessed material. The micronized dolomite, under both mild and real conditions, maintained more stable conversion after 10 cycles. Full article

Background: Orlistat (ORL) is an effective irreversible inhibitor of the lipase enzyme, and it possesses anticancer effects and limited aqueous solubility. This study was designed to improve the aqueous solubility, oral absorption, and tissue distribution of ORL via the formulation of nanocrystals (NCs). Methods: ORL-NC was prepared using the liquid antisolvent precipitation method (bottom-up technology), and it demonstrated significantly improved solubility compared with that of the blank crystals (ORL-BCs) and untreated ORL powder. The biodistribution and relative bioavailability of ORL-NC were investigated via the radiolabeling technique using Technetium-99m (^99mTc). Female Swiss albino mice were used to examine the antitumor activity of ORL-NC against solid Ehrlich carcinoma (SEC)-induced hepatic damage in mice. Results: The prepared NCs improved ORL’s solubility, bioavailability, and tissue distribution, with evidence of 258.70% relative bioavailability. In the in vivo study, the ORL-NC treatment caused a reduction in all tested liver functions (total and direct bilirubin, AST, ALT, and ALP) and improved modifications in liver sections that were marked using hematoxylin and eosin staining (H&E) and immunohistochemical staining (Ki-67 and ER-α) compared with untreated SEC mice. Conclusions: The developed ORL-NC could be considered a promising formulation approach to enhance the oral absorption tissue distribution of ORL and suppress the liver damage caused by SEC. Full article

Because of the specific thermodynamic properties of active pharmaceutical ingredients, the process of crystallization often meets implementation challenges in the pharmaceutical industry. Therefore, it is essential to select the appropriate method and system for the crystallization of a drug. Ceritinib, an active ingredient in the treatment of lung cancer, was formed as a result of pH modification during the cooling crystallization of ceritinib dihydrochloride solution. By carrying out processes in various solvent systems, several polymorphs were produced. A combination of forms B and C was generated in the ethanol–water system, resulting in smaller crystals. The acetone–water system produced pure form A, which has larger crystals and is more applicable for forthcoming studies. To additionally enhance granulometric properties, ceritinib form A was recrystallized in tetrahydrofuran at different temperatures using antisolvent crystallization. Crystallization at a higher saturation temperature results in larger and more compact crystals, which enhances filtration and drying. Full article

The aim of the study was to obtain untreated and treated betulin colloidal particles and assess their effect on the viability, morphology, proliferation and cytokine secretion of human dermal fibroblasts. To improve bioavailability, betulin treatment was performed by an antisolvent precipitation technique. The average particle size after treatment in the aqueous dispersion decreased from 552.9 ± 11.3 to 278.2 ± 1.6 nm. Treated betulin colloidal particles showed no cytotoxicity up to a concentration of 400 µg·mL⁻¹ in the colorimetric tetrazolium salt viability test (CCK-8). Moreover, the cell morphology was not changed in the presence of betulin colloidal particles at a concentration range from 0.78 to 400 µg·mL⁻¹. The obtained results also show that betulin particles induce the secretion of the proinflammatory and angiogenesis-stimulating cytokine IL-8. However, further studies would be required to clarify the mechanism of IL-8 secretion induction. Full article

Background: Ursodeoxycholic acid (UDCA) is a therapeutic agent used for the treatment of cholestatic hepatobiliary diseases in pediatric patients. It is a bile acid that presents high lipophilicity, and it belongs to Class II of the Biopharmaceutical Classification System (BCS), which exhibits low water solubility and high intestinal permeability, which leads to poor oral absorption. The objective of this work was to design and optimize UDCA nanosuspensions by means of the precipitation-ultrasonication method to improve the solubility, dissolution, and oral bioavailability of UDCA. Methods: A three-level, three-factor Box–Behnken design was used to optimize formulation variables and obtain uniform, small-particle-size UDCA nanosuspensions. The independent variables were: stabilizer percentage (X₁), amplitude (X₂), and sonication time (X₃), and the dependent variable was the particle size (Y₁). In the precipitation–ultrasonication method, UDCA was dissolved in acetone:PEG 400 (1:1 v/v) and quickly incorporated into the antisolvent (pre-cooled aqueous dispersion of HPMC E-15 0.3%), by means of intense sonication at 50 W for 5 min, controlling temperature through an ice water bath. The lyophilization efficacy was evaluated by means of a cryoprotective efficacy test, working with 10% maltose at −80 °C. The nanosuspensions were characterized by dynamic light scattering (DLS), X-ray diffraction, and scanning electron microscopy (SEM). The physicochemical stability was determined at 25 °C and 4 °C at 7, 14, 30, and 60 days, and the UDCA content was analyzed via HPLC-UV. An in vitro dissolution assay and an oral bioavailability study were performed in male Wistar rats. Results: A significant impact was achieved in the optimized nanosuspension with 0.3% (stabilizer), 50 W (amplitude), and 5 min (sonication time), with a particle size of 352.4 nm, PDI of 0.11, and zeta potential of −4.30 mV. It presented adequate physicochemical stability throughout the study and the UDCA content was between 90% and 110%. In total, 86% of UDCA was dissolved in the in vitro dissolution test. The relative oral bioavailability was similar without significant statistical differences when comparing the lyophilized nanosuspension and the commercial tablet, the latter presenting a more erratic behavior. The pharmacokinetic parameters of the nanosuspension and the commercial tablet were T_max (1.0 ± 0.9 h vs. 2.0 ± 0.8 h, respectively), C_max (0.558 ± 0.118 vs. 0.366 ± 0.113 µM, respectively), ΔC_max (0.309 ± 0.099 vs. 0.232 ± 0.056, respectively), AUC (4.326 ± 0.471 vs. 2.188 ± 0.353 µg/mL.h, respectively, p < 0.02), and IAUC_0–24h (2.261 ± 0.187 µg/mL.h vs. 1.924 ± 0.440 µg/mL.h, respectively). Conclusions: The developed nanosuspension presents an appropriate dosage and administration for pediatric patients. On the other hand, it exhibits an adequate absorption and UDCA oral bioavailability. Full article

In contrast to their well-known physiological properties, phytochemicals, such as flavonoids, have been less frequently examined for their physiochemical properties (e.g., surface activity). A natural quercetin self-stabilizing Pickering emulsion was fabricated and characterized in the present study. The antisolvent precipitation method was used to modify quercetin (in dihydrate form), and the obtained particles were characterized by light microscope, atom force microscope, XRD, and contact angle. The antisolvent treatment was found to reduce the particle size, crystallinity, and surface hydrophobicity of quercetin. We then examined the effects of the antisolvent ratio, particle concentration, and oil fraction on the properties of the quercetin particle-stabilized emulsions. In addition, increasing the antisolvent ratio (1:1~1:10) effectively improved the emulsification performance of the quercetin particles. The emulsion showed good storage stability, and the particle size of the emulsion decreased with the rising particle concentration and increased with the rising oil phase ratio. The findings indicate that natural quercetin treated with antisolvent method has a good ability to stabilize Pickering emulsion, and this emulsion may have good prospective application potential for the development of novel and functional emulsion foods. Full article

We have investigated the effects of the methylammonium bromide (MABr) content of the precursor solution on the properties of wide-bandgap methylammonium lead tribromide (MAPbBr₃) perovskite solar cells (PSCs). In addition, the anti-solvent process for fabricating MAPbBr₃ perovskite thin films was optimized. The MAPbBr₃ precursor was prepared by dissolving MABr and lead bromide (PbBr₂) in N,N-dimethylformamide and N,N-dimethyl sulfoxide. Chlorobenzene (CB) was used as the anti-solvent. We found that both the morphology of the MAPbBr₃ layer and the PSCs performance are significantly affected by the MABr content in perovskite precursor solution and anti-solvent dripping time. The best-performing device was obtained when the molar ratio of MABr:PbBr₂ was 1:1 and the CB drip time was 10 s. The best device exhibited a power conversion efficiency of 7.58%, short-circuit current density of 7.32 mA·cm⁻², open-circuit voltage of 1.30 V, and fill factor of 79.87%. Full article