Search Results (194)

Incorporating hydrophobic flavonoids such as naringenin into food systems is challenging due to their poor water solubility and instability. Effective delivery systems are essential to improve solubility, dispersibility, and controlled release during digestion. This study developed a food-grade encapsulation system using basil seed gum water-soluble extract (BSG-WSE) combined with proteins, sodium caseinate (NaCas) and whey protein isolate (WPI), via pH-driven and mild heat treatments in aqueous media, without the use of organic solvents, to ensure safety and sustainability. BSG-WSE and NaCas were tested at mass ratios of 1:1, 1:3, and 1:5 under pH conditions of 4, 5, and 7, followed by heat treatments at 60 °C or 80 °C for 30 min. The total biopolymer concentrations were 0.15%, 0.3%, and 0.45% (w/v). The most stable colloidal system was obtained at a 1:1 ratio, pH 4, and 60 °C, which was further evaluated for two additional flavonoids (rutin and quercetin) and with WPI as an alternative protein source. The highest loading capacity (11.18 ± 0.17%) and encapsulation efficiency (72.50 ± 0.85%) were achieved for naringenin under these conditions. Quercetin exhibited superior performance, with a loading capacity of 14.1 ± 3.12% and an encapsulation efficiency of 94.36 ± 5.81%, indicating a stronger affinity for the delivery system. WPI showed lower encapsulation efficiency than NaCas. Ternary systems (BSG-WSE, NaCas, and naringenin) formed under different pH and heat treatments displayed distinct morphologies and interactions. The pH 4 system demonstrated good dispersion and pH-responsive release of naringenin, highlighting its potential as a delivery vehicle for hydrophobic flavonoids. BSG-WSE significantly improved the stability of protein-based complexes formed via pH-driven assembly. Physicochemical characterization, rheological analysis, and release studies suggest that this system is particularly suitable for semi-solid food products such as yogurt or emulsions, supporting its application in functional food development. Full article

Background/Objectives: Advancing information on the key physicochemical properties of biologically active substances enables the development of formulations with reduced dosing, lower toxicity, and minimal adverse effects. This work addresses the knowledge gap concerning the pharmacologically relevant properties of harmaline (HML), with a focus on thermodynamic and kinetic aspects. New data were obtained on the compound’s solubility and distribution coefficients across a wide temperature range. Specifically, solubility was measured in aqueous buffers (pH 2.0 and 7.4), 1-octanol (OctOH), n-hexane (Hex), and isopropyl myristate (IPM), while distribution coefficients were determined in OctOH/pH 7.4, Hex/pH 7.4, and IPM/pH 7.4 systems. Methods: Three membranes—regenerated cellulose (RC), PermeaPad (PP) and polydimethylsiloxane-polycarbonate (PDS)—were used as barriers in permeability studies using a Franz diffusion cell. Results: At 310.15 K, the molar solubility of HML in the solvents decreased in the following order: OctOH > pH 2.0 > pH 7.4 > IPM > Hex. The distribution coefficient of HML showed a strong dependence on the nature of the organic phase, correlating with its solubility in the respective solvents. The OctOH/pH 7.4 distribution coefficient ranged from 0.973 at 293.15 K to 1.345 at 313.15 K, falling within the optimal range for potential drug bioavailability. The transfer of HML into OctOH (from either pH 7.4 or hexane) is thermodynamically spontaneous, whereas its transfer into Hex is unfavorable. Conclusions: Based on its permeability across the PP barrier, HML was classified as highly permeable. The distribution and permeation profiles of HML showed similar trends over 5 h in both the OctOH/pH 7.4–PP and IPM/pH 7.4–PDS systems. These systems were therefore proposed as suitable models for studying HML transport in vitro. Full article

Gold–silver nanoshells (GS-NSs) are hollow spherical nanoparticles with an alloyed Ag-Au shell. GS-NSs exhibit a tunable localized surface plasmon resonance (LSPR) in the visible to near-IR wavelengths as a function of composition and shell thickness and offer greater stability across pH ranges compared to other metal nanoparticles. These properties make GS-NSs promising materials for diagnostics, photothermal therapy, and photocatalysis. However, current research has explored GS-NSs only in aqueous systems, since they immediately aggregate in other solvents, limiting their utility. This paper provides an in-depth study of the choice and effect of non-thiol ligands on the stability and phase-transfer of GS-NSs from aqueous to non-aqueous solvents, such as ethylene glycol, tetrahydrofuran, dichloromethane, and toluene. Ligand exchange for functionalization of GS-NSs was performed with Triton X-100 (TX100), sodium stearate (NaSt), polyvinylpyrrolidone (PVP), and hydroxypropyl cellulose (HPC), prior to phase-transfer. The nanoparticles were phase-transferred to the non-aqueous solvents, and the stability of the colloids in the various solvents before and after functionalization was recorded with UV–visible spectroscopy, dynamic light scattering (DLS), zeta potential (ζ), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The study was also extended to include silver nanoparticles (AgNPs) and gold nanoparticles (AuNPs) to evaluate broad-range applicability. Among the ligands studied, HPC functionalization demonstrated the widest range of phase-transfer stability across 21 days for all three particle systems studied. UV–vis spectroscopy demonstrated sustained LSPR integrity after HPC functionalization in EG, THF, and DCM. SEM, TEM, and hydrodynamic size measurements by DLS further confirmed no aggregation in EG, THF, and DCM but suggested possible twinning or clustering in the solution. Overall, this work successfully identified non-toxic alternatives to expand the LSPR stability of citrate-synthesized metal nanoparticles in organic solvents. Full article

A study on the selective solvent extraction (SX) of molybdenum (Mo) and rhenium (Re) from two industrial pregnant leach solutions (PLSs) was carried out using Alamine 336 as the extractant and the ionic liquid (IL) 1-octyl-3-methyl Imidazolium bis (trifluoromethylsulfonyl) imide [Omim][Tf₂N] as the diluent. One industrial PLS was rich in Mo (VI) (PLS-Mo) and the second one rich in Re (VII) (PLS-Re). Experiments were carried out in open vials in which the concentration of Alamine336 in the diluent, the aqueous-to-organic ratio (A/O), and the stripping with ammonium carbonate (${\left(\mathrm{N}{\mathrm{H}}_4\right)}_2\mathrm{C}{\mathrm{O}}_3$) were carried out systematically. Results indicate that decreasing the aqueous-to-organic (A/O) ratio led to an enhancement in the extraction performances of both Mo (VI) and Re (VII), reaching recoveries of 95%–98% at an A/O ratio of 1:1. However, differences between PLSs became evident at higher ratios, as Re extraction declined more sharply than Mo. Third-phase formation was observed only in the Mo-containing PLS. The PLS–Re system did not exhibit the formation of a third phase due to a lower concentration of metal (1 g/L Mo). The use of ammonium carbonate for stripping led to enhanced recoveries, achieving 84.4% for Re and 46.8% for Mo. A total of 50 extraction-stripping cycles were carried out in this work. These demonstrated nearly total initial extraction, but performance decreased over the cycles because of insufficient stripping and solvent loading. Overall, [Omim][Tf₂N] proved to be an effective and environmentally friendly alternative to conventional diluents for Mo and Re separation and recovery from industrial leach solutions. Full article

The recovery of rare earth elements (REEs) from the spent NdFeB magnets has great strategic significance for ensuring the security of critical mineral resources. This process requires scientifically designed separation technologies to ensure high output and purity of the obtained rare earths. Hydrometallurgy has been widely applied to extract REEs from spent permanent magnets. This paper summarizes and reviews hydrometallurgical technologies, mechanisms, and applications for the separation and recovery of REEs and iron (Fe) from the spent permanent magnets. Key methods include: The hydrochloric acid total solution method, where the spent NdFeB is completely dissolved in hydrochloric acid, iron is precipitated and removed, and then REEs are extracted. The hydrochloric acid preferential dissolution method, where spent NdFeB magnets are first fully oxidized by oxidative roasting, converting Fe²⁺ to Fe³⁺, which hydrolyzes to Fe(OH)₃, and is precipitated and removed, allowing for the subsequent extraction of REEs to obtain rare earth oxides. Acid baking and water leaching, where spent NdFeB is calcined with acidification reagents, and the calcined products are dissolved in water to leach out REEs. At the same time, Fe is retained in the leaching residue. Electrolysis in aqueous solution, where Fe is electrolyzed at the anode or deposited at the cathode to separate it from REES. Organic acids leaching, where organic acids dissolve metals through acidolysis and complexation. Bioleaching, which utilizes microorganisms to recover metal through biological oxidation and complexation. Ionic liquid systems, where Fe or REEs are extracted using ionic liquid or leached by deep eutectic solvents. This paper provides an in-depth discussion on the challenges, advantages, and disadvantages of these strategies for recycling spent NdFeB magnets, as well as the leaching and extraction behavior of REEs. It focuses on environmental impact assessment, improving recovery efficiency, and decreasing reagent consumption. The future development direction for recycling spent NdFeB magnets is proposed, and a research idea of proposing a combined process to avoid the drawbacks of a single recycling method is introduced. Full article

Background/Objectives: The inherent low aqueous solubility of lipophilic drugs, belonging to Class II based on Biopharmaceutical classification system, negatively impacts their oral bioavailability. However, the manufacturing of pharmaceutical dosage forms for these drugs faces challenges related to environmental impact and production complexity. Herein, the surfactant-enriched cross-linked scaffold addresses the limitations of conventional approaches, such as the use of organic solvents, energy-intensive processing, and the demand for sophisticated equipment. Methods: Scaffold former (Pluronic F68) and scaffold trigger agent (propylene glycol) were used to prepare cross-linked scaffold loaded with candesartan cilexetil as a model for lipophilic drugs. Moreover, surfactants were selected based on the measured solubility to enhance formulation loading capacity. Design-Expert was used to study the impact of Tween 80, propylene glycol, and Pluronic F68 concentrations on the measured responses. In addition, in vitro dissolution study was implemented to investigate the drug release profile. The current approach was assessed against the limitations of conventional approach in terms of environmental and manufacturing feasibility. Results: The optimized formulation (59.27% Tween 80, 30% propylene glycol, 10.73% Pluronic F68) demonstrated a superior drug loading capacity (19.3 mg/g) and exhibited a solid-to-liquid phase transition at 35.5 °C. Moreover, it exhibited a rapid duration of solid-to-liquid transition within about 3 min. In vitro dissolution study revealed a remarkable enhancement in dissolution with 92.87% dissolution efficiency compared to 1.78% for the raw drug. Conclusions: Surfactant-enriched cross-linked scaffold reduced environmental impact by eliminating organic solvents usage and reducing energy consumption. Moreover, it offers significant manufacturing advantages through simplified production processing. Full article

Alkylic molecules are found as some of the main components of natural essential oils. These essential oils offer several therapeutic properties in skin treatments and cosmetics. Systems providing controlled release of these molecules through the skin tissue are a challenge for their applications. This work explores some properties of the crystal structure of α-pinene and the adsorption and desorption of five terpenoid components of essential oils, such as α-pinene, limonene, β-ocimene, β-caryophyllene, and β-elemene, in the confined surfaces provided by natural clay minerals, particularly montmorillonite (MNT). These terpenoids have a methyl-ethenyl group as their common structural feature. Molecular modelling calculations have been applied at the atomic scale, including force fields, quantum mechanical methods, and molecular dynamics simulations. We calculated the crystallographic and spectroscopic properties of the α-pinene crystal via density functional theory (DFT)-level calculations, which were very close to the known experimental data. Moreover, this work explored the adsorption and desorption of these molecules in confined surfaces provided by MNT. Molecular dynamics simulations also showed the adsorption of these organics in the confined interlayer space of MNT at room temperature and allowed us to know the diffusion coefficient of these adsorbates in this material. The direct adsorption process of these molecules in the vapour phase is not energetically favourable, suggesting the use of non-aqueous solvents and kinetics and thermodynamic conditions for this process. However, the release of these molecules into aqueous media are energetically favourable, predicting that MNT–essential oil can be an excellent pharmaceutical formulation to be delivered in skin as a bioactive preparation with anti-inflammatory or cosmetic power. This research was performed to predict possible therapeutic applications for future experimental works. Full article

The thermal and optical properties of aqueous dispersions of magnetite nanoparticles were studied by dual-beam thermal-lens spectrometry. Surface-modified magnetite nanoparticles with an average crystal size of 7.5 nm were synthesized by a simple, one-stage method of coprecipitation followed by surface functionalization. For this purpose, the most popular and promising modifiers based on surfactants, polyelectrolytes, biopolymers and organic acids were used. The effect of the concentration of nanoparticles (in the range from 0.01 to 5 mg/L) and the nature of the surface modifier on the thermal diffusivity of the dispersion was studied. It was found that at concentrations of 0.4–0.6 mg/L, the dispersions exhibit heat-accumulating properties, which may be promising in the development of a magnetically controlled heat-conducting liquid. Thermal lens spectrometry in the steady-state measurement mode was used to reveal the processes of deposition and adsorption of magnetite nanoparticles on the surface of a quartz cell, leading to an apparent increase in thermal diffusivity by more than 30%. The paper touches upon the issues of accuracy and precision of temperature diffusion measurements, processing, and presentation of measurement results of time-resolved transient and steady-state signals for dispersed systems. The ratio of the change in the steady-state thermal-lens signals to the change in concentration regarding the concentration (dϑ/dc vs. c) provides a way to identify a systematic error at a low level (less than 5%) of thermal-lens measurements caused by a high concentration (or optical absorption) of the object. Various options for signal normalization (in terms of power, absorbance, and pure-solvent signal) are considered, and their advantages and disadvantages are discussed. An approach to using thermal diffusivity as a function of the steady-state signal of the sample is proposed. This approach allows for a comparative thermal-lens analysis of objects with different optical and thermal properties. Full article

Background/Objectives: The present work deals with the sol–gel synthesis of hybrid materials based on a silica–polyvinylpyrrolidone (Si-PVP) system. Methods: The nanohybrids have been prepared using an acidic catalyst at ambient temperature. Ibuprofen (IBP) was used as a model substance in the obtained model drug systems, while tetraethyl orthosilicate (TEOS) was used as a silica precursor. Poly(vinylpyrrolidone) (PVP) and IBP were introduced into the reaction mixture as solutions in ethanol using two different approaches: (i) a direct introduction of a drug solution into the reaction mixture during sol–gel synthesis, and (ii) a solvent deposition technique. Results: XRD data provide evidence that IBP entrapped in the silica–PVP network is in an amorphous state. By SEM it was revealed that in the adsorbate, the IBP particles possess an average particle size of about 20 μm. Based on the obtained IR and UV-Vis spectral results, the existence of hydrogen bonding of IBF with silica and PVP could be suggested. Solid-state NMR analysis allowed the identification of the presence of both crystalline-like and amorphous phases in the hybrid material prepared by the sol–gel method, while it was demonstrated that in the adsorbate, the rigid crystalline dimeric structure of the drug has been preserved. Conclusions: The overall analysis of the structural characteristics of the two materials indicated that in the hybrid material obtained by the sol–gel method, the interactions between the amorphous drug, PVP, and the silica matrix are more pronounced as compared to the adsorbate. An improvement of the drug’s aqueous solubility as well of in vitro drug release profile (up to 8 h) was achieved, demonstrating the potential of the developed drug–silica–organic polymer nanohybrid as a promising drug delivery system. Full article

Significant depletion of natural resources, coupled with increased environmental pollution resulting from the constant evolution of global industrialization, poses a considerable problem. Therefore, it is unsurprising that sustainable “green” chemistry and technology are gathering the worldwide scientific community, whose common goal is to find applicable solutions for the abovementioned problems. This paper combined the ultrasonic extraction method (a form of “green” technology) with natural deep eutectic solvents (NADESs, a type of “green” solvent) for the production of extracts from an industrial by-product (discarded waste wild apple dust). Waste wild apple dust was pretreated with different NADESs in order to explore the pretreatment benefits regarding ultrasonic extraction of bioactive compounds. Among all solvents used, aqueous propylene glycol was chosen as the best system, which, combined with Reline NADES pretreatment, provided the highest TPC and TFC values, together with the best antioxidant activities. UHPLC-DAD-MS analyses of extracts revealed the presence of natural organic acids, quercetin and kaempferol derivatives, tannins, and flavones. Following this procedure, valorization of agro-industrial apple herbal waste resulted in obtaining extracts with high potential for utilization in different industrial branches (food and pharmaceutical industries), contributing to both cleaner production and reduced environmental impact. Full article

Vacuum Membrane Distillation (VMD) is a separation process applied to liquid solutions; however, there are phenomenological and operational differences depending on whether the component to be separated is the solute or the solvent. The objective of this article is to develop a mathematical and phenomenological model of the VMD process applied to the separation of volatile organic compound (VOCs) from aqueous solutions and the desalination of saline aqueous solutions. This approach enabled the evaluation of the influence of variables and operating conditions on both separation efficiency and system productivity. Under the analyzed conditions, increasing the temperature, flow rate, and vacuum pressure led to approximate increases in permeate flux of 400%, 10%, and 50%, respectively. In the case of concentration increase, the permeate flux increases linearly for VOC separation and decreases asymptotically for saline solution desalination. Therefore, adjusting the feed temperature is recommended to achieve significant changes in permeate flux. Full article

Background/Objectives: Alectinib, a second-generation tyrosine kinase inhibitor indicated for the treatment of non-small-cell lung cancer (NSCLC), exhibits suboptimal oral bioavailability, primarily attributable to its inherently low aqueous solubility and limited dissolution kinetics. This study aimed to enhance Alectinib’s solubility and therapeutic efficacy by formulating a G4-NH2-PAMAM dendrimer complex. Methods: The complex was prepared using the organic solvent evaporation method and characterized by DSC, FTIR, dynamic light scattering (DLS), and zeta potential measurements. A validated high-performance liquid chromatography (HPLC) method quantified the Alectinib. In vitro drug release studies compared free Alectinib with the G4-NH2-PAMAM dendrimer complex. Cytotoxicity against NSCLC cell line A549 was assessed using MTT assays, clonogenic assay, and scratch-wound assay. Xenograft effect was investigated in the H460 lung cell line. Pharmacokinetic parameters were evaluated in rats using LC–MS/MS. Results: Alectinib exhibited an encapsulation efficiency of 59 ± 5%. In vitro release studies demonstrated sustained drug release at pH 6.8 and faster degradation at pH 2.5. Anticancer activity in vitro showed comparable efficacy to free Alectinib, with 98% migration inhibition. In vivo tumor suppression studies revealed near-complete tumor regression (~100%) after 17 days of treatment, compared to 75% with free Alectinib. Pharmacokinetic analysis indicated enhanced absorption (shorter Tmax), prolonged systemic circulation (longer half-life), and higher bioavailability (increased AUC) for the dendrimer-complexed drug. Conclusions: These findings suggest that the G4-NH2-PAMAM dendrimer system significantly improves Alectinib’s pharmacokinetics and therapeutic potential, making it a promising approach for NSCLC treatment. Full article

The development of ceria (CeO_2−x)-based nanoantioxidants requires fine-tuning of structural and surface properties for enhancing antioxidant behavior in biological environments. In this contest, here ultrasmall water-dispersible CeO_2−x nanoparticles (NPs), characterized by a high Ce³⁺/Ce⁴⁺ ratio, were synthesized in a non-polar solvent and phase-transfer to an aqueous environment through ligand-exchange reactions using citric acid (CeO_2−x@Cit) and post-treatment with dopamine hydrochloride (CeO_2−x@Dopa). The concept behind this work is to enhance via surface engineering the intrinsic antioxidant properties of CeO_2−x NPs. For this purpose, thanks to electron transfer reactions between dopamine and CeO_2−x, the CeO_2−x@Dopa was obtained, characterized by increased surface Ce³⁺ sites and surface functionalized with polydopamine bearing o-quinone structures as demonstrated by complementary spectroscopic (UV–vis, FT-IR, and XPS) characterizations. To test the antioxidant properties of CeO_2−x NPs, the scavenging activity before and after dopamine treatment against artificial radical 1,1-diphenyl-2-picrylhydrazyl (DPPH^·) and the ability to reduce the reactive oxygen species in Diencephalic Immortalized Type Neural Cell line 1 were evaluated. CeO_2−x@Dopa demonstrated less efficiency in DPPH^· scavenging (%radical scavenging activity 13% versus 42% for CeO_2−x@Cit before dopamine treatment at 33 μM DPPH^· and 0.13 mg/mL loading of NPs), while it markedly reduced intracellular ROS levels (ROS production 35% compared to 66% of CeO_2−x@Cit before dopamine treatment with respect to control—p < 0.001 and p < 0.01, respectively). While steric hindrance from the dopamine-derived polymer layer limited direct electron transfer from CeO_2−x NP surface to DPPH^·, within cells the presence of o-quinone groups contributed with CeO_2−x NPs to break the autoxidation chain of organic substrates, enhancing the antioxidant activity. The functionalization of NPs with o-quinone structures represents a valuable approach to increase the inherent antioxidant properties of CeO_2−x NPs, enhancing their effectiveness in biological systems by promoting additional redox pathways. Full article

Background/objectives: Propolis, known for its medicinal properties, faces challenges in pharmaceutical applications due to its low aqueous solubility, attributed to its resinous and hydrophobic nature. This limits oral administration, reducing its bioavailability and pharmacological activities. To overcome these barriers, cyclodextrins (CDs), cyclic oligosaccharides, are widely studied as carrier systems that enhance the solubility and bioavailability of propolis and other nonpolar compounds. This study aimed to review patents that developed innovative therapeutic approaches to improve the physicochemical and biological properties of propolis through complexation with CDs. Methods: Active and application patents registered over the last 17 years were searched across multiple databases, resulting in the selection of eight inventions for detailed analysis. Results: These patents highlight therapeutic applications of propolis–CD systems for conditions such as diabetes and skin and gastrointestinal cancers, as well as antimicrobial, immunostimulant, and antioxidant effects. Additionally, novel extraction processes free of organic solvents, including nanometric-scale powder extracts, are described. Conclusions: Findings from scientific articles support the patent data, demonstrating that CD complexation significantly enhances the solubility and therapeutic efficacy of propolis. Thus, these patents present an innovative and promising strategy for developing propolis-based pharmaceutical products. Full article

Background/Objectives: In this study, we present a green, scalable platform for the production of water-dispersible powders co-encapsulating the lipophilic bioactives curcumin (Cur) and eugenol (Eug) within the amphiphilic polymer Soluplus^® (SP) via low-temperature spray drying. Methods: The amount of Cur (1%, 5%, and 10%) and Eug (5%, 10%, 15%, and 20%) was varied to achieve single- and double-loaded water-soluble powders with the maximum amount of active substances. The powders containing a higher loading of Cur, 5% and 10% (and Eug), were obtained from water/ethanol mixtures (2:1 and 5:1 v/v ratio), while the formulation with 1% of Cur was spray-dried by using water as a solvent. Results: By leveraging aqueous or aqueous–ethanolic feed systems, we achieved high loading of the bioactive substances—up to 10% Cur and 20% Eug (w/w)—while minimizing organic solvent use. Myo-inositol was incorporated as a stabilizing excipient to modulate particle morphology, improve powder flowability, and enhance redispersibility. Physicochemical characterization revealed nanoscale micellization (53–127 nm), amorphization of both actives as confirmed by XRD and DSC, and the absence of crystalline residue. Encapsulation efficiencies exceeded 95% for Cur and 93% for Eug. Dissolution tests demonstrated a rapid release from the 5% Cur/5% Eug formulation (>85% in 5 min), while higher-loaded single-formulations showed progressively slower release (up to 45 min). Conclusions: This work demonstrates a robust and environmentally responsible encapsulation strategy, suitable for delivering poorly water-soluble phytochemicals with potential applications in oral nutraceuticals and pharmaceutical dosage forms. Full article