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13 pages, 4546 KiB  
Article
Efficient and Green Flotation Separation of Molybdenite from Chalcopyrite Using 1-Thioglycerol as Depressant
by Feng Jiang, Shuai He, Wei Sun, Yuanjia Luo and Honghu Tang
Metals 2025, 15(3), 299; https://doi.org/10.3390/met15030299 (registering DOI) - 9 Mar 2025
Viewed by 131
Abstract
The effective and environmental separation of chalcopyrite and molybdenite has long presented a challenge in mineral processing due to their similar floatability and close association at room temperature. This study explores the non-toxic 1-thioglycerol (1-TG) as a selective depressant for chalcopyrite–molybdenite flotation separation. [...] Read more.
The effective and environmental separation of chalcopyrite and molybdenite has long presented a challenge in mineral processing due to their similar floatability and close association at room temperature. This study explores the non-toxic 1-thioglycerol (1-TG) as a selective depressant for chalcopyrite–molybdenite flotation separation. An impressive separation effect was realized through single-mineral and mixed-mineral flotation experiments when using 1-TG as a depressant and kerosene as a collector. Contact angle measurements, zeta potential tests, and Fourier transform infrared spectroscopy (FT-IR) confirm the selective adsorption of 1-TG on the chalcopyrite surface, leading to enhanced surface hydrophilicity and the inhibition of collector adsorption. The depression mechanism is further elucidated through X-ray photoelectron spectroscopy (XPS), which demonstrates that it occurs via chemosorption between the thiol group in 1-TG and active iron sites on the chalcopyrite surface. These findings provide a potential efficient depressant for chalcopyrite–molybdenite flotation separation with low dosage, environmental friendliness, and human harmlessness. Full article
(This article belongs to the Special Issue Advances in Flotation Separation and Mineral Processing)
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Figure 1
<p>XRD patterns of (<b>a</b>) chalcopyrite and (<b>b</b>) molybdenite samples.</p>
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<p>Flotation recovery rates of chalcopyrite and molybdenite vary with the (<b>a</b>) concentration of 1-TG and (<b>b</b>) pH value (2.8 × 10<sup>−4</sup> mol/L 1-TG, 2.5 × 10<sup>−4</sup> mol/L kerosene, and 4.5 × 10<sup>−4</sup> mol/L terpineol).</p>
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<p>Recovery rate and grade of flotation concentrate for artificially mixed ore were measured at room temperature.</p>
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<p>Contact angles of chalcopyrite and molybdenite before and after treatment with various reagents.</p>
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<p>Zeta potentials of (<b>a</b>) chalcopyrite and (<b>b</b>) molybdenite versus pH value.</p>
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<p>FT-IR spectra of (<b>a</b>) kerosine and 1-TG; (<b>b</b>) chalcopyrite and (<b>c</b>) molybdenite treated with different reagents.</p>
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<p>(<b>a</b>) Cu 2p<sub>3/2</sub>, (<b>b</b>) Fe 2p<sub>3/2</sub>, and (<b>c</b>) S 2p high-resolution XPS spectra of chalcopyrite.</p>
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<p>(<b>a</b>) Mo 3d and (<b>b</b>) S 2p high-resolution XPS spectra of molybdenite.</p>
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<p>Illustration of the probable adsorption mechanism of 1-TG on chalcopyrite surface.</p>
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13 pages, 4135 KiB  
Article
On-Chip Electrochemical Sensor Based on 3D Graphene Assembly Decorated Ultrafine RuCu Alloy Nanocatalyst for In Situ Detection of NO in Living Cells
by Haibo Liu, Kaiyuan Yao, Min Hu, Shanting Li, Shengxiong Yang and Anshun Zhao
Nanomaterials 2025, 15(6), 417; https://doi.org/10.3390/nano15060417 (registering DOI) - 8 Mar 2025
Viewed by 77
Abstract
In this work, we developed 3D ionic liquid (IL) functionalized graphene assemblies (GAs) decorated by ultrafine RuCu alloy nanoparticles (RuCu-ANPs) via a one-step synthesis process, and integrated it into a microfluidic sensor chip for in situ electrochemical detection of NO released from living [...] Read more.
In this work, we developed 3D ionic liquid (IL) functionalized graphene assemblies (GAs) decorated by ultrafine RuCu alloy nanoparticles (RuCu-ANPs) via a one-step synthesis process, and integrated it into a microfluidic sensor chip for in situ electrochemical detection of NO released from living cells. Our findings have demonstrated that RuCu-ANPs on 3D IL-GA exhibit high density, uniform distribution, lattice-shaped arrangement of atoms, and extremely ultrafine size, and possess high electrocatalytic activity to NO oxidation on the electrode. Meanwhile, the 3D IL-GA with hierarchical porous structures can facilitate the efficient electron/mass transfer at the electrode/electrolyte interface and the cell culture. Moreover, the graft of IL molecules on GA endows it with high hydrophilicity for facile and well-controllable printing on the electrode. Consequently, the resultant electrochemical microfluidic sensor demonstrated excellent sensing performances including fast response time, high sensitivity, good anti-interference ability, high reproducibility, long-term stability, as well as good biocompatibility, which can be used as an on-chip sensing system for cell culture and real-time in situ electrochemical detection of NO released from living cells with accurate and stable characteristics in physiological conditions. Full article
(This article belongs to the Special Issue The 15th Anniversary of Nanomaterials—Women in Nanomaterials)
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<p>Schematic depiction for the synthesis of RuCu-ANPs/IL-GA nanohybrid electrode material and the fabrication of a microfluidic electrochemical cell sensing chip.</p>
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<p>(<b>a</b>) TEM image of GON; (<b>b</b>) dark-field TEM image of IL-GA, inset of (<b>b</b>) is the photograph of IL-GA hydrogel cylinder; (<b>c</b>) SEM images of IL-GA, inset of (<b>c</b>) is the photograph of IL-GA dispersed in aqueous solution to form a homogenous ink; (<b>d</b>) TEM image and (<b>e</b>) dark-field TEM image of RuCu-ANPs/IL-GA. Inset of (<b>d</b>) is the HR-TEM image of RuCu-ANP on IL-GA; (<b>f</b>) AC-STEM image of RuCu-ANPs on IL-GA. (<b>g</b>) EDX elemental mapping images of C, Ru, and Cu and elements over IL-GA.</p>
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<p>(<b>a</b>) XRD pattern of RuCu-ANPs/IL-GA, Ru-NPs/IL-GA, and IL-GA. (<b>b</b>) XPS survey spectrum of RuCu-ANPs/IL-GA. High-resolution XPS spectra of Ru 3p regions in (<b>c</b>) Ru-NPs/IL-GA and (<b>d</b>) RuCu-ANPs/IL-GA.</p>
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<p>(<b>a</b>) CV curves of different electrodes in 0.1 M PBS (PH 7.0) containing 0.5 mM NO, scan rate: 50 mV s<sup>−1</sup>. (<b>b</b>) Amperometric current response of RuCu-ANPs/IL-GA-based sensor to successive addition of NO in PBS at 0.74 V (vs. Ag/AgCl); inset of (<b>b</b>) is the linear dependence of the amperometric current response vs. NO concentration. (<b>c</b>) Amperometric curve to 3.0 mM NO<sub>3</sub><sup>−</sup> and NO<sub>2</sub><sup>−</sup>, and 1.0 mM UA, AA, DA, Glu and 0.3 mM NO. (<b>d</b>) Relative current responses of 0.3 mM NO on the same sensor after being stored for different days; inset of (<b>d</b>) is the relative current responses of ten sensors towards 0.3 mM NO. Error bars represent the standard deviation from six parallel tests.</p>
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<p>(<b>a</b>) Quantitative cell viability results of CCK-8 assay for MCF-7 cells incubated with RuCu-ANPs/IL-GA electrode from 0 to 72 h; inset of (<b>a</b>) is the dark-field fluorescent images of MCF-7 cells after the calcein-AM/PI assay to stain the viable cells green by calcein-AM. (<b>b</b>) Amperometric current responses of the electrochemical sensor to the addition of 5.0 mM L-Arg and L-NAME into the culture medium in the chip containing MCF-7 cells (5 × 10<sup>6</sup> cells mL<sup>−1</sup>) by microfluidic channels.</p>
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15 pages, 911 KiB  
Article
Preclinical Evaluation of a Novel PSMA-Targeted Agent 68Ga-NOTA-GC-PSMA for Prostate Cancer Imaging
by Wenjin Li, Yihui Luo, Yuqi Hua, Qiaoling Shen, Liping Chen, Yu Xu, Haitian Fu and Chunjing Yu
Tomography 2025, 11(3), 29; https://doi.org/10.3390/tomography11030029 - 7 Mar 2025
Viewed by 203
Abstract
Objectives: Prostate-specific membrane antigen (PSMA)-targeted radioligands are promising diagnostic tools for the targeted positron emission tomography (PET) imaging of prostate cancer (PCa). In present work, we aimed to develop a novel PSMA tracer to provide an additional option for prostate cancer diagnosis. Methods: [...] Read more.
Objectives: Prostate-specific membrane antigen (PSMA)-targeted radioligands are promising diagnostic tools for the targeted positron emission tomography (PET) imaging of prostate cancer (PCa). In present work, we aimed to develop a novel PSMA tracer to provide an additional option for prostate cancer diagnosis. Methods: Our team designed a new structure of the PSMA tracer and evaluated it with cellular experiments in vitro to preliminarily verify the targeting and specificity of 68Ga-NOTA-GC-PSMA. PET/CT imaging of PSMA-positive xenograft-bearing models in vivo to further validate the in vivo specificity and targeting of the radiotracer. Pathological tissue sections from prostate cancer patients were compared with pathological immunohistochemistry and pathological tissue staining results by radioautography experiments to assess the targeting-PSMA of 68Ga-NOTA-GC-PSMA on human prostate cancer pathological tissues. Results: The novel tracer showed high hydrophilicity and rapid clearance rate. Specific cell binding and micro-PET imaging experiments showed that 68Ga-NOTA-GC-PSMA displayed a high specific LNCaP tumor cell uptake (1.70% ± 0.13% at 120 min) and tumor-to-muscle (T/M) and tumor-to-kidney (T/K) ratio (13.87 ± 11.20 and 0.20 ± 0.08 at 60 min, respectively). Conclusions: The novel tracer 68Ga-NOTA-GC-PSMA is promising radionuclide imaging of PCa. Full article
(This article belongs to the Section Cancer Imaging)
24 pages, 4217 KiB  
Article
Optimization of Mechanical and Dynamic Properties of Tread Rubber Using Fumed Silica and Hydration Processing
by Qingchen Chu, Xiaolong Tian, Huiguang Bian and Chuansheng Wang
Polymers 2025, 17(6), 714; https://doi.org/10.3390/polym17060714 - 7 Mar 2025
Viewed by 130
Abstract
Fumed silica, a nanomaterial with a high specific surface area, excellent chemical stability, and electrical insulation, serves as an effective filler for rubber compounding. Compared to traditional carbon black, silica (SiO2), the main component of fumed silica, improves the hardness and [...] Read more.
Fumed silica, a nanomaterial with a high specific surface area, excellent chemical stability, and electrical insulation, serves as an effective filler for rubber compounding. Compared to traditional carbon black, silica (SiO2), the main component of fumed silica, improves the hardness and tear resistance of tread rubber, making it a viable substitute in some formulations. However, silica-filled compounds generally exhibit lower tensile properties and abrasion resistance than carbon black. Fumed silica, with its higher structural integrity, provides additional reinforcement points within natural rubber matrices, enhancing tensile strength and abrasion resistance. Studies demonstrate that replacing carbon black with an equivalent amount of fumed silica as the primary filler significantly improves tread rubber’s hardness (by 20%) and 300% tensile modulus (by 14%) while also reducing rolling resistance and enhancing wet skid performance. Fumed silica’s large specific surface area and low density (10–15% of conventional silica) make it challenging to use directly as a tread rubber filler due to dust formation and prolonged mixing times. This study developed a process combining fumed silica with deionized water, followed by drying and ball milling. This treatment reduces the material’s volume, forming a cohesive gel that, upon processing, minimizes dust and significantly decreases mixing time and difficulty. The interaction between the hydroxyl (–OH) groups on the surface of fumed silica and water molecules likely results in hydrated silica. This interaction enhances surface polarity and forms a hydration layer, improving the hydrophilicity and dispersion of fumed silica in rubber matrices. This reduces the shear modulus difference (ΔG′) between low and high strain, maintaining a consistent elastic modulus over a wide strain range. Such stability enables rubber to perform better under dynamic loads or in complex working conditions. The experimental results demonstrate that the hydration–ball milling process enhances the tensile strength of vulcanizates, improves the dispersion of fumed silica in rubber, strengthens the filler network, boosts dynamic performance, and enhances the wet skid resistance of tread rubber. Full article
(This article belongs to the Section Polymer Processing and Engineering)
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<p>Pretreatment process of fumed silica.</p>
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<p>Experimental processes and testing procedures.</p>
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<p>Hardness of the hybrid rubber.</p>
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<p>The 100% and 300% constant tensile stress of the hybrid rubber.</p>
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<p>Tensile strength of the hybrid rubber.</p>
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<p>Elongation at break of the hybrid rubber.</p>
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<p>Resilience of the hybrid rubber.</p>
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<p>Abrasion resistance of the hybrid rubber.</p>
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<p>G′-strain curve of the hybrid rubber.</p>
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<p>ΔG′ energy storage modulus difference in the compounds.</p>
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<p>SEM micrographs of cross-sections of vulcanized rubber (10 k magnification); (<b>a</b>) N326 carbon black as the main filling material, (<b>b</b>) 1165MP silica as the main filling material, (<b>c</b>) fumed silica as the main filling material, and (<b>d</b>) Sample A as the main filling material.</p>
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<p>SEM micrographs of cross-sections of vulcanized rubber (10 k magnification); (<b>a</b>) N326 carbon black as the main filling material, (<b>b</b>) 1165MP silica as the main filling material, (<b>c</b>) fumed silica as the main filling material, and (<b>d</b>) Sample A as the main filling material.</p>
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<p>Tan δ–temperature curves of compounds.</p>
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11 pages, 4011 KiB  
Article
Enhancing the Properties of Sodium Alginate with a Glycerol–Silicate Plasticizer
by Anthony Fasulo, Corradina Towie, Lucie Mouchiroud, Hamza Malik, Daniel Foucher and Guerino Sacripante
Polysaccharides 2025, 6(1), 20; https://doi.org/10.3390/polysaccharides6010020 - 7 Mar 2025
Viewed by 146
Abstract
The impact of a glycerol–silicate (GS) plasticizer on the mechanical, thermal and hydrophobic properties pertaining to sodium alginate (NaAlg) and calcium alginate (CaAlg) films were investigated. Spectroscopic and physio-chemical analysis were conducted to evaluate the effects of the GS incorporation. The results determine [...] Read more.
The impact of a glycerol–silicate (GS) plasticizer on the mechanical, thermal and hydrophobic properties pertaining to sodium alginate (NaAlg) and calcium alginate (CaAlg) films were investigated. Spectroscopic and physio-chemical analysis were conducted to evaluate the effects of the GS incorporation. The results determine that both NaAlg and CaAlg films exhibited poor mechanical properties which only improved by increasing the GS loading (up to 25 wt%), after which it declined. CaAlg exhibited the highest tensile strength after 25 wt% GS loading was incorporated. The elongation at break varied, with NaAlg films showing a ~10-fold increase, while the CaAlg films remained relatively unchanged. Thermal gravimetric analysis (TGA) revealed that GS reduced the onset decomposition temperature of NaAlg films, whereas CaAlg films maintained a greater onset decomposition temperature. The advancing contact angle measurements indicated a nearly linear decrease (from 54° to 39°) in hydrophobicity for the NaAlg films while the hydrophobicity for CaAlg films initially increased from 65° to 74°, and then became more hydrophilic with greater GS loading. These findings highlight the potential of GS plasticization to enhance and tailor alginate film properties, providing insights into the development of sustainable bioplastics with improved mechanical properties. Full article
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Graphical abstract
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<p>(<b>a</b>) Visual morphology of the GS 5.0–35% (Na<sup>+</sup>) films and (<b>b</b>) the GS 5.0–35% (Ca<sup>2+</sup>) films.</p>
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<p>FTIR spectra of (<b>a</b>) the glycerol−silicate precursor, (<b>b</b>) films for the sodium alginate complex (NaAlg, GS 5.0%, GS 25%) and (<b>c</b>) films from the calcium complex (CaAlg, GS 5.0%, GS 25%).</p>
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<p>Comparative data of (<b>a</b>) tensile strength (MPa) and (<b>b</b>) elongation (%) for the NaAlg and CaAlg complexes.</p>
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<p>Weight loss (%) of (<b>a</b>) NaAlg plasticization complex and (<b>b</b>) CaAlg plasticization complex.</p>
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<p>Contact angle measurements for (<b>a</b>) NaAlg materials and (<b>b</b>) CaAlg materials with varying GS plasticizer concentrations.</p>
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<p>Reaction Scheme (<b>a</b>): A reaction involving a glycerol–silicate plasticizer and sodium alginate (NaAlg). Reaction Scheme (<b>b</b>): Plasticization of sodium alginate with glycerol–silicate immersed in 1 wt% CaCl<sub>2</sub>.</p>
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18 pages, 8753 KiB  
Article
Enhanced Protein Separation Performance of Cellulose Acetate Membranes Modified with Covalent Organic Frameworks
by Shurui Shao, Maoyu Liu, Baifu Tao, Kayode Hassan Lasisi, Wenqiao Meng, Xing Wu and Kaisong Zhang
Membranes 2025, 15(3), 84; https://doi.org/10.3390/membranes15030084 - 6 Mar 2025
Viewed by 151
Abstract
As a porous crystalline material, covalent organic frameworks (COFs) have attracted significant attention due to their extraordinary features, such as an ordered pore structure and excellent stability. Synthesized through the aldehyde amine condensation reaction, TpPa-1 COFs (Triformylphloroglucinol-p-Phenylenediamine-1 COFs) were blended with cellulose acetate [...] Read more.
As a porous crystalline material, covalent organic frameworks (COFs) have attracted significant attention due to their extraordinary features, such as an ordered pore structure and excellent stability. Synthesized through the aldehyde amine condensation reaction, TpPa-1 COFs (Triformylphloroglucinol-p-Phenylenediamine-1 COFs) were blended with cellulose acetate (CA) to form a casting solution. The TpPa-1 COF/CA ultrafiltration membrane was then prepared using the non-solvent-induced phase inversion (NIPS) method. The influence of TpPa-1 COFs content on the hydrophilicity, stability and filtration performance of the modified membrane was studied. Due to the hydrophilic groups in TpPa-1 COFs and the network structure formed by covalent bonds, the modified CA membranes exhibited higher hydrophilicity and lower protein adsorption compared with the pristine CA membrane. The porous crystalline structure of TpPa-1 COFs increased the water permeation path in the CA membrane, improving the permeability of the modified membrane while maintaining an outstanding bovine serum albumin (BSA) rejection. Furthermore, the addition of TpPa-1 COFs reduced protein adsorption on the CA membrane and overcame the trade-off between permeability and selectivity in CA membrane bioseparation applications. This approach provides a sustainable method for enhancing membrane performance while enhancing the application of membranes in protein purification. Full article
(This article belongs to the Special Issue Membrane Separation and Water Treatment: Modeling and Application)
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<p>The synthetic schematic diagram of TpPa-1 COFs (<b>A</b>) and preparation process of TpPa-1 COF/CA membranes (<b>B</b>).</p>
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<p>Characterization of TpPa-1 COFs: (<b>A</b>) FE-SEM and EDS; (<b>B</b>) FTIR; (<b>C</b>–<b>E</b>) XPS and the detailed spectral analysis of XPS; (<b>F</b>) XRD; (<b>G</b>) the particle size distribution.</p>
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<p>The SEM images of prepared membranes. (Red squares and straight lines represent the position of the third column of pictures in the membranes).</p>
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<p>The AFM images of prepared membranes.</p>
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<p>The water contact angle of the prepared membranes.</p>
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<p>The thermogravimetric analysis and derivative thermogravimetry of M0–M5.</p>
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<p>(<b>A</b>) The pure water flux of M0–M5; (<b>B</b>) the flux and protein rejection of M0–M5; (<b>C</b>) the molecular weight cut-off of M0–M5; (<b>D</b>) the anti-fouling performance of M0 and M3.</p>
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<p>(<b>A</b>–<b>D</b>) The fluorescence images of the membrane surfaces; (<b>E</b>,<b>F</b>) simulation system for BSA adsorption of membranes without and with TpPa-1 COFs: BSA molecule, yellow; C, gray; O, red; N, blue; H, white; (<b>G</b>) the protein adsorption mass of membranes; (<b>H</b>) the interaction energy between membranes and BSA; (<b>I</b>) the comparison of TpPa-1 COF/CA membranes and other CA membranes.</p>
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<p>(<b>A</b>–<b>D</b>) The fluorescence images of the membrane surfaces; (<b>E</b>,<b>F</b>) simulation system for BSA adsorption of membranes without and with TpPa-1 COFs: BSA molecule, yellow; C, gray; O, red; N, blue; H, white; (<b>G</b>) the protein adsorption mass of membranes; (<b>H</b>) the interaction energy between membranes and BSA; (<b>I</b>) the comparison of TpPa-1 COF/CA membranes and other CA membranes.</p>
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16 pages, 12999 KiB  
Article
One-Pot Synthesis of Amphiphilic Linear and Hyperbranched Polyelectrolytes and Their Stimuli-Responsive Self-Assembly in Aqueous Solutions
by Angelica Maria Gerardos, Aleksander Forys, Barbara Trzebicka and Stergios Pispas
Polymers 2025, 17(5), 701; https://doi.org/10.3390/polym17050701 - 6 Mar 2025
Viewed by 117
Abstract
Stimuli-responsive polymeric nanostructures are compelling vectors for a wide range of application opportunities. The objective we sought was to broaden the array of self-assembling amphiphilic copolymers with stimuli-responsive characteristics by introducing a hydrophilic tunable monomer, (2-dimethylamino)ethyl methacrylate (DMAEMA), together with a hydrophilic one, [...] Read more.
Stimuli-responsive polymeric nanostructures are compelling vectors for a wide range of application opportunities. The objective we sought was to broaden the array of self-assembling amphiphilic copolymers with stimuli-responsive characteristics by introducing a hydrophilic tunable monomer, (2-dimethylamino)ethyl methacrylate (DMAEMA), together with a hydrophilic one, lauryl methacrylate (LMA), within linear and branched copolymer topologies. Size exclusion chromatography was used to evaluate the resultant linear and hyperbranched copolymers’ molecular weight and dispersity, and FT-IR and 1H-NMR spectroscopy techniques were used to delineate their chemical structure. The structural changes in the obtained self-organized supramolecular structures were thoroughly investigated using aqueous media with varying pH and salinity by dynamic light scattering (DLS), fluorescence spectroscopy (FS), and transmission electron microscopy (TEM). The nanoscale assemblies formed by the amphiphiles indicate significant potential for applications within the field of nanotechnology. Full article
(This article belongs to the Special Issue Advances and Applications of Block Copolymers II)
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<p>Synthesis route of hyperbranched H-P(LMA-co-DMAEMA) copolymer.</p>
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<p>SEC curves of the hyperbranched (<b>a</b>) and linear (<b>b</b>) LMA/DMAEMA copolymers.</p>
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<p><sup>1</sup>H-NMR spectrum of P2 in CDCl<sub>3</sub>. Letters above the spectra peaks correspond to the relevant H nuclei shown in the chemical structure of the copolymer in the inset.</p>
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<p>ATR-FTIR spectra of the hyperbranched copolymers (in the solid state).</p>
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<p>DLS size distributions for P1 (<b>a</b>) and P2 (<b>b</b>) linear copolymer aqueous solutions, C<sub>polymer</sub> = 10<sup>−3</sup> g/mL.</p>
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<p>DLS size distributions for H1 (<b>a</b>) and H2 (<b>b</b>) hyperbranched copolymer aqueous solutions.</p>
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<p>Collective DLS data as a function of salinity. (<b>a</b>) P1 and (<b>b</b>) P2 linear copolymers, C<sub>polymer</sub> = 10<sup>−3</sup> g/mL, pH = 7.</p>
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<p>Collective DLS data as a function of salinity. (<b>a</b>) H1 and (<b>b</b>) H2 hyperbranched copolymers, C<sub>polymer</sub> = 10<sup>−3</sup> g/mL, pH = 7.</p>
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<p>I<sub>1</sub>/I<sub>3</sub> vs. polymer concentration plots for CAC determination regarding (<b>a</b>) P1 and (<b>b</b>) P2 copolymer aqueous solutions, C<sub>pyrene</sub> = 1 μM. (Green lines refer to the two tangent lines described in the text).</p>
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<p>I<sub>1</sub>/I<sub>3</sub> vs. polymer concentration plots for CAC determination regarding (<b>a</b>) H1 and (<b>b</b>) H2 copolymer aqueous solutions. (Green lines refer to the two tangent lines described in the text).</p>
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<p>TEM images from (<b>a</b>) P1 and (<b>b</b>) P2 copolymer solutions.</p>
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<p>TEM images from (<b>a</b>) H1 and (<b>b</b>) H2 copolymer solutions.</p>
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16 pages, 3369 KiB  
Article
Few-Layer Graphene-Based Optical Nanobiosensors for the Early-Stage Detection of Ovarian Cancer Using Liquid Biopsy and an Active Learning Strategy
by Obdulia Covarrubias-Zambrano, Deepesh Agarwal, Joan Lewis-Wambi, Raul Neri, Andrea Jewell, Balasubramaniam Natarajan and Stefan H. Bossmann
Cells 2025, 14(5), 375; https://doi.org/10.3390/cells14050375 - 4 Mar 2025
Viewed by 232
Abstract
Ovarian cancer survival depends strongly on the time of diagnosis. Detection at stage 1 must be the goal of liquid biopsies for ovarian cancer detection. We report the development and validation of graphene-based optical nanobiosensors (G-NBSs) that quantify the activities of a panel [...] Read more.
Ovarian cancer survival depends strongly on the time of diagnosis. Detection at stage 1 must be the goal of liquid biopsies for ovarian cancer detection. We report the development and validation of graphene-based optical nanobiosensors (G-NBSs) that quantify the activities of a panel of proteases, which were selected to provide a crowd response that is specific for ovarian cancer. These G-NBSs consist of few-layer explosion graphene featuring a hydrophilic coating, which is linked to fluorescently labeled highly selective consensus sequences for the proteases of interest, as well as a fluorescent dye. The panel of G-NBSs showed statistically significant differences in protease activities when comparing localized (early-stage) ovarian cancer with both metastatic (late-stage) and healthy control groups. A hierarchical framework integrated with active learning (AL) as a prediction and analysis tool for early-stage detection of ovarian cancer was implemented, which obtained an overall accuracy score of 94.5%, with both a sensitivity and specificity of 0.94. Full article
(This article belongs to the Special Issue Nanofluidics, Nanopores, and Nanomaterials for Understanding Biology)
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<p>(<b>A</b>) Coating of graphene with TEG4amine. (<b>B</b>) Attachment of consensus sequence and attached fluorophore (TCPP). (<b>C</b>) Enzymatic activation of a fluorescence readout.</p>
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<p>(<b>A</b>) Bar graphs and (<b>B</b>) box plots for fluorescence intensity measured for all 6 protease biomarkers in serum samples collected from ovarian cancer (LOC n = 46; MOC n = 50) and healthy control patients (n = 50). The lines shown in the box plots are the maximum and minimum values measured for each dataset analyzed. Each box has 3 lines, going from top to bottom; the 1st line is the 1st quartile, the 2nd is the median line, and the 3rd line is the 3rd quartile.</p>
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<p>Feature relevance scores for samples in (<b>A</b>) healthy, (<b>B</b>) localized ovarian cancer, and (<b>C</b>) metastatic ovarian cancer classes.</p>
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14 pages, 4947 KiB  
Article
Application of Textile Composite Materials as a Sorbent for Cleaning Up Oil Spills
by Daniela Angelova, Desislava Staneva, Daniela Atanasova and Vesislava Toteva
Materials 2025, 18(5), 1146; https://doi.org/10.3390/ma18051146 - 4 Mar 2025
Viewed by 167
Abstract
This article compares two new textile materials used to clean up spills of oil or two oil products (crude oil, diesel fuel, and base oil SN 150). The plain-woven cotton fabric is hydrophilic, with a typical porous structure. After coating with a layer [...] Read more.
This article compares two new textile materials used to clean up spills of oil or two oil products (crude oil, diesel fuel, and base oil SN 150). The plain-woven cotton fabric is hydrophilic, with a typical porous structure. After coating with a layer of chitosan modified with benzaldehyde and cross-linked with glutaraldehyde (CB), its hydrophobicity increases, hence the sorption affinity to hydrophobic hydrocarbons. Including in situ synthesized zinc oxide particles in the hydrophobic chitosan layer (CBZ) changes its structure and increases the sorption capacity. The morphology of the layers was assessed using scanning electron microscopy (SEM) and by comparing the contact angles of the pollutants against the cotton fabric and the composite materials. EDX analysis and mapping for the Zn element show that zinc is homogeneously distributed on the fabric surface. The roughness enhancement and mesoporous structure under the influence of zinc oxide particles were established by the Brunauer Emmett Teller (BET) method and atomic force microscopy (AFM). The advantages of textile composites are their flexibility, stability, and ability to float on the water and wipe up oil spills. It was found that the materials can be successfully regenerated and used repeatedly, making them highly effective because the sorbed crude oil or petroleum products can be separated and utilized. Full article
(This article belongs to the Section Polymeric Materials)
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<p>Schematic representation of the CB and CBZ sorbent materials’ preparation.</p>
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<p>SEM micrographs of (<b>A</b>) cotton fabric; (<b>B</b>) CB fabric; (<b>C</b>) CBZ fabric.</p>
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<p>EDX analysis, EDX mapping for Zn element distribution and SEM micrographs of CBZ (<b>A</b>) on the yarn surface and (<b>B</b>) in the void space between the yarns.</p>
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<p>SEM images at 10.00k× magnification and AFM 2D and 3D images of (<b>A</b>) cotton fibers; (<b>B</b>) CB fibers; (<b>C</b>) CBZ fibers.</p>
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<p>Nitrogen adsorption/desorption isotherms of the cotton fabric CO and CB and CBZ samples.</p>
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<p>Water sorption capacity of the cotton fabric CO and samples CB and CBZ.</p>
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<p>Sorption capacity of the CB and CBZ samples.</p>
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<p>Regenerability of CBZ material.</p>
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16 pages, 6337 KiB  
Article
Preparation of Crown Ether-Containing Polyamide Membranes via Interfacial Polymerization and Their Desalination Performance
by Liqing Xing, Liping Lin, Jiaxin Guo, Xinping He and Chunhai Yi
Membranes 2025, 15(3), 77; https://doi.org/10.3390/membranes15030077 - 3 Mar 2025
Viewed by 262
Abstract
The large-scale application of aromatic polyamide (PA) thin-film composite (TFC) membranes for reverse osmosis has provided an effective way to address worldwide water scarcity. However, the water permeability and salt rejection capabilities of the PA membrane remain limited. In this work, cyclic micropores [...] Read more.
The large-scale application of aromatic polyamide (PA) thin-film composite (TFC) membranes for reverse osmosis has provided an effective way to address worldwide water scarcity. However, the water permeability and salt rejection capabilities of the PA membrane remain limited. In this work, cyclic micropores based on crown ether were introduced into the PA layer using a layer-by-layer interfacial polymerization (LbL-IP) method. After interfacial polymerization between m-phenylenediamine (MPD) and trimesoyl chloride (TMC), the di(aminobenzo)-18-crown-6 (DAB18C6) solution in methanol was poured on the membrane to react with the residual TMC. The cyclic micropores of DAB18C6 provided the membrane with rapid water transport channels and improved ion rejection due to its hydrophilicity and size sieving effect. The membranes were characterized by FTIR, XPS, SEM, and AFM. Compared to unmodified membranes, the water contact angle decreased from 54.1° to 31.6° indicating better hydrophilicity. Moreover, the crown ether-modified membrane exhibited both higher permeability and enhanced rejection performance. The permeability of the crown ether-modified membrane was more than ten times higher than unmodified membranes with a rejection above 95% for Na2SO4, MgSO4, MgCl2, and NaCl solution. These results highlight the potential of this straightforward surface grafting strategy and the modified membranes for advanced water treatment technologies, particularly in addressing seawater desalination challenges. Full article
(This article belongs to the Section Membrane Fabrication and Characterization)
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<p>Different crown ether structures and their hydration radii.</p>
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<p>The synthesis of diamino-dibenzo-18-crown-6.</p>
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<p>Schematic diagram of membranes preparation.</p>
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<p>Diagram of the Testing Device.</p>
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<p>Nuclear magnetic resonance spectra of crown ethers. (<b>a</b>) Nuclear magnetic resonance spectra of DNB18C6. (<b>b</b>) Nuclear magnetic resonance spectra of DAB18C6.</p>
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<p>ATR-FTIR spectra of membrane M0 (base membrane), membrane M1 (PA membrane), and membrane M2 (diamino crown ether-modified membrane).</p>
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<p>XPS spectra of C 1s, N 1s, and O 1s for M1 and M2.</p>
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<p>The surface images of membranes evaluated by SEM and AFM.</p>
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<p>Water contact angle of membranes M0, M1, and M2.</p>
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<p>Performance with different salt solutions.</p>
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<p>Performance under varying pressures.</p>
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<p>Performance with different concentrations.</p>
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<p>Stability performance test.</p>
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20 pages, 20557 KiB  
Article
Effect of Droplet Contamination on Camera Lens Surfaces: Degradation of Image Quality and Object Detection Performance
by Hyunwoo Kim, Yoseph Yang, Youngkwang Kim, Dong-Won Jang, Dongil Choi, Kang Park, Sangkug Chung and Daegeun Kim
Appl. Sci. 2025, 15(5), 2690; https://doi.org/10.3390/app15052690 - 3 Mar 2025
Viewed by 325
Abstract
Recently, camera sensors have been widely used in a variety of applications, including advanced driver assistance systems (ADASs), surveillance systems, and unmanned aerial vehicles (UAVs). These sensors are often integrated with intelligent algorithms to automatically analyze information and perform specific functions. However, during [...] Read more.
Recently, camera sensors have been widely used in a variety of applications, including advanced driver assistance systems (ADASs), surveillance systems, and unmanned aerial vehicles (UAVs). These sensors are often integrated with intelligent algorithms to automatically analyze information and perform specific functions. However, during rainy weather, droplets on the camera lens surface can obstruct the view, leading to degraded image quality and reduced algorithm performance. This paper quantitatively evaluates the effect of droplet contamination on image quality and object detection performance. Image quality degradation was analyzed using the modulation transfer function (MTF), with droplet volume and number as variables. Results show that the MTF50 decreased by up to 80% when the droplet volume reached 10 μL. To assess the effect on object detection, performance changes were evaluated across different detection algorithms. The findings reveal that droplet contamination can reduce the detection performance of small objects by up to 90%, as measured by the mean average precision (mAP) metric. Furthermore, degradation was more severe on hydrophilic surfaces compared to hydrophobic ones. This study demonstrates that droplet characteristics such as volume, number, and shape significantly influence both image quality and object detection performance. It provides critical insights into selecting appropriate camera lens materials by comparing hydrophilic and hydrophobic surfaces while also highlighting the susceptibility of intelligent algorithms to environmental factors and underscoring the importance of effective cleaning techniques. Full article
(This article belongs to the Section Computing and Artificial Intelligence)
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<p>Image quality degradation by droplet contamination on the camera lens surface.</p>
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<p>Experimental setup for analyzing image degradation from droplet contamination using a slanted-edge target: (<b>a</b>) Configuration of the MTF measurement apparatus; two contamination methods for the camera cover glass: (<b>b</b>) single droplet contamination and (<b>c</b>) multiple droplet contamination.</p>
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<p>Side view of droplet on the cover glass parallel to the ground: (<b>a</b>) hydrophobic surface; and (<b>b</b>) hydrophilic surface.</p>
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<p>Image of a slanted-edge target with (<b>a</b>) clean cover glass; (<b>b</b>) hydrophobic cover glass; (<b>c</b>) hydrophilic cover glass, each contaminated by single droplet of varying volumes (1, 3, 5, and 10 μL); and (<b>d</b>) MTF50<sub>loss</sub> due to single droplet contamination.</p>
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<p>(<b>a</b>) Image capture setup for measuring droplet contamination area; images of cover glass surface for each contamination level with different spray volumes (0.1, 0.5, and 1.0 mL) on (<b>b</b>) hydrophobic and (<b>c</b>) hydrophilic surfaces.</p>
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<p>Contamination area measurement process: (<b>a</b>) Real image with droplets on the cover glass surface. (<b>b</b>) Convert color image to 8-bit grayscale; (<b>c</b>) Highlight the boundaries of droplets using the threshold function. (<b>d</b>) Find the edge of the droplets. (<b>e</b>) Fill the area within the edge of the droplets with white color. (<b>f</b>) Measure the droplet area over the total area of the glass.</p>
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<p>Contamination area measurement results on hydrophobic and hydrophilic cover glass under different contamination levels.</p>
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<p>Slanted-edge target images taken at each contamination level (slight, moderate, severe) with (<b>a</b>) hydrophobic cover glass and (<b>b</b>) hydrophilic cover glass; (<b>c</b>) MTF50<sub>loss</sub> caused by multiple droplet contamination. Note that the minimum MTF50 value observed was 0.005, indicating a significant decrease in image quality due to the contamination.</p>
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<p>(<b>a</b>) Image capture setup for acquiring the object detection performance evaluation dataset. (<b>b</b>) Object detection performance evaluation process: (<b>b1</b>) The preparation of droplet-contaminated and clean datasets. (<b>b2</b>) Inference of the collected dataset with object detection model. (<b>b3</b>) Calculation of the mAP based on the precision–recall curve.</p>
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<p>Images for assessing the effects of single droplet contamination, with droplet volumes (1, 3, 5, and 10 µL) and object sizes (XL, L, M, S, and XS) as variables on (<b>a</b>) hydrophobic and (<b>b</b>) hydrophilic cover glass.</p>
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<p>Object detection performance evaluation results with five different object sizes and droplet volume on hydrophobic and hydrophilic cover glass: (<b>a</b>) mAP for person class; and (<b>b</b>) mAP<sub>loss</sub>, representing the difference between the mAP<sub>clean</sub> and mAP<sub>contamination</sub>.</p>
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<p>Images for evaluating object detection performance degradation on camera sensors resulting from multiple droplet contamination on hydrophobic and hydrophilic surfaces, with contamination levels as follows: (<b>a</b>) clean; (<b>b</b>) slight; (<b>c</b>) moderate; and (<b>d</b>) severe.</p>
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<p>The mAP<sub>loss</sub> caused by multiple droplet contamination for various object detection algorithms: (<b>a</b>) RTMDet; (<b>b</b>) YOLOv8x; (<b>c</b>) DetectoRS; and (<b>d</b>) DINO.</p>
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24 pages, 4800 KiB  
Article
The Role of Natural Deep Eutectic Solvents in a Hydrogel Formulation Containing Lidocaine
by Feria Hasanpour, Mária Budai-Szűcs, Anita Kovács, Rita Ambrus, Orsolya Jójárt-Laczkovich, Boglárka Szalai, Branimir Pavlić, Péter Simon, Levente Törteli and Szilvia Berkó
Pharmaceutics 2025, 17(3), 324; https://doi.org/10.3390/pharmaceutics17030324 - 2 Mar 2025
Viewed by 311
Abstract
Background/Objectives: This study investigates the use of natural deep eutectic solvents (NADESs) in enhancing the solubility and skin permeation of a lidocaine base, a lipophilic form, in hydrogel systems. The aim was to develop an environmentally sustainable and biocompatible alternative to conventional [...] Read more.
Background/Objectives: This study investigates the use of natural deep eutectic solvents (NADESs) in enhancing the solubility and skin permeation of a lidocaine base, a lipophilic form, in hydrogel systems. The aim was to develop an environmentally sustainable and biocompatible alternative to conventional lidocaine formulations, improving the dermal permeation and therapeutic efficacy. Methods: The lidocaine base was dissolved in a hydrophilic NADES system composed of choline chloride and citric acid, facilitating enhanced solubility, likely through new molecular interactions. Then, pH-adjusted hydrogels were formulated and optimized by employing a 32 full factorial design. Raman and nuclear magnetic resonance (NMR) spectroscopy were applied to evaluate the stability of lidocaine in the optimal formulation. The biopharmaceutical properties were investigated using in vitro drug release and skin permeation studies. In vivo tests assessed physiological skin parameters such as the hydration and transepidermal water loss. Results: The developed NADES-containing hydrogel significantly improved the solubility and stability of lidocaine. Skin permeation studies demonstrated enhanced dermal permeation compared with conventional hydrogel and ointment. These improvements, namely the enhanced solubility of lidocaine in the formulation and its increased permeation, were attributed to the dual effect of the NADES. Conclusions: NADES-containing hydrogels represent a promising green technology for formulating lidocaine-containing dermal preparations. This approach offers a biocompatible, natural-based alternative that can enhance the bioavailability and efficacy of topical anesthetics. Full article
(This article belongs to the Special Issue Transdermal Delivery: Challenges and Opportunities)
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<p>Illustration of the preparation process for lidocaine-loaded NADES-containing hydrogel. The image of the preparation was created with <a href="http://Biorender.com" target="_blank">Biorender.com</a>.</p>
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<p>Flow curves of the hydrogel formulations of the DoE with varying concentrations of NADES and sodium citrate: (<b>a</b>) fixed 10 <span class="html-italic">w</span>/<span class="html-italic">w</span>% NADES with 8 and 13 <span class="html-italic">w</span>/<span class="html-italic">w</span>% sodium citrate; (<b>b</b>) constant 15 <span class="html-italic">w</span>/<span class="html-italic">w</span>% NADES with 8, 13, and 18 <span class="html-italic">w</span>/<span class="html-italic">w</span>% sodium citrate; and (<b>c</b>) fixed 20 <span class="html-italic">w</span>/<span class="html-italic">w</span>% NADES with 8, 13, and 18 <span class="html-italic">w</span>/<span class="html-italic">w</span>% sodium citrate.</p>
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<p>Effect of the sodium citrate and NADES concentrations on the pH (<b>a</b>) and viscosity (<b>b</b>) of the formulations.</p>
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<p>XRD diffractogram showing the crystalline profiles of raw lidocaine, sodium citrate (Na Citrate), hydroxyethyl cellulose (HEC), and Hydrogel NADES.</p>
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<p>Raman spectra of NADES(S7) compared with the spectra of NADES(S7) + lidocaine and pure lidocaine.</p>
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<p><sup>1</sup>H NMR spectrum of (<b>a</b>) lidocaine base, (<b>b</b>) lidocaine hydrochloride, (<b>c</b>) NADES(S7), and (<b>d</b>) 2,6-dimethylaniline in DMSO-<span class="html-italic">d</span><sub>6</sub>.</p>
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<p><sup>1</sup>H-NMR spectra and chemical shifts of the lidocaine-containing samples (<b>a</b>) NADES(S7) and lidocaine, and (<b>b</b>) NADES(S7) and lidocaine buffered with sodium citrate compared to both the lidocaine base and hydrochloride.</p>
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<p>In vitro release profile of the cumulative amount of Hydrogel NADES compared with Hydrogel Ref and Ointment Ref (*** <span class="html-italic">p</span> &lt; 0.001 vs. Hydrogel NADES).</p>
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<p>In vitro permeation test of the cumulative plot of the Hydrogel NADES compared with the Ointment Ref and Hydrogel Ref formulations (** <span class="html-italic">p</span> &lt; 0.01 vs. Hydrogel NADES).</p>
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<p>Hydration effect of the preparations (* <span class="html-italic">p</span> &lt; 0.05, *** <span class="html-italic">p</span> &lt; 0.001 vs. Hydrogel NADES at each measurement time).</p>
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<p>Effect of the preparations on the transepidermal water loss (TEWL) (* <span class="html-italic">p</span> &lt; 0.05, ** <span class="html-italic">p</span> &lt; 0.01, *** <span class="html-italic">p</span> &lt; 0.001 vs. Hydrogel NADES at each measurement time).</p>
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16 pages, 2594 KiB  
Article
A Highly Hydrophobic Siloxane-Nanolignin Coating for the Protection of Wood
by Mariana M. M. Ramos, Christina P. Pappa, Panagiotis N. Manoudis, Vasiliki Kamperidou, Eleni Pavlidou, Vasilios Tsiridis, Maria Petala, Konstantinos S. Triantafyllidis, Panagiotis K. Spathis and Ioannis Karapanagiotis
Coatings 2025, 15(3), 293; https://doi.org/10.3390/coatings15030293 - 2 Mar 2025
Viewed by 332
Abstract
Wood, a vital material for both modern and heritage objects, is particularly susceptible to degradation caused by water due to its hydrophilic nature and porous structure. Therefore, developing sustainable strategies to protect wood is of significant importance. This study aims to produce a [...] Read more.
Wood, a vital material for both modern and heritage objects, is particularly susceptible to degradation caused by water due to its hydrophilic nature and porous structure. Therefore, developing sustainable strategies to protect wood is of significant importance. This study aims to produce a highly hydrophobic coating for the protection of wood following a straightforward procedure and using materials that are compatible with wood. First, nano/sub-microlignin (NL) is isolated and produced from beech wood through a one-step tailored organosolv process. Next, NL is incorporated into Sivo 121, a water-borne and solvent-free silane system recommended by the manufacturer for protecting wood surfaces. Composite coatings containing various concentrations of NL and Sivo 121 are applied to chestnut (Castanea spp.) and oak (Quercus spp.). The impact of NL concentration on the contact angles of water drops (CAs) and colour changes (ΔE) of the treated wood specimens is investigated. The coating with 4% w/w NL demonstrates enhanced hydrophobicity (CA = 145°) and has a negligible effect on the colour of pristine oak (ΔE < 3). The wetting properties of coated oak are not affected after 100 tape peeling cycles. However, the coating exhibits poorer performance on chestnut, i.e., CA = 135°, which declines after 80 peeling cycles, and ΔE > 5. The drop pH does not have any noticeable effect on CA. The latter remains stable even after prolonged exposure of coated oak and chestnut samples to artificial UV radiation and outdoor environmental conditions. Finally, the composite coating offers good and comparable protection for both wood species in the biological durability soil burial test Full article
(This article belongs to the Special Issue Superhydrophobic Coatings, 2nd Edition)
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<p>Photographs illustrating the procedure to conduct the biological durability soil burial test. The photographs show (<b>a</b>) the samples placed at a depth of 10 cm and (<b>b</b>) the burial site after covering the samples with soil.</p>
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<p>Contact angle of water drops (CA) on coated chestnut and oak vs. the NL concentration.</p>
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<p>SEM images showing the surface structures of chestnut coated with (<b>a</b>) pure Sivo and (<b>b</b>) Sivo + 4% <span class="html-italic">w</span>/<span class="html-italic">w</span> NL. (<b>c</b>) Pinned drop on chestnut tilted to a perpendicular position and coated with Sivo + 4% <span class="html-italic">w</span>/<span class="html-italic">w</span> NL.</p>
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<p>Colour change (<math display="inline"><semantics> <mrow> <mo>Δ</mo> <mi mathvariant="normal">E</mi> </mrow> </semantics></math>) in the coated wood samples vs. the NL concentration. The colours of the wood samples changed due to the application of the coatings.</p>
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<p>Results of the test of water absorption by capillarity: amount of water absorbed per unit area vs. treatment time for uncoated woods, woods coated with Sivo, and woods coated with the selected composite (Sivo + 4.0% <span class="html-italic">w</span>/<span class="html-italic">w</span> NL). Results for (<b>a</b>) chestnut and (<b>b</b>) oak samples are shown.</p>
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<p>(<b>a</b>,<b>b</b>) Results of the biological durability soil burial test: mass loss (%) vs. the time wood samples remained buried in the soil. Results for uncoated woods, woods coated with Sivo, and woods coated with the selected composite (Sivo + 4.0% <span class="html-italic">w</span>/<span class="html-italic">w</span> NL) are shown. The two photographs show oak specimens (<b>c</b>) before and (<b>d</b>) after the test.</p>
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<p>CA vs. the pH of drops on woods coated with Sivo and woods coated with the selected composite (Sivo + 4.0% <span class="html-italic">w</span>/<span class="html-italic">w</span> NL). Results for (<b>a</b>) chestnut and (<b>b</b>) oak samples are shown. Photographs of drops on chestnut coated with the composite material are included in (<b>a</b>).</p>
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<p>Results of the tape peeling test: CA vs. peeling cycles on woods coated with Sivo and woods coated with the selected composite (Sivo + 4.0% <span class="html-italic">w</span>/<span class="html-italic">w</span> NL). Results for (<b>a</b>) chestnut and (<b>b</b>) oak samples are shown. The figure includes photographs of water drops on wood surfaces coated with the composite material, captured before testing (0 cycles) and after 100 peeling cycles.</p>
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<p>CA vs. exposure time for wood samples kept (<b>a</b>,<b>b</b>) outdoors and (<b>c</b>,<b>d</b>) within the UV chamber. Results for wood samples coated with Sivo and wood samples coated with the selected composite (Sivo + 4.0% <span class="html-italic">w</span>/<span class="html-italic">w</span> NL) are shown.</p>
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16 pages, 4460 KiB  
Article
Tailoring the Performance of a Composite PEI Nanofiltration Membrane via Incorporating Activated PDA for Efficient Dye Sieving and Salt Separation
by Wanting Li, Jiaye Liu, Weifu Wang, Shichun Chen, Fengwei Jia, Xiang Li, Ying Zhao, Wenjuan Zhang, Dan Song and Jun Ma
Membranes 2025, 15(3), 75; https://doi.org/10.3390/membranes15030075 - 2 Mar 2025
Viewed by 355
Abstract
Efficient dye sieving and salt separation can facilitate the recycling of valuable resources in textile wastewater treatment. This study focuses on developing a high-performance nanofiltration membrane (NF) by co-depositing activated polydopamine (O-PDA), oxidized with KMnO4, and polyethyleneimine (PEI) onto a polysulfone [...] Read more.
Efficient dye sieving and salt separation can facilitate the recycling of valuable resources in textile wastewater treatment. This study focuses on developing a high-performance nanofiltration membrane (NF) by co-depositing activated polydopamine (O-PDA), oxidized with KMnO4, and polyethyleneimine (PEI) onto a polysulfone support membrane (PSF), thereby enabling effective dye sieving and salt separation. Due to the high hydrophilicity of PDA and the formation of high molecular polymers after oxidation, it was anticipated that O-PDA would crosslink the PEI layer, providing rapid permeating channels. Filtration experiments demonstrated that the formation of O-PDA significantly enhanced the salt retention rate of nanofiltration membranes, achieving a nearly threefold increase in NaCl retention from 15% to 45.7%. It was observed that the retention performance of O-PDA could be adjusted by controlling its loading or oxidation level. Furthermore, despite a notable reduction in permeability, the dye removal efficiency of the O-PDA/PEI membrane increased substantially to 99.5%. Long-term filtration experiments also confirmed both the stability and anti-fouling properties of this membrane design. Clearly, owing to its excellent operational stability and anti-fouling characteristics, the O-PDA/PEI membrane exhibits great potential for applications in dye sieving and salt separation. Full article
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<p>Schematic diagram of the membrane preparation process.</p>
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<p>Schematic diagram of the cross-flow membrane filtration test setup.</p>
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<p>UV-vis absorbance at 357 nm and 420 nm for KMnO<sub>4</sub>-activated DA solutions with varying molar ratios.</p>
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<p>Surface images of the (<b>a</b>) PSf, DE, KD, and KDE8 membranes; (<b>b</b>) surface roughness of the PSf, DE, KD, and KDE8 membranes; and (<b>c</b>) roughness parameters (<span class="html-italic">R<sub>q</sub></span>, <span class="html-italic">R<sub>a</sub></span> and <span class="html-italic">R<sub>p</sub></span>) of the membranes.</p>
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<p>ATR-FTIR spectra of the PSf, KD, and KDE8 membranes.</p>
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<p>(<b>a</b>) XPS spectra overview for the PSf, KD, KDE2, and KDE8 membranes. (<b>b</b>) Elemental distribution on the membrane surfaces pre- and post-modification. High-resolution XPS N1s spectra of the (<b>c</b>) KDE8-C1s and (<b>d</b>) KDE8-N1s.</p>
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<p>The changes in (<b>a</b>) CA and (<b>b</b>) zeta potential on the membrane surface pre- and post-modification.</p>
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<p>(<b>a</b>) Membrane permeability, (<b>b</b>) rejection of salts, and (<b>c</b>) dyes of pre- and post-modification.</p>
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<p>(<b>a</b>) Membrane permeability in two cycles of filtration and (<b>b</b>) the flux recovery of these membranes after BSA fouling cleaning processes.</p>
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24 pages, 5773 KiB  
Article
An Investigation into the Effect of Maltitol, Sorbitol, and Xylitol on the Formation of Carbamazepine Solid Dispersions Through Thermal Processing
by Madan Sai Poka, Marnus Milne, Anita Wessels and Marique Aucamp
Pharmaceutics 2025, 17(3), 321; https://doi.org/10.3390/pharmaceutics17030321 - 2 Mar 2025
Viewed by 208
Abstract
Background: Carbamazepine (CBZ) is a Biopharmaceutical Classification System (BCS) class II drug, that is practically insoluble in water, influencing the oral bioavailability. Polyols are highly hydrophilic crystalline carriers studied for their success in developing solid dispersions (SDs) for improved solubility and dissolution rate. [...] Read more.
Background: Carbamazepine (CBZ) is a Biopharmaceutical Classification System (BCS) class II drug, that is practically insoluble in water, influencing the oral bioavailability. Polyols are highly hydrophilic crystalline carriers studied for their success in developing solid dispersions (SDs) for improved solubility and dissolution rate. Polyols are generally regarded as safe (GRAS) and maltitol (MAL), xylitol (XYL) and sorbitol (SOR) are among the approved polyols for market use. While xylitol (XYL) and sorbitol, have shown promise in improving the solubility and dissolution rates of poorly soluble drugs, their full potential in the context of improving the solubility of carbamazepine have not been thoroughly investigated. To the best of our knowledge, maltitol (MAL) was not studied previously as a carrier for preparing SDs. Hence, the purpose of this study was to investigate their use in the preparation of CBZ SDs by the fusion method. Methods: CBZ-polyol SDs were prepared in varying molar ratios (2:1, 1:1 and 1:2) and characterised for solid-state nature, solubility and in-vitro dissolution rate. Results: Solid-state characterisation of the CBZ-polyol SDs revealed the existence of the SDs as continuous glass suspensions with fine CBZ crystallites suspended in the amorphous polyol carriers. Among the polyols studied, XYL exhibited good miscibility with CBZ and showed significant improvement in the solubility and dissolution rate. The prepared SDs showed a 2 to 6-folds increase in CBZ solubility and 1.4 to 1.9-folds increase in dissolution rate in comparison with pure CBZ. Conclusions: The study explains the possible use of polyols (XYL and SOR) based SDs of BCS Class II drugs with good glass forming ability for enhanced solubility and dissolution. Full article
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<p>Molecular structures of (<b>a</b>) CBZ, (<b>b</b>) MAL, (<b>c</b>) SORB, and (<b>d</b>) XYL.</p>
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<p>Overlay of DSC thermograms obtained for (<b>a</b>) MAL, CBZ, and CBZ-MAL PMs and (<b>b</b>) CBZ-MAL SDs.</p>
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<p>HSM micrographs obtained for the prepared (<b>a</b>) CBZ–MAL(1:1)PM, (<b>b</b>) CBZ–MAL(2:1)SD, (<b>c</b>) CBZ–MAL(1:1)SD, and (<b>d</b>) CBZ–MAL(1:2)SD during heating at 10 °C/min.</p>
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<p>PXRD diffractograms obtained for pure CBZ, MAL (<b>a</b>) and the prepared SDs of CBZ–MAL in the molar ratios of 2:1, 1:1, and 1:2 (<b>b</b>).</p>
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<p>Overlay of the FTIR spectra obtained for (<b>A</b>) CBZ and MAL in comparison with the CBZ–MAL PMs and (<b>B</b>) all CBZ–MAL SDs, with (a) indicating the observed peak broadening in the 3464 cm<sup>−1</sup> and (b) 1674 cm<sup>−1</sup> wavenumber regions and (c) denoting the absorbance band at 760 cm<sup>−1</sup>, considered characteristic of CBZ Form III.</p>
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<p>PXRD diffractogram for CBZ form I crystals formed under isothermal conditions of recrystallisation.</p>
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<p>Overlay of DSC thermograms obtained for (<b>a</b>) SOR, CBZ, and CBZ-SOR PMs and (<b>b</b>) CBZ-SOR SDs.</p>
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<p>HSM micrographs obtained for the prepared CBZ–SOR(1:1)PM (<b>a</b>), CBZ–SOR(2:1)SD (<b>b</b>), CBZ–SOR(1:1)SD (<b>c</b>), and CBZ–SOR(1:2)SD (<b>d</b>) during heating at 10 °C/min.</p>
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<p>PXRD diffractograms obtained for pure SOR and the prepared SDs of CBZ–SOR in the molar ratios of 2:1, 1:1, and 1:2.</p>
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<p>Overlay of the FTIR spectra obtained for CBZ and SOR in comparison with (<b>A</b>) the CBZ–SOR PMs and (<b>B</b>) CBZ–SOR SDs, with (a) indicating the observed peak broadening in the 3464 cm<sup>−1</sup> and (b) 1674 cm<sup>−1</sup> wavenumber regions and (c) denoting the absorbance band at 760 cm<sup>−1</sup>, considered characteristic of CBZ Form III.</p>
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<p>Overlay of DSC thermograms obtained for (<b>a</b>) XYL, CBZ, CBZ-XYL PMs and (<b>b</b>) CBZ-XYL SDs.</p>
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<p>HSM micrographs obtained for the prepared (<b>a</b>) CBZ–XYL(1:1)PM, (<b>b</b>) CBZ–XYL(2:1)SD, (<b>c</b>) CBZ–XYL(1:1)SD, and (<b>d</b>) CBZ–XYL(1:2)SD during heating at 10 °C/min.</p>
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<p>PXRD diffractograms obtained for pure XYL and the prepared SDs of CBZ–XYL in the molar ratios of 2:1, 1:1, and 1:2.</p>
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<p>Overlay of the FTIR spectra obtained for CBZ and XYL in comparison with (<b>A</b>) the CBZ–XYL PMs and (<b>B</b>) CBZ–XYL SDs, with (a) indicating the observed peak broadening in the 3464 cm<sup>−1</sup> and (b) 1674 cm<sup>−1</sup> wavenumber regions and (c) denoting the absorbance band at 760 cm<sup>−1</sup>, considered characteristic of CBZ Form III.</p>
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<p>(<b>a</b>–<b>c</b>)In vitro release profiles of pure CBZ, PMs, and SDs in combination with polyols in varying molecular ratios.</p>
Full article ">Figure 15 Cont.
<p>(<b>a</b>–<b>c</b>)In vitro release profiles of pure CBZ, PMs, and SDs in combination with polyols in varying molecular ratios.</p>
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