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20 pages, 4292 KiB  
Article
A Novel Method for Analysing the Curvature of the Anterior Lens: Multi-Radial Scheimpflug Imaging and Custom Conic Fitting Algorithm
by María Arcas-Carbonell, Elvira Orduna-Hospital, María Mechó-García, Guisela Fernández-Espinosa and Ana Sanchez-Cano
J. Imaging 2025, 11(8), 257; https://doi.org/10.3390/jimaging11080257 (registering DOI) - 1 Aug 2025
Abstract
This study describes and validates a novel method for assessing anterior crystalline lens curvature along vertical and horizontal meridians using radial measurements derived from Scheimpflug imaging. The aim was to evaluate whether pupil diameter (PD), anterior lens curvature, and anterior chamber depth (ACD) [...] Read more.
This study describes and validates a novel method for assessing anterior crystalline lens curvature along vertical and horizontal meridians using radial measurements derived from Scheimpflug imaging. The aim was to evaluate whether pupil diameter (PD), anterior lens curvature, and anterior chamber depth (ACD) change during accommodation and whether these changes are age-dependent. A cross-sectional study was conducted on 104 right eyes from healthy participants aged 21–62 years. Sixteen radial images per eye were acquired using the Galilei Dual Scheimpflug Placido Disk Topographer under four accommodative demands (0, 1, 3, and 5 dioptres (D)). Custom software analysed lens curvature by calculating eccentricity in both meridians. Participants were analysed as a total group and by age subgroups. Accommodative amplitude and monocular accommodative facility were inversely correlated with age. Both PD and ACD significantly decreased with higher accommodative demands and age. Relative eccentricity decreased under accommodation, indicating increased lens curvature, especially in younger participants. Significant curvature changes were detected in the horizontal meridian only, although no statistically significant differences between meridians were found overall. The vertical meridian showed slightly higher eccentricity values, suggesting that it remained less curved. By enabling detailed, meridionally stratified in vivo assessment of anterior lens curvature, this novel method provides a valuable non-invasive approach for characterizing age-related biomechanical changes during accommodation. The resulting insights enhance our understanding of presbyopia progression, particularly regarding the spatial remodelling of the anterior lens surface. Full article
(This article belongs to the Special Issue Current Progress in Medical Image Segmentation)
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18 pages, 3793 KiB  
Review
Research Progress on Vaterite Mineral and Its Synthetic Analogs
by Guoxi Sun, Xiuming Liu, Bin Lian and Shijie Wang
Minerals 2025, 15(8), 796; https://doi.org/10.3390/min15080796 - 29 Jul 2025
Viewed by 193
Abstract
As the most unstable crystalline form of calcium carbonate, vaterite is rarely found in nature due to being highly prone to phase transitions. However, its high specific surface area, excellent biocompatibility, and high solubility properties have led to a research boom and the [...] Read more.
As the most unstable crystalline form of calcium carbonate, vaterite is rarely found in nature due to being highly prone to phase transitions. However, its high specific surface area, excellent biocompatibility, and high solubility properties have led to a research boom and the following breakthroughs in the last two decades: (1) From primitive calculations and spectroscopic analyses to modern multidimensional research methods combining calculations and experiments, the crystal structure of vaterite has turned from early identifications in orthorhombic and hexagonal crystal systems to a complex polymorphic structure within the monoclinic crystal system. (2) The formation process of vaterite not only conforms to the classical crystal growth theory but also encompasses the nanoparticle aggregation theory, which incorporates the concepts of oriented nanoparticle assembly and mesoscale transformation. (3) Regardless of the conditions, the formation of vaterite depends on an excess of CO32− relative to Ca2+, and its stability duration relates to preservation conditions. (4) Vaterite demonstrates significant value in biomedical applications—including bone repair scaffolds, targeted drug carriers, and antibacterial coating materials—leveraging its porous structure, high specific surface area, and exceptional biocompatibility. While it also shows utility in environmental pollutant adsorption and general coating technologies, the current research remains predominantly concentrated on its medical applications. Currently, the rapid transformation of vaterite presents the primary limitation for its industrial application. Future research should prioritize investigating its formation kinetics and stability. Full article
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15 pages, 2865 KiB  
Article
Mitigation of Alkali–Silica Reactivity of Greywacke Aggregate in Concrete for Sustainable Pavements
by Kinga Dziedzic, Aneta Brachaczek, Dominik Nowicki and Michał A. Glinicki
Sustainability 2025, 17(15), 6825; https://doi.org/10.3390/su17156825 - 27 Jul 2025
Viewed by 338
Abstract
Quality requirements for mineral aggregate for concrete used to construct pavement for busy highways are high because of the fatigue traffic loads and environmental exposure. The use of local aggregate for infrastructure projects could result in important sustainability improvements, provided that the concrete’s [...] Read more.
Quality requirements for mineral aggregate for concrete used to construct pavement for busy highways are high because of the fatigue traffic loads and environmental exposure. The use of local aggregate for infrastructure projects could result in important sustainability improvements, provided that the concrete’s durability is assured. The objective of this study was to identify the potential alkaline reactivity of local greywacke aggregate and select appropriate mitigation measures against the alkali–silica reaction. Experimental tests on concrete specimens were performed using the miniature concrete prism test at 60 °C. Mixtures of coarse greywacke aggregate up to 12.5 mm with natural fine aggregate of different potential reactivity were evaluated in respect to the expansion, compressive strength, and elastic modulus of the concrete. Two preventive measures were studied—the use of metakaolin and slag-blended cement. A moderate reactivity potential of the greywacke aggregate was found, and the influence of reactive quartz sand on the expansion and instability of the mechanical properties of concrete was evaluated. Both crystalline and amorphous alkali–silica reaction products were detected in the cracks of the greywacke aggregate. Efficient expansion mitigation was obtained for the replacement of 15% of Portland cement by metakaolin or the use of CEM III/A cement with the slag content of 52%, even if greywacke aggregate was blended with moderately reactive quartz sand. It resulted in a relative reduction in expansion by 85–96%. The elastic modulus deterioration was less than 10%, confirming an increased stability of the elastic properties of concrete. Full article
(This article belongs to the Special Issue Sustainability of Pavement Engineering and Road Materials)
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16 pages, 5151 KiB  
Article
Design and Characterization of Curcumin-Modified Polyurethane Material with Good Mechanical, Shape-Memory, pH-Responsive, and Biocompatible Properties
by Man Wang, Hongying Liu, Wei Zhao, Huafen Wang, Yuwei Zhuang, Jie Yang, Zhaohui Liu, Jing Zhu, Sichong Chen and Jinghui Cheng
Biomolecules 2025, 15(8), 1070; https://doi.org/10.3390/biom15081070 - 24 Jul 2025
Viewed by 208
Abstract
In the context of critical challenges in curcumin-modified polyurethane synthesis—including limited curcumin bioavailability and suboptimal biodegradability/biocompatibility—a novel polyurethane material (Cur-PU) with good mechanical, shape memory, pH-responsive, and biocompatibility was synthesized via a one-pot, two-step synthetic protocol in which HO-PCL-OH served as the soft [...] Read more.
In the context of critical challenges in curcumin-modified polyurethane synthesis—including limited curcumin bioavailability and suboptimal biodegradability/biocompatibility—a novel polyurethane material (Cur-PU) with good mechanical, shape memory, pH-responsive, and biocompatibility was synthesized via a one-pot, two-step synthetic protocol in which HO-PCL-OH served as the soft segment and curcumin was employed as the chain extender. The experimental results demonstrate that with the increase in Cur units, the crystallinity of the Cur-PU material decreases from 32.6% to 5.3% and that the intensities of the diffraction peaks at 2θ = 21.36°, 21.97°, and 23.72° in the XRD pattern gradually diminish. Concomitantly, tensile strength decreased from 35.5 MPa to 19.3 MPa, and Shore A hardness declined from 88 HA to 65 HA. These observations indicate that the sterically hindered benzene ring structure of Cur imposes restrictions on HO-PCL-OH crystallization, leading to lower crystallinity and retarded crystallization kinetics in Cur-PU. As a consequence, the material’s tensile strength and hardness are diminished. Except for the Cur-PU-3 sample, all other variants exhibited exceptional shape-memory functionality, with Rf and Rr exceeding 95%, as determined by three-point bending method. Analogous to pure curcumin solutions, Cur-PU solutions demonstrated pH-responsive chromatic transitions: upon addition of hydroxide ion (OH) solutions at increasing concentrations, the solutions shifted from yellow-green to dark green and finally to orange-yellow, enabling sensitive pH detection across alkaline gradients. Hydrolytic degradation studies conducted over 15 weeks in air, UPW, and pH 6.0/8.0 phosphate buffer solutions revealed mass loss <2% for Cur-PU films. Surface morphological analysis showed progressive etching with the formation of micro-to-nano-scale pores, indicative of a surface-erosion degradation mechanism consistent with pure PCL. Biocompatibility assessments via L929 mouse fibroblast co-culture experiments demonstrated ≥90% cell viability after 72 h, while relative red blood cell hemolysis rates remained below 5%. Collectively, these findings establish Cur-PU as a biocompatible material with tunable mechanical properties, and pH responsiveness, underscoring its translational potential for biomedical applications such as drug delivery systems and tissue engineering scaffolds. Full article
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22 pages, 1375 KiB  
Review
Polymorphic Transformations of Pharmaceutical Materials Induced by Mechanical Milling: A Review
by Mathieu Guerain and Jean-François Willart
Pharmaceutics 2025, 17(7), 946; https://doi.org/10.3390/pharmaceutics17070946 - 21 Jul 2025
Viewed by 345
Abstract
A review of the literature on polymorphic transformations by milling on pharmaceutical materials was carried out. The available information on 18 pharmaceutical materials was compiled. In particular, when data are available, the starting and final crystalline forms, their enantiotropic or monotropic relationship, the [...] Read more.
A review of the literature on polymorphic transformations by milling on pharmaceutical materials was carried out. The available information on 18 pharmaceutical materials was compiled. In particular, when data are available, the starting and final crystalline forms, their enantiotropic or monotropic relationship, the glass transition temperature of the compound and its melting temperature, the experimental observation of a transient or partial amorphization of compounds, and the transformation kinetics make it possible to suggest a two-step transformation mechanism. First, an amorphization occurs under milling of the starting polymorphic form. Secondly, a recrystallization of the amorphous form occurs towards the final form. The observed transformation kinetics are due to the fact that the recrystallization of the amorphous material towards the final form depends on the accidental formation of a cluster of this form during milling. Moreover, the observation of the transient amorphous form depends on the relative position of the glass transition temperature of the material with respect to the milling temperature. This mechanism seems to be independent of the enantiotropic or monotropic character of the polymorphic forms involved in the transformation. Full article
(This article belongs to the Collection Feature Papers in Pharmaceutical Technology)
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14 pages, 2226 KiB  
Article
Investigation of the Effect of C-Terminal Adjacent Phenylalanine Residues on Asparagine Deamidation by Quantum Chemical Calculations
by Koichi Kato, Haruka Asai, Tomoki Nakayoshi, Ayato Mizuno, Akifumi Oda and Yoshinobu Ishikawa
Int. J. Mol. Sci. 2025, 26(14), 6819; https://doi.org/10.3390/ijms26146819 - 16 Jul 2025
Viewed by 191
Abstract
The deamidation rate is relatively high for Asn residues with Phe as the C-terminal adjacent residue in γS-crystallin, which is one of the human crystalline lens proteins. However, peptide-based experiments indicated that bulky amino acid residues on the C-terminal side impaired Asn deamination. [...] Read more.
The deamidation rate is relatively high for Asn residues with Phe as the C-terminal adjacent residue in γS-crystallin, which is one of the human crystalline lens proteins. However, peptide-based experiments indicated that bulky amino acid residues on the C-terminal side impaired Asn deamination. In this study, we hypothesized that the side chain of Phe affects the Asn deamidation rate and investigated the succinimide formation process using quantum chemical calculations. The B3LYP density functional theory was used to obtain optimized geometries of energy minima and transition states, and MP2 and M06-2X calculations were used to obtain the single-point energy. Activation barriers and rate-determining step changed depending on the orientation of the Phe side chain. In pathways where an interaction occurred between the benzene ring and the amide group of the Asn residue, the activation barrier was lower than in pathways where this interaction did not occur. Since the aromatic ring is oriented toward the Asn side in experimentally determined structures of γS-crystallin, the above interaction is considered to enhance the Asn deamidation. Full article
(This article belongs to the Section Molecular Biophysics)
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22 pages, 4482 KiB  
Article
Cu-Doping Induced Structural Transformation and Magnetocaloric Enhancement in CoCr2O4 Nanoparticles
by Ming-Kang Ho, Yun-Tai Yu, Hsin-Hao Chiu, K. Manjunatha, Shih-Lung Yu, Bing-Li Lyu, Tsu-En Hsu, Heng-Chih Kuo, Shuan-Wei Yu, Wen-Chi Tu, Chiung-Yu Chang, Chia-Liang Cheng, H. Nagabhushana, Tsung-Te Lin, Yi-Ru Hsu, Meng-Chu Chen, Yue-Lin Huang and Sheng Yun Wu
Nanomaterials 2025, 15(14), 1093; https://doi.org/10.3390/nano15141093 - 14 Jul 2025
Viewed by 317
Abstract
This study systematically investigates the impact of Cu2+ doping on the structural, magnetic, and magnetocaloric properties of CuxCo1−xCr2O4 nanoparticles synthesized via a solution combustion method. Cu incorporation up to x = 20% induces a [...] Read more.
This study systematically investigates the impact of Cu2+ doping on the structural, magnetic, and magnetocaloric properties of CuxCo1−xCr2O4 nanoparticles synthesized via a solution combustion method. Cu incorporation up to x = 20% induces a progressive structural transformation from a cubic spinel to a trigonal corundum phase, as confirmed by X-ray diffraction and Raman spectroscopy. The doping process also leads to increased particle size, improved crystallinity, and reduced agglomeration. Magnetic measurements reveal a transition from hard to soft ferrimagnetic behavior with increasing Cu content, accompanied by a notable rise in the Curie temperature from 97.7 K (x = 0) to 140.2 K (x = 20%). The magnetocaloric effect (MCE) is significantly enhanced at higher doping levels, with the 20% Cu-doped sample exhibiting a maximum magnetic entropy change (−ΔSM) of 2.015 J/kg-K and a relative cooling power (RCP) of 58.87 J/kg under a 60 kOe field. Arrott plot analysis confirms that the magnetic phase transitions remain second-order in nature across all compositions. These results demonstrate that Cu doping is an effective strategy for tuning the magnetostructural response of CoCr2O4 nanoparticles, making them promising candidates for low-temperature magnetic refrigeration applications. Full article
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22 pages, 3797 KiB  
Article
Structurally Ordered NIPUs via Catalyst-Free Synthesis with Hard Segments Based on Erythritol and a Long-Chain Diamine
by Edyta Hebda, Karolina Wróbel, Aleksandra Cieślik, Kinga Szołdrowska, Jan Ozimek, Paulina Zając, Konstantinos N. Raftopoulos and Krzysztof Pielichowski
Molecules 2025, 30(14), 2912; https://doi.org/10.3390/molecules30142912 - 10 Jul 2025
Viewed by 726
Abstract
A series of linear isocyanate-free polyurethanes (NIPUs) were obtained via the aminolysis of erythritol dicarbonate (EDC) with polyethers (diamino-PEG, diamino-PPO, and diamino-PEG/PPO) and 1,12-diaminododecane (DADD), which acts as a chain extender to form hard segments. The obtained NIPUs contained different concentrations of DADD [...] Read more.
A series of linear isocyanate-free polyurethanes (NIPUs) were obtained via the aminolysis of erythritol dicarbonate (EDC) with polyethers (diamino-PEG, diamino-PPO, and diamino-PEG/PPO) and 1,12-diaminododecane (DADD), which acts as a chain extender to form hard segments. The obtained NIPUs contained different concentrations of DADD relative to the polyether (72.5–80 wt%). A detailed chemical structure analysis of the synthesized NIPU was performed using a combination of FTIR and 1H NMR. FTIR spectra confirmed that the EDC/DADD segments formed a network of hydrogen bonds. This is reflected in WAXD diffractograms showing ordered crystalline domains originating in DADD. The reflections assigned to the EDC/DADD segments exhibited changes in their position and intensity with decreasing concentration, indicating an increase in interplanar spacing and a loss of higher-order order. WAXD also showed that the soft segments of PEG and PEG/PPO retain their ordered crystal structure regardless of the EDC/DADD content. At a larger length scale, SAXS revealed similar micromorphology for the different polyethers, with a broad peak indicating long-range order in the EDC/DADD-rich segments and a weak separation of the soft and hard phases. DSC analyses confirmed the complex phase behavior, where the PEG-based materials showed melting of crystalline fragments, and the amorphous PPO showed a glass transition. DMA indicated the stability of the glass transition temperature in the PPO samples and the presence of an unusual structural transition. The results emphasize the influence of the type of poly(ether) on the thermal and microphase properties of the studied non-isocyanate polyurethanes. Full article
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14 pages, 5135 KiB  
Article
Effect of Cd Doping on the Gas-Sensitive Properties of ZnSn(OH)6
by Yufeng Wen, Yanlin Yu, Huaizhang Gu, Guilian Wang and Fangqiang Yuan
Materials 2025, 18(13), 3176; https://doi.org/10.3390/ma18133176 - 4 Jul 2025
Viewed by 296
Abstract
The influence of Cd doping on the performance of ZnSn(OH)6 (ZHS) as a gas sensor was systematically investigated through experimental and theoretical approaches. ZHS and Cd-doped ZHS samples were synthesized using the hydrothermal method. The microstructures of pure and Cd-doped ZHS were [...] Read more.
The influence of Cd doping on the performance of ZnSn(OH)6 (ZHS) as a gas sensor was systematically investigated through experimental and theoretical approaches. ZHS and Cd-doped ZHS samples were synthesized using the hydrothermal method. The microstructures of pure and Cd-doped ZHS were characterized using various techniques. The results revealed that the pure ZHS sample exhibits good crystallinity and an octahedral morphology with particle sizes ranging from 800 to 1900 nm. After Cd doping, the particle size range was decreased to 700–1500 nm. A systematic investigation of the gas-sensing properties revealed that Cd-doped ZHS exhibits superior sensing performance toward ethanol gas compared to pure ZHS. Under operating conditions of 240 °C, 100 ppm concentration, and 30% relative humidity, the response of ZHS to ethanol gas exhibited a significantly higher value compared to other tested gases. After Cd doping, the response approximately doubled. Density functional theory calculations of electronic structures revealed that the enhanced ethanol sensing mechanism of Cd-doped ZHS is attributed to the narrowed band gap caused by Cd doping, which increases electron concentration and enhances O ion adsorption on the surface. Full article
(This article belongs to the Special Issue Materials for Photocatalytic and Electrocatalytic Applications)
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23 pages, 1856 KiB  
Article
Comparative Evaluation of Gelatin and HPMC Inhalation Capsule Shells Exposed to Simulated Humidity Conditions
by Sabrina Magramane, Nikolett Kállai-Szabó, Dóra Farkas, Károly Süvegh, Romána Zelkó and István Antal
Pharmaceutics 2025, 17(7), 877; https://doi.org/10.3390/pharmaceutics17070877 - 3 Jul 2025
Viewed by 574
Abstract
Background/Objectives: This study investigates the impact of high humidity (25 °C, 75% relative humidity) on gelatin and hydroxypropyl methylcellulose (HPMC) capsules used in dry powder inhalers (DPIs), focusing on moisture dynamics, structural responses, and mechanical performance, with an emphasis on understanding how [...] Read more.
Background/Objectives: This study investigates the impact of high humidity (25 °C, 75% relative humidity) on gelatin and hydroxypropyl methylcellulose (HPMC) capsules used in dry powder inhalers (DPIs), focusing on moisture dynamics, structural responses, and mechanical performance, with an emphasis on understanding how different capsule types respond to prolonged exposure to humid conditions. Methods: Capsules were exposed to controlled humidity conditions, and moisture uptake was measured via thermal analysis. Visual observations of silica bead color changes were performed to assess moisture absorption, while surface wettability was measured using the sessile drop method. Hardness testing, mechanical deformation, and puncture tests were performed to evaluate structural and mechanical changes. Positron annihilation lifetime spectroscopy (PALS) was used to analyze free volume expansion. Results: HPMC capsules exhibited rapid moisture uptake, attributed to their lower equilibrium moisture content and ability to rearrange dynamically, preventing brittleness. In contrast, gelatin capsules showed slower moisture absorption but reached higher equilibrium levels, resulting in plasticization and softening. Mechanical testing showed that HPMC capsules retained structural integrity with minimal deformation, while gelatin capsules became softer and exhibited reduced puncture resistance. Structural analysis revealed greater free volume expansion in HPMC capsules, consistent with their amorphous nature, compared with gelatin’s semi-crystalline matrix. Conclusions: HPMC capsules demonstrated superior humidity resilience, making them more suitable for protecting moisture-sensitive active pharmaceutical ingredients (APIs) in DPI formulations. These findings underline the importance of appropriate storage conditions, as outlined in the Summary of Product Characteristics, to ensure optimal capsule performance throughout patient use. Full article
(This article belongs to the Section Physical Pharmacy and Formulation)
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15 pages, 2226 KiB  
Article
Perovskite Solar Cells Modified with Conjugated Self-Assembled Monolayers at Buried Interfaces
by Guorong Zhou, Faeze Hashemi, Changzeng Ding, Xin Luo, Lianping Zhang, Esmaeil Sheibani, Qun Luo, Askhat N. Jumabekov, Ronald Österbacka, Bo Xu and Changqi Ma
Nanomaterials 2025, 15(13), 1014; https://doi.org/10.3390/nano15131014 - 1 Jul 2025
Viewed by 545
Abstract
In recent years, inverted perovskite solar cells (PSCs) have garnered widespread attention due to their high compatibility, excellent stability, and potential for low-temperature manufacturing. However, most of the current research has primarily focused on the surface passivation of perovskite. In contrast, the buried [...] Read more.
In recent years, inverted perovskite solar cells (PSCs) have garnered widespread attention due to their high compatibility, excellent stability, and potential for low-temperature manufacturing. However, most of the current research has primarily focused on the surface passivation of perovskite. In contrast, the buried interface significantly influences the crystal growth quality of perovskite, but it is difficult to effectively control, leading to relatively slow research progress. To address the issue of poor interfacial contact between the hole transport-layer nickel oxide (NiOX) and the perovskite, we introduced a conjugated self-assembled monolayer (SAM), 4,4′-[(4-(3,6-dimethoxy-9H-carbazole)triphenylamine)]diphenylacetic acid (XS21), which features triphenylamine dicarboxylate groups. For comparison, we also employed the widely studied phosphonic acid-based SAM, [2-(3,6-dimethoxy-9H-carbazole-9-yl)ethyl] phosphonic acid (MeO-2PACz). A systematic investigation was carried out to evaluate the influence of these SAMs on the performance and stability of inverted PSCs. The results show that both XS21 and MeO-2PACz significantly enhanced the crystallinity of the perovskite layer, reduced defect densities, and suppressed non-radiative recombination. These improvements led to more efficient hole extraction and transport at the buried interface. Consequently, inverted PSCs incorporating XS21 and MeO-2PACz achieved impressive power-conversion efficiencies (PCEs) of 21.43% and 22.43%, respectively, along with marked enhancements in operational stability. Full article
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19 pages, 8298 KiB  
Article
Screening for Polymorphism, Cyclodextrin Complexation, and Co-Crystallization of the Non-Steroidal Anti-Inflammatory Drug Fenbufen: Isolation and Characterization of a Co-Crystal and an Ionic Co-Crystal of the API with a Common Coformer
by Hannah M. Frösler, Neo Refiloe Mancapa, Laura Catenacci, Milena Sorrenti, Maria Cristina Bonferoni and Mino R. Caira
Pharmaceutics 2025, 17(7), 842; https://doi.org/10.3390/pharmaceutics17070842 - 27 Jun 2025
Viewed by 415
Abstract
Background/Objectives: Increasing the solid-state landscape of an active pharmaceutical ingredient (API) by generating new crystalline forms (e.g., polymorphs, cyclodextrin (CD) inclusion complexes, co-crystals, and salts) can yield products with significantly enhanced biopharmaceutical properties (especially increased water solubility), thereby improving API delivery and [...] Read more.
Background/Objectives: Increasing the solid-state landscape of an active pharmaceutical ingredient (API) by generating new crystalline forms (e.g., polymorphs, cyclodextrin (CD) inclusion complexes, co-crystals, and salts) can yield products with significantly enhanced biopharmaceutical properties (especially increased water solubility), thereby improving API delivery and extending its lifetime. The aim of this study was the isolation of new solid forms of the poorly water-soluble non-steroidal anti-inflammatory drug fenbufen (FBF), for which relatively few solid phases have been reported to date. Further motivation for the study is the recent finding that it has potential for repurposing to treat acute pancreatitis. Methods: Interventions for generating new solid forms of FBF included (a) polymorph screening with a variety of solvent media, (b) attempts to form solid inclusion complexes with the native cyclodextrins α-, β-, and γ-CD using various preparative methods, and (c) co-crystallization with a series of coformers to produce co-crystals and/or molecular salts. Results: No new polymorphic forms of FBF were identified, but screening with CDs resulted in isolation and characterization of a new solid inclusion complex with γ-CD. However, co-crystallization of FBF with the water-soluble coformer isonicotinamide yielded two new products, namely a 1:1 co-crystal and an unusual multi-component ionic co-crystal, whose aqueous solubility indicated significant enhancement of FBF solubility. Conclusions: Due to its extremely low water solubility, FBF presented challenges during the study aimed at modifying its crystalline form. However, two new supramolecular forms, a co-crystal and an ionic co-crystal, were isolated, the latter phase having potential for further formulation owing to its significantly enhanced solubility. Full article
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20 pages, 5699 KiB  
Article
Upcycling of Agro-Waste: Research on Performance of a Novel Super-Hygroscopic Material Prepared by Exploiting the Porous Structure of Steam-Exploded Modified Corn Stalk Pith
by Nan Wang, Chuntao Xia, Tingting Liu and Dawei Wang
Polymers 2025, 17(13), 1779; https://doi.org/10.3390/polym17131779 - 27 Jun 2025
Viewed by 271
Abstract
Herein, a novel super-hygroscopic material, steam-exploded modified corn stalk pith (SE-CSP), was developed from corn stalk pith (CSP) via the steam explosion (SE) method, and its hygroscopic properties and mechanisms were evaluated. The results confirmed that SE effectively removed lignin and hemicellulose, disrupted [...] Read more.
Herein, a novel super-hygroscopic material, steam-exploded modified corn stalk pith (SE-CSP), was developed from corn stalk pith (CSP) via the steam explosion (SE) method, and its hygroscopic properties and mechanisms were evaluated. The results confirmed that SE effectively removed lignin and hemicellulose, disrupted the thin cell walls of natural CSP, and formed an aligned porous structure with capillary channels. SE changed the bonding distribution and surface morphology, and enhanced the crystallinity and thermal stability of CSP. The equilibrium hygroscopic percentage of SE-CSP (62.50%) was higher than that of CSP (44.01%) at 25 °C and 80% relative humidity (RH), indicating significantly greater hygroscopicity. The hygroscopic process of SE-CSP followed a Type III isotherm and fitted the Guggenheim–Anderson–de Boer (GAB), Peleg, and pseudo-first-order kinetic models. This process exhibited multi-layer adsorption with enthalpy-driven, exothermic behavior, primarily through physical adsorption involving hydrogen bonds and van der Waals forces. This work offered a new approach for advancing sorption dehumidification technology. Full article
(This article belongs to the Special Issue Applications of Polymer-Based Absorbent Materials)
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22 pages, 4058 KiB  
Article
Thermal, Mechanical, Morphological, and Piezoresistive Properties of Poly(ethylene-co-methacrylic acid) (EMAA) with Carbon Nanotubes and Expanded Graphite
by Francesca Aliberti, Luigi Vertuccio, Raffaele Longo, Andrea Sorrentino, Roberto Pantani, Liberata Guadagno and Marialuigia Raimondo
Nanomaterials 2025, 15(13), 994; https://doi.org/10.3390/nano15130994 - 26 Jun 2025
Viewed by 357
Abstract
This paper presents a comparative study examining the effects of carbon nanotubes (CNTs) and expanded graphite (EG) on the thermal, mechanical, morphological, electrical, and piezoresistive properties of poly(ethylene-co-methacrylic acid) (EMAA) nanocomposites. To this end, different amounts of carbonaceous fillers (EG and CNTs separately) [...] Read more.
This paper presents a comparative study examining the effects of carbon nanotubes (CNTs) and expanded graphite (EG) on the thermal, mechanical, morphological, electrical, and piezoresistive properties of poly(ethylene-co-methacrylic acid) (EMAA) nanocomposites. To this end, different amounts of carbonaceous fillers (EG and CNTs separately) were added to the EMAA thermoplastic matrix, and the relative electrical percolation thresholds (EPTs) were determined. The effect of filler concentration on thermo-oxidative degradation and the EMAA crystallinity was investigated via thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC), respectively. Dynamic mechanical analysis (DMA) demonstrated that both fillers enhance the Young’s and storage moduli, as well as the glass transition temperature, with a greater improvement for the bidimensional nanofiller, most likely due to the cumulative effect of more extensive EG-matrix interactions. In tensile tests, a very relevant difference was detected in the Gauge Factor (G.F.) and the elongation at break of the two typologies of nanocomposites. The G.F. of EMAA 10% CNT and EMAA 15% EG were found to be 0.5 ± 0.08 and 165 ± 14, respectively, while elongation at break was about 68% for EMAA 10% CNT and 8% for EMAA 15% EG. Emission Scanning Electron Microscopy (FESEM) and Tunneling Atomic Force Microscopy (TUNA) have contributed to explaining the differences between EG- and CNT-based nanocomposites from a morphological point of view, underlying the pivotal role of the filler aspect ratio and its structural features in determining different mechanical and piezoresistive performance. The comprehensive analysis of EMAA-EG and EMAA-CNT nanocomposites provides a guide for selecting the best self-sensing system for the specific application. More specifically, EMAA-CNT nanocomposites with high elongation at break and lower sensitivity to small strains are suitable for movement sensors in the soft robotic field, where high deformation has to be detected. On the other hand, the high sensitivity at a low strain of EMAA-EG systems makes them suitable for integrated sensors in more rigid composite structures, such as aeronautical and automotive components or wind turbines. Full article
(This article belongs to the Special Issue Functional and Structural Properties of Polymeric Nanocomposites)
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17 pages, 4413 KiB  
Article
Impact of Fatty Acid Types and Microwave Post-Treatment on the Physicochemical Properties of Water Caltrop Starch–Lipid Complexes
by Pei-Chang Lee and Lih-Shiuh Lai
Foods 2025, 14(13), 2254; https://doi.org/10.3390/foods14132254 - 25 Jun 2025
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Abstract
This study investigates the effects of microwave post-treatment and fatty acid type on the physicochemical properties of starch–lipid complexes derived from water caltrop (Trapa taiwanensis Nakai) starch. Complexes were prepared using stearic acid (C18:0) or oleic acid (C18:1), [...] Read more.
This study investigates the effects of microwave post-treatment and fatty acid type on the physicochemical properties of starch–lipid complexes derived from water caltrop (Trapa taiwanensis Nakai) starch. Complexes were prepared using stearic acid (C18:0) or oleic acid (C18:1), followed by microwave post-treatment at varying durations. Morphological analysis revealed that the starch–stearic acid complex exhibited more plate-like structures and birefringent spots compared to the starch–oleic acid complex. The complexing index increased with extended microwave exposure, indicating enhanced complex formation. Fourier-transform infrared spectroscopy showed no significant variation in the 1047/1022 cm−1 absorption ratio, suggesting that the short-range molecular order remained unaffected. However, X-ray diffraction analysis indicated increased relative crystallinity, particularly in the stearic acid complex (10.4%) compared to the oleic acid complex (4.8%), likely due to the higher linearity and saturation of stearic acid. Differential scanning calorimetry confirmed the presence of both type I and type II crystallization in all samples. The starch–stearic acid complex exhibited greater thermal stability, promoted type II crystallization, and enhanced the ordered structure of type I crystallization. In contrast, microwave treatment had limited influence on the thermal properties of the starch–oleic acid complex. These findings demonstrate that microwave post-treatment facilitates starch–lipid complex formation and improves structural organization, particularly when saturated fatty acids are employed. Full article
(This article belongs to the Special Issue Research on the Structure and Physicochemical Properties of Starch)
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