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23 pages, 2942 KiB  
Article
Bone Marrow Stromal Cells Generate a Pro-Healing Inflammasome When Cultured on Titanium–Aluminum–Vanadium Surfaces with Microscale/Nanoscale Structural Features
by David J. Cohen, Christine M. Van Duyn, Jingyao Deng, Musaddiq K. Lodi, Michelle B. Gallagher, James T. Sugar, Jeremy J. Rawlinson, Preetam Ghosh, Barbara D. Boyan and Zvi Schwartz
Biomimetics 2025, 10(1), 66; https://doi.org/10.3390/biomimetics10010066 (registering DOI) - 19 Jan 2025
Viewed by 402
Abstract
The surface topography and chemistry of titanium–aluminum–vanadium (Ti6Al4V) implants play critical roles in the osteoblast differentiation of human bone marrow stromal cells (MSCs) and the creation of an osteogenic microenvironment. To assess the effects of a microscale/nanoscale (MN) topography, this study compared the [...] Read more.
The surface topography and chemistry of titanium–aluminum–vanadium (Ti6Al4V) implants play critical roles in the osteoblast differentiation of human bone marrow stromal cells (MSCs) and the creation of an osteogenic microenvironment. To assess the effects of a microscale/nanoscale (MN) topography, this study compared the effects of MN-modified, anodized, and smooth Ti6Al4V surfaces on MSC response, and for the first time, directly contrasted MN-induced osteoblast differentiation with culture on tissue culture polystyrene (TCPS) in osteogenic medium (OM). Surface characterization revealed distinct differences in microroughness, composition, and topography among the Ti6Al4V substrates. MSCs on MN surfaces exhibited enhanced osteoblastic differentiation, evidenced by increased expression of RUNX2, SP7, BGLAP, BMP2, and BMPR1A (fold increases: 3.2, 1.8, 1.4, 1.3, and 1.2). The MN surface also induced a pro-healing inflammasome with upregulation of anti-inflammatory mediators (170–200% increase) and downregulation of pro-inflammatory factors (40–82% reduction). Integrin expression shifted towards osteoblast-associated integrins on MN surfaces. RNA-seq analysis revealed distinct gene expression profiles between MSCs on MN surfaces and those in OM, with only 199 shared genes out of over 1000 differentially expressed genes. Pathway analysis showed that MN surfaces promoted bone formation, maturation, and remodeling through non-canonical Wnt signaling, while OM stimulated endochondral bone development and mineralization via canonical Wnt3a signaling. These findings highlight the importance of Ti6Al4V surface properties in directing MSC differentiation and indicate that MN-modified surfaces act via signaling pathways that differ from OM culture methods, more accurately mimicking peri-implant osteogenesis in vivo. Full article
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Figure 1

Figure 1
<p>Optical profilometry measurements of surface micro-roughness of smooth machined (SM), anodized (AN), and micro/nano-rough (MN) Ti6Al4V surfaces: average peak-to-valley distance (<b>A</b>), skewness (<b>B</b>), microroughness (<b>C</b>), and kurtosis (<b>D</b>). Data are means ± SEM and were evaluated using analysis of variance (ANOVA) with Tukey post hoc test. Statistical significance was established at <span class="html-italic">p</span>-values equal to or less than 0.05 (*** <span class="html-italic">p</span> &lt; 0.001; **** <span class="html-italic">p</span> &lt; 0.0001).</p>
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<p>Implant surface characterization of smooth machined (SM), anodized (AN), and micro/nano-rough (MN) Ti6Al4V surfaces: (<b>A</b>) X-ray photoelectron spectroscopy (XPS) was used to determine elemental composition, shown as mean atomic percentage (%) of carbon (<b>C</b>), oxygen (O), titanium (Ti), aluminum (Al), and vanadium (V). (<b>B</b>) Surface wettability was quantified through sessile drop contact angle measurements performed on each surface. (<b>C</b>) Semi-quantitative energy-dispersive X-ray spectroscopy (EDX) analysis of surface elemental composition was obtained from ion-milled cross-sections of each surface, shown as mean atomic percentage (%) of titanium (Ti), aluminum (Al), and vanadium (V). (<b>D</b>) X-ray diffraction (XRD) profiles were used to determine distribution of α-Ti and β-Ti phases for each surface material, with circles depicting α-Ti, whereas triangles distinguish β-Ti phase based on elemental reference standards for EDX. Data are presented as mean + SEM and were evaluated using analysis of variance (ANOVA) with Tukey post hoc test. Statistical significance was established at <span class="html-italic">p</span>-values equal to or less than 0.05 (*** <span class="html-italic">p</span> &lt; 0.001; **** <span class="html-italic">p</span> &lt; 0.0001).</p>
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<p>Characterization of surface topography using scanning electron microscopy (SEM). SEM micrographs/images of smooth, anodized, and micro/nano-rough (MN) Ti6Al4V surfaces were captured at macroscale (35×), microscale (1000×), mesoscale (10,000×), and nanoscale (100,000×) resolutions. Macro/micro/meso/nanoscale images have scale bars of 1 mm, 50 μm, 5 μm, and 500 nm, respectively.</p>
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<p>Relative expression of osteogenesis-related genes in human BMSCs cultured for 14 days on TCPS, smooth, anodized, or micro/nano-rough (MN) surfaces via RT-qPCR. Genes were normalized to GAPDH, and their relative expression compared to TCPS, determined using the 2<sup>−ΔΔCT</sup> method. Values presented are mean ± SE of twelve independent cultures per surface, pooled in duplicate with <span class="html-italic">n</span> of 6 per group. Groups were evaluated using analysis of variance (ANOVA) with Tukey post hoc test. Statistical significance was established at <span class="html-italic">p</span>-values equal to or less than 0.05 (* <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; **** <span class="html-italic">p</span> &lt; 0.0001).</p>
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<p>Relative expression of anti-/pro-inflammatory genes in human BMSCs cultured for 14 days on TCPS, smooth, anodized, or micro/nano-rough (MN) surfaces via RT-qPCR. Genes related to innate and adaptive immune mechanisms related to inflammation, including genes that encode for cytokines/chemokines and inflammasome components with anti-inflammatory (top) and pro-inflammatory (bottom) effects, were analyzed. Fold changes to TCPS were normalized to GAPDH and relative expression determined using 2<sup>−ΔΔCT</sup> method. Values are presented as mean ± SE of twelve independent cultures per surface, pooled in duplicate with <span class="html-italic">n</span> of 6 per group. Groups were evaluated using analysis of variance (ANOVA) with Tukey post hoc test. Statistical significance was established at <span class="html-italic">p</span>-values equal to or less than 0.05 (* <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).</p>
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<p>Relative expression of extracellular matrix (ECM)-related genes related to integrin binding and cell adhesion in human BMSCs. Cells were cultured for 14 days on TCPS, smooth, anodized, or micro-/nano-rough (MN) surfaces via RT-qPCR. Representative genes related to integrin binding are on top, and components of ECM are shown in bottom row. Fold changes to TCPS were normalized to GAPDH and relative expression determined using 2<sup>−ΔΔCT</sup> method. Values are presented as mean ± SE of twelve independent cultures per surface, pooled in duplicate with <span class="html-italic">n</span> of 6 per group. Groups were evaluated using analysis of variance (ANOVA) with Tukey post hoc test. Statistical significance was established at <span class="html-italic">p</span>-values equal to or less than 0.05 (* <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; **** <span class="html-italic">p</span> &lt; 0.0001).</p>
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<p>Comparison of 12,000 differentially expressed genes (DEGs) of human BMSCs grown in osteogenic media (OM), compared with BMSCs cultured on micro/nano-rough (MN) surfaces or TCPS in standard growth media: (<b>A</b>) Heatmap of sample z-scores clustered using Euclidean distance measurement. Red and green in heat map denote upregulated and downregulated genes, respectively, while gray denotes no significant difference between groups. (<b>B</b>) Principal component analysis (PCA) plot generated from 12,000 differentially expressed genes in hBMSCs grown for 14 days on TCPS in OM, TCPS in growth media, or MN surfaces in growth media, as determined by RNA-seq. Results from two independent experiments are shown.</p>
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<p>Comparison of 12,000 differentially expressed of genes (DEGs) of human BMSCs grown on TCPS in osteogenic media (OM), or BMSCs cultured on micro/nano-rough (MN) surfaces in growth media, compared to cells on TCPS in growth media. (<b>A</b>) Venn diagram displaying overlap of differentially expressed genes, showing overlap between OM and MN cultures. (<b>B</b>) Volcano plot of MN vs. TCPS genes with Log2 fold change greater than 2 and adjusted <span class="html-italic">p</span>-value less than 0.05. (<b>C</b>) Volcano plot of OM vs. TCPS genes with Log2 fold change greater than 2 and adjusted <span class="html-italic">p</span>-value less than 0.05. Red and blue denote upregulated and downregulated genes, respectively, while gray denotes no significant difference between groups.</p>
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<p>Functional enrichment analysis of genes expressed by BMSCs grown on TCPS in growth media (TCPS), TCPS in osteogenic media (OM), and micro/nano-rough Ti6Al4V in growth media (MN). The enriched pathways were visualized using a barplot for each pairwise comparison of treatments: (<b>A</b>) MN vs. TCPS, (<b>B</b>) OM vs. TCPS, and (<b>C</b>) MN vs. OM. (<b>D</b>) The Venn diagrams were created by determining the overlapping pathways between OM vs. TCPS and MN vs. TCPS.</p>
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11 pages, 12673 KiB  
Article
Effect of Tool Shoulder Profile on Grain and Texture Development in the Weld Interface Zone of Friction-Stir-Welded Dissimilar AA2024/AA7075 Joints
by Qi Li, Chenghang Zhang, Jianhong Sun and Haoge Shou
Materials 2025, 18(2), 340; https://doi.org/10.3390/ma18020340 - 14 Jan 2025
Viewed by 315
Abstract
Friction-stir-welded dissimilar AA2024/AA7075 joints have an apparent influence on grain and texture development at the weld interface due to differences in physical and chemical properties between the two aluminum alloys. In this work, the effect of tool shoulder profile on grain structure and [...] Read more.
Friction-stir-welded dissimilar AA2024/AA7075 joints have an apparent influence on grain and texture development at the weld interface due to differences in physical and chemical properties between the two aluminum alloys. In this work, the effect of tool shoulder profile on grain structure and texture evolution in the center interface zone (CIZ) and bottom interface zone (BIZ) of dissimilar AA2024/AA7075 joints were quantitatively studied by electron back-scattering diffraction (EBSD). The results indicate that abundant fine and coarse equiaxial grains are produced in the CIZ and BIZ of the joints produced with a concentric circle shoulder (CCS) and three-helix shoulder (THS), and the average grain size of the BIZ is lower than that of the CIZ for the same CCS or THS joint. A higher degree of recrystallization occurs in the CIZ of the joint with a CCS than that of the joint with a THS, while a similar degree of recrystallization is presented in the BIZ of the two joints. For the distribution of local misorientation angle between the two sides of the interface in the same CCS or THS joint, the CIZ manifests relatively uniform behavior, while the BIZ presents the characteristics of uneven distribution. Tool shoulder profile has a significant impact on the texture components at the weld interface, which results in different types of shear textures generated in the CIZ and BIZ of the two joints. It is beneficial to make out the microstructural evolution mechanism at the weld interface in dissimilar FSW joints for engineering applications in this study. Full article
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Figure 1
<p>Cross-section appearances of dissimilar AA2024/AA7075 FSW joints: (<b>a</b>) CCS joint; (<b>b</b>) THS joint.</p>
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<p>Euler angle diagrams (Euler angles 1, 2 and 3 represent the angle (<sup>o</sup>) of rotation around ND, WD and TD, respectively) in the welded zone: (<b>a</b>) CCS-CIZ; (<b>b</b>) THS-CIZ; (<b>c</b>) CCS-BIZ; (<b>d</b>) THS-BIZ.</p>
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<p>Analysis maps of the grain recrystallization degree in the welded zone: (<b>a</b>) CCS-CIZ; (<b>b</b>) THS-CIZ; (<b>c</b>) CCS-BIZ; (<b>d</b>) THS-BIZ.</p>
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<p>Statistical results of the grain recrystallization degree in the welded zone of the dissimilar joints shown in <a href="#materials-18-00340-f003" class="html-fig">Figure 3</a>.</p>
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<p>Distribution images of local misorientation in the welded zone: (<b>a</b>) CCS-CIZ; (<b>b</b>) THS-CIZ; (<b>c</b>) CCS-BIZ; (<b>d</b>) THS-BIZ.</p>
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<p>Statistical results of local misorientation in the welded zone shown in <a href="#materials-18-00340-f005" class="html-fig">Figure 5</a>: (<b>a</b>) CIZ; (<b>b</b>) BIZ (relative frequency is described as the occurrence frequency of a local misorientation within the set local misorientation range).</p>
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<p>Distribution images of shear texture components in the welded zone: (<b>a</b>) CCS-CIZ; (<b>b</b>) THS-CIZ; (<b>c</b>) CCS-BIZ; (<b>d</b>) THS-BIZ.</p>
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<p>Statistical results of shear textures in the welded zone of the dissimilar joints shown in <a href="#materials-18-00340-f007" class="html-fig">Figure 7</a>.</p>
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20 pages, 2844 KiB  
Article
Rheology and Stability of Hydrocarbon-Based Gelled Fuels for Airbreathing Applications
by Simone Dell’Acqua, Francesco Morando, Stefania Carlotti and Filippo Maggi
Aerospace 2025, 12(1), 49; https://doi.org/10.3390/aerospace12010049 - 13 Jan 2025
Viewed by 416
Abstract
Gelled fuels are rheologically complex, non-Newtonian fluids. They combine the benefits of both liquid and solid states, reducing risks of leakage, spilling, and sloshing during storage while maintaining the ability to be sprayed inside a combustion chamber. Additionally, suspending energetic particles, such as [...] Read more.
Gelled fuels are rheologically complex, non-Newtonian fluids. They combine the benefits of both liquid and solid states, reducing risks of leakage, spilling, and sloshing during storage while maintaining the ability to be sprayed inside a combustion chamber. Additionally, suspending energetic particles, such as metal powders of aluminum and boron, can significantly enhance their energy density compared to conventional liquid fuels. In this study, several kerosene-based and ethanol-based formulations were experimentally investigated, using both organic and inorganic gelling agents. The compositions were optimized in terms of the gellant amount and manufacturing process. Some of the most promising gellants for kerosene include fatty acids, such as Thixcin® R or THIXATROL® ST, and metallic soaps, such as aluminum stearate and zinc stearate. The effects of various co-solvents were assessed, including ketones (methyl isoamyl ketone, methyl ethyl ketone, and acetone) and alcohols (ethanol and octadecanol). Sugar polymers like hydroxypropyl cellulose were tested as gelling agents for ethanol. A preliminary rheological analysis was conducted to characterize their behavior at rest and under shear stress. Finally, a novel approach was introduced to study the stability of the gels under vibration, which was derived from a realistic mission profile of a ramjet. Finally, the ideal gravimetric specific impulse was evaluated through ideal thermochemical computations. The results showed that promising formulations can be found in both kerosene-based and ethanol-based gels. Such compositions are of interest in practical airbreathing applications as they have demonstrated excellent stability under vibration, ideal combustion properties, and pronounced shear-thinning behavior. Full article
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<p>Conceptual scheme of the experimental setup implemented for the vibration assessment of gelled fuels.</p>
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<p>Picture of the experimental setup for the vibration tests. The power amplifier is not shown in the figure.</p>
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<p>Qualitative representation of gel liquefaction behavior under vibration, describing the best (<b>a</b>) and worst (<b>b</b>) performances. Grade A2 is associated with an intermediate performance.</p>
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<p>Kerosene–aluminum stearate gels, highlighting the appearance in different preparation phases. Immediately after the original preparation (<b>a</b>); after a few hours (<b>b</b>); after the second mixing (<b>c</b>).</p>
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<p>Thermogravimetry analysis results for the most promising gels (<b>a</b>) and for gel components (<b>b</b>).</p>
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<p>Frequency-sweep dynamic measurements for different strain percentages.</p>
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<p>Dynamic strain–sweep analysis outcomes. (<b>a</b>) Storage modulus–shear stress curves, from which the yield stress <math display="inline"><semantics> <msub> <mi>τ</mi> <mrow> <mi>y</mi> <mi>i</mi> <mi>e</mi> <mi>l</mi> <mi>d</mi> </mrow> </msub> </semantics></math> can be derived; (<b>b</b>) storage modulus (black) and loss modulus (gray) profiles, identifying the flow point <math display="inline"><semantics> <msub> <mi>γ</mi> <mrow> <mi>f</mi> <mi>l</mi> <mi>o</mi> <mi>w</mi> </mrow> </msub> </semantics></math>.</p>
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<p>Rheological measurements from steady tests represented in logarithmic axes.</p>
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<p>Gravimetric specific impulse for gelled propellants and pure liquid fuels as a function of the air-to-fuel mass ratio.</p>
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17 pages, 3333 KiB  
Article
Evaluation of Alpaca Yarns Dyed with Buddleja Coriaceous Dye and Metallic Mordants
by Arturo Quispe-Quispe, Franklin Lozano, Luz María Pinche-Gonzales and Fulgencio Vilcanqui-Perez
Fibers 2025, 13(1), 2; https://doi.org/10.3390/fib13010002 - 28 Dec 2024
Viewed by 514
Abstract
The objective of this research was to evaluate the effect of dye obtained from Buddleja coriacea and metallic mordants on the chromatic properties, textile characteristics, spectral profiles, and color stability in alpaca fibers. The dye extraction technique involved boiling in an aqueous solution, [...] Read more.
The objective of this research was to evaluate the effect of dye obtained from Buddleja coriacea and metallic mordants on the chromatic properties, textile characteristics, spectral profiles, and color stability in alpaca fibers. The dye extraction technique involved boiling in an aqueous solution, followed by filtration. Subsequently, alpaca yarns were dyed using the resulting extract following a standard protocol. The applied mordants included sodium sulfate (Na2SO4), aluminum sulfate and potassium dodecahydrate (KAl(SO4)2·12H2O), and oxalic acid (C2H2O4). Spectroscopy UV-Vis and FTIR spectrophotometry methods were used for the characterization of the dyed samples and analysis of the dye during the dyeing process. The findings revealed the formation of four distinct color tones. Additionally, it was determined that the mordants influenced the chromatic properties of the fibers dyed with Buddleja coriacea extract without modifying their textile characteristics. The identified spectral bands corresponded to keratin, the structural protein of the fibers. Changes in the intensity of these spectral bands were observed in the dyed samples, attributable to the presence of different mordants. Wet rub fastness was found to be inferior to dry rub fastness, which has implications for textile maintenance. In conclusion, Buddleja coriacea flowers provide an effective yellow dye, and when combined with various mordants, they allow for a variety of shades and hues in alpaca fiber yarns. Full article
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Figure 1
<p>Dyeing process diagram of alpaca fiber with Buddleja coriácea dye.</p>
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<p>Dyeing procedure for alpaca fiber threads using <span class="html-italic">Buddleja coriacea</span> flower extract and mordants. 1, <span class="html-italic">Buddleja coriacea</span> tree; 2, <span class="html-italic">Buddleja coriacea</span> flowers; 3, drying of flowers in a forced air circulation oven; 4, extraction of natural dye from the flowers; 5, alpaca fiber threads; 6, metallic mordants; 7, alpaca fiber thread dyed with <span class="html-italic">Buddleja coriacea</span> flowers and mordants. T1, white fiber; T2, dyed with <span class="html-italic">Buddleja coriacea</span>; T3, <span class="html-italic">Buddleja coriacea</span> + KAl(SO<sub>4</sub>)<sub>2</sub>·12H<sub>2</sub>O; T4, <span class="html-italic">Buddleja coriacea</span> + C<sub>2</sub>H<sub>2</sub>O; T5, <span class="html-italic">Buddleja coriacea</span> + Na<sub>2</sub>SO<sub>4</sub>.</p>
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<p>FTIR analysis of <span class="html-italic">Buddleja coriacea</span> flower extract.</p>
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<p>Colorimetry parameters after treatment.</p>
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<p>Reflectance spectrum R (%) of alpaca fiber dyed with <span class="html-italic">Buddleja coriacea</span> flower extract and mordants.</p>
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<p>Change in colorimetry parameters due to treatment.</p>
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<p>FTIR analysis of alpaca fiber dyed with <span class="html-italic">Buddleja coriacea</span> flower extract and mordants.</p>
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17 pages, 3059 KiB  
Article
Can Aluminum Affect Social Behavior and Cortisol Plasma Profile in the Neotropical Freshwater Teleost Astyanax lacustris (Teleostei: Characidae)?
by Natália Pires Vieira Morais de Faria, Bruno Cavalheiro Araújo, Bianca Mayumi Silva Kida, Raisa Pereira Abdalla, Diego dos Santos Brito, Renata Guimarães Moreira and Renato Massaaki Honji
Life 2024, 14(12), 1697; https://doi.org/10.3390/life14121697 - 21 Dec 2024
Viewed by 575
Abstract
Aluminum (Al) can cause endocrine disruption in aquatic animals, but assessments of animal social behavior in neotropical teleost fish species with importance for Brazilian aquaculture have still not been addressed so far, which can further complete this ecotoxicological knowledge. In order to evaluate [...] Read more.
Aluminum (Al) can cause endocrine disruption in aquatic animals, but assessments of animal social behavior in neotropical teleost fish species with importance for Brazilian aquaculture have still not been addressed so far, which can further complete this ecotoxicological knowledge. In order to evaluate the social behavior and plasma cortisol concentration of fish exposed to Al, we performed a 1 h acute exposure with Astyanax lacustris couples in three different experimental groups: control in neutral pH (CTL/n group), acid pH (pH/ac group), and aluminum in acid pH (Al/ac group; 2.0 mg L−1). An ethogram of social interactions between males and females and swimming activities were performed. Furthermore, the cortisol plasma concentration was measured by enzyme-linked immunosorbent, and the gonadal maturation stage of the animals was evaluated by histology. Adult and mature females in the CTL/n and pH/ac groups were more aggressive and active than mature males, including several attacks on the male. Moreover, males did not present attack behavior in these groups at any time, but did show submission behavior and constant avoidance of female attacks. In the Al/ac, females did not attack males, couple decreased swimming activity, a repetitive movement toward the aquarium surface, and high mucus production were observed, making the water cloudy. Regarding cortisol plasma concentration, males had higher cortisol plasma concentrations than females in the CTL/n and pH/ac groups, which was not observed in the Al/ac group. Therefore, Al in addition to being described in the literature as an endocrine disruptor, it can be considered as behavioral disrupter in A. lacustris in this important freshwater species cultivated in South America. Full article
(This article belongs to the Special Issue Ecotoxicity Effects of Metals and Microplastics on Aquatic Organisms)
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Graphical abstract

Graphical abstract
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<p>Schematic representation of the experimental design. Exposure of couples (male (blue fish) and female (red fish); <span class="html-italic">n</span> = 2) (in triplicate; <span class="html-italic">n</span> = 6) of <span class="html-italic">Astyanax lacustris</span> in different experimental groups and digitally recorded (1 h): control (CTL/n group) in neutral pH; acid pH (pH/ac group); and aluminum (Al/ac group) in acid pH.</p>
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<p>Histological sections of <span class="html-italic">Astyanax lacustris</span> gonads. (<b>a</b>) mature female showing vitellogenic oocytes (arrow) and perinucleolar oocytes (arrowhead); (<b>b</b>) mature male showing several ducts full of sperm (asterisk). Stain: Schiff periodic acid (PAS)/iron-hematoxylin/metanil yellow. Bar: (<b>a</b>) 200 μm; (<b>b</b>) 100 μm.</p>
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<p>Evaluating the aggressiveness in <span class="html-italic">Astyanax lacustris</span>: (<b>a</b>) behavioral analysis of a couple in the experimental aquarium (60 L); (<b>b</b>) behaviors observed in <span class="html-italic">A. lacustris</span> (a couple, with a more aggressive female and bigger than the male) in experimental aquariums; the last gray box represents the aquarium with aluminum and “cloudy water”, and its main behaviors. For more information, see the text.</p>
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<p>General social behavior of <span class="html-italic">Astyanax lacustris</span> females and males in different experimental groups: control (CTL/n) in neutral pH; aluminum in acid pH (Al/ac); acid pH (pH/ac). Number (based on 10 min) of bites, chases with bites, chases without bites, and approaches. Data are presented as the mean ± standard error of the mean (M ± SEM). # indicates no behavior in this group.</p>
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<p>Social behavior of <span class="html-italic">Astyanax lacustris</span> females. Number (based on 10 min) of attacks and movements (right/left; bottom/front; superior/inferior) in different experimental groups: control (CTL/n) in neutral pH; aluminum in acid pH (Al/ac); acid pH (pH/ac). *, **, *** Asterisk indicates a statistical difference between experimental groups (right/left: CTL/n (<span class="html-italic">p</span> &lt; 0.006) and pH/ac (<span class="html-italic">p</span> &lt; 0.004) groups compared with Al/ac group; bottom/front: CTL/n compared with pH/ac (<span class="html-italic">p</span> &lt; 0.022); CTL/n compared with Al/ac (<span class="html-italic">p</span> &lt; 0.001); pH/ac compared with Al/ac (<span class="html-italic">p</span> &lt; 0.025)); # indicates no behavior in this group. Data that were not statistically significant <span class="html-italic">p</span> &gt; 0.05.</p>
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<p>Plasma cortisol concentration in <span class="html-italic">Astyanax lacustris</span> female (F) and male (M) in different groups: CTL/n (control group in neutral pH); Al/ac (aluminum group in acid pH); pH/ac (acid pH group). Data are presented as the mean ± standard error of the mean (M ± SEM). <sup>A,B,C,a,b</sup> Different uppercase letters indicate differences between females and males in different groups (males in CTL/n (<span class="html-italic">p</span> &lt; 0.011) and pH/ac (<span class="html-italic">p</span> &lt; 0.001) groups compared with Al/ac group; pH/ac (<span class="html-italic">p</span> &lt; 0.038) compared with CTL/n group), and lowercase letters indicate differences between females and males in the same group (CTL/n (<span class="html-italic">p</span> &lt; 0.001) and pH/ac (<span class="html-italic">p</span> = 0.004) groups compared with Al/ac group). Data that were not statistically significant <span class="html-italic">p</span> &gt; 0.05.</p>
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21 pages, 7763 KiB  
Article
The Antioxidant and Anti-Inflammatory Activities of the Methanolic Extract, Fractions, and Isolated Compounds from Eriosema montanum Baker f. (Fabaceae)
by Gaétan Tchangou Tabakam, Emmanuel Mfotie Njoya, Chika Ifeanyi Chukwuma, Samson Sitheni Mashele, Yves Martial Mba Nguekeu, Mathieu Tene, Maurice Ducret Awouafack and Tshepiso Jan Makhafola
Molecules 2024, 29(24), 5885; https://doi.org/10.3390/molecules29245885 - 13 Dec 2024
Viewed by 1028
Abstract
Background: Inflammation is a natural body’s defense mechanism against harmful stimuli such as pathogens, chemicals, or irradiation. But when the inflammatory response becomes permanent, it can lead to serious health problems. In the present study, the antioxidant and anti-inflammatory potentials of the Eriosema [...] Read more.
Background: Inflammation is a natural body’s defense mechanism against harmful stimuli such as pathogens, chemicals, or irradiation. But when the inflammatory response becomes permanent, it can lead to serious health problems. In the present study, the antioxidant and anti-inflammatory potentials of the Eriosema montanum methanolic extract (EMME), as well as its isolated fractions (FA-FJ) and compounds (17), were evaluated by using in vitro and cellular models. Methods: The total phenolic and flavonoid contents were determined using, respectively, Folin–Ciocalteu and aluminum chloride colorimetric methods, while 2,2′-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid (ABTS), 2,2′-diphenyl-1-picrylhy-drazyl (DPPH), and ferric ion reducing antioxidant power (FRAP) were used to determine the antioxidant activity. Thin Layer Chromatography (TLC) and column chromatography (CC) were used to isolate and purify the compounds and their elucidation using their NMR spectroscopic data. Results: EMME had moderate antioxidant and anti-inflammatory activities, while fraction FF showed much higher efficacy with IC50 values of 34.64, 30.60, 16.43, and 77.29 μg/mL against DPPH, ABTS, NO, and 15-LOX inhibitory activities, respectively. The EMME fraction was found to be very rich in flavonoids and phenolic compounds, with 82.11 mgQE/g and 86.77 mgGAE/g of dry extract, respectively. Its LC-MS profiling allowed us to identify genistin (5) as the most concentrated constituent in this plant species, which was further isolated together with six other known compounds, namely, n-hexadecane (1), heptacosanoic acid (2), tricosan-1-ol (3), lupinalbin A (4), d-pinitol (6), and stigmasterol glucoside (7). Given these compounds, genistin (5) showed moderate activity against reactive oxygen species (ROS) and NO production in LPS-stimulated RAW264.7 cells compared to EMME, which suggested a synergy of (5) with other compounds. To the best of our knowledge, compounds (1), (2), and (3) were isolated for the first time from this plant species. Full article
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<p>Extraction protocol, fractionation, and isolation of compounds from <span class="html-italic">E. montanum</span>.</p>
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<p>Chemical structures of compounds identified in <span class="html-italic">E. montanum</span>.</p>
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<p>Liquid chromatography–mass spectrometric (LC-MS) profile of <span class="html-italic">E. montanum</span> methanolic extract (<span class="html-italic">EMME</span>). Major compounds detected: Anopyranosylapigenin (t<sub>R</sub>: 7.585 min), genistin (t<sub>R</sub>: 7.902 min), and genistein (t<sub>R</sub>: 11.055 min).</p>
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<p>Nitric oxide (NO) production and cell viability in LPS-stimulated RAW 264.7 cells pre-treated with extract, fractions, and purified compounds. (<b>A</b>) The cytotoxic effect of tested samples was evaluated using MTT assay; (<b>B</b>) RAW 264.7 cells were pre-treated with tested samples at 100 µg/mL for 2 h, followed by exposure to 500 ng/mL of LPS for 24 h to quantify NO in cell supernatants. Each bar depicts the mean ± SD of three replicates (n = 3). One-way ANOVA combined Dunnett or Student–Newman–Keuls’s tests were used for data analysis. * <span class="html-italic">p</span> &lt; 0.05 vs. Ctrl. # <span class="html-italic">p</span> &lt; 0.05 vs. LPS, ns: non-significant.</p>
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<p>Bioactive samples’ concentration-dependent NO inhibitory action. The means ± SD of duplicate (n = 2) studies are shown for each bar. One-way ANOVA and either Dunnett’s or Student–Newman–Keuls tests were used to evaluate the data. # <span class="html-italic">p</span> &lt; 0.01 versus Ctrl. * <span class="html-italic">p</span> &lt; 0.01 about LPS.</p>
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<p>Reactive oxygen species (ROS) production in LPS-stimulated RAW 264.7 cells. RAW 264.7 cells were pre-treated with different concentrations (25, 50, and 100 µg/mL) of <span class="html-italic">E. montanum</span> methanolic extract (<span class="html-italic">EMME</span>), genistin, and ascorbic acid (AA) for two hours, then exposed to 200 ng/mL of LPS for twenty-four hours. Cell fluorescence was monitored at 485 nm (excitation) and 535 nm (emission) (<b>A</b>), and intracellular ROS levels were assessed using the DCFH-DA probe (10 µM). Percentages of negative control cells (<b>B</b>) are used to represent intracellular ROS levels. The means ± SD of three studies in triplicate are shown by each bar. One-way ANOVA and either Dunnett’s or Student–Newman–Keuls tests were used to evaluate the data. * <span class="html-italic">p</span> &lt; 0.05 vs. LPS, # <span class="html-italic">p</span> &lt; 0.05 vs. Ctrl.</p>
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19 pages, 8503 KiB  
Article
Using Random Forest Regression to Model the Spatial Distribution of Concentrations of Selected Metals in Groundwater in Forested Areas of the Wielkopolska National Park, Poland
by Michał Fiedler
Forests 2024, 15(12), 2191; https://doi.org/10.3390/f15122191 - 12 Dec 2024
Viewed by 457
Abstract
Monitoring groundwater pollution is an important issue in terms of analyzing threats to protected, environmentally valuable areas. The topographical and environmental characteristics of a given area are often mentioned among the factors affecting the dynamics and chemistry of groundwater. In this study, the [...] Read more.
Monitoring groundwater pollution is an important issue in terms of analyzing threats to protected, environmentally valuable areas. The topographical and environmental characteristics of a given area are often mentioned among the factors affecting the dynamics and chemistry of groundwater. In this study, the random forest regression (RFR) model was used to determine the spatial distribution of selected metals, such as aluminum, calcium, iron, potassium, magnesium, manganese, sodium, and zinc. In the role of indicators describing terrain variability, derivatives of the digital elevation model (DEM) were employed, with a spatial resolution of 5 m, describing the topography of the terrain on a local scale, such as, among others, slopes, the aspect and curvatures of slopes, the topographic position index, and the SAGA wetness index, as well as generalized values determined for each sampling point of the areas contributing their runoff. In addition, environmental parameters were taken into consideration: forest habitat types, the structure of soil cover, and the seasons when samples were collected. This study used samples collected from 15 wells located in forested areas of the Wielkopolska National Park on seven dates. The results obtained show that random forest can be used with very good results to model the spatial variability of the concentrations of aluminum, potassium, magnesium, manganese, and sodium in groundwater. However, in the case of calcium and zinc, no correlations were found between the adopted indicators describing the spatial variability of the area and their concentrations in groundwater. In addition, the degree of importance of each predictor was determined in order to rank their importance in modeling the concentration of each of the metals in groundwater. The summary ranking of predictors indicates that the strongest influence on the predicted concentration of metals in groundwater is exhibited by profile curvatures, planar curvatures, multiscale TPI, and then the habitat type of the forest. On the other hand, curvature classifications, soil composition, and seasonality exhibit the smallest generalized impact on the results of modeling. Full article
(This article belongs to the Special Issue Soil Pollution and Remediation of Forests Soil)
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<p>Location and DEM of the Wielkopolski Park Narodowy.</p>
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<p>Workflow for analysis of a single metal, using aluminum as an example. Part A is common to all metals.</p>
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<p>Topography of WPN.</p>
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<p>Topography of WPN. TPI Landforms: 1—streams, 2—midslope drainages, 3—upland drainages, 4—valleys, 5—plains, 6—open slopes, 7—upper slopes, 8—local ridges, 9—midslope ridges, 10—high ridges. Curvature class: 0—concave, 1—flat, 2—convex.</p>
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<p>Forest habitat types (FHT) and soil types. FHT: BMsw—fresh mixed coniferous forest, Bsw—fresh coniferous forest, LMsw—fresh mixed broadleaved forest, LMw—moist mixed broadleaved forest, LMb—swamp mixed broadleaved forest, Lsw—fresh broadleaved forest, Lw—moist broadleaved forest, Lł—riparian forest, Ol—alder and alder–ash forest; soil: gs—medium clay, gp—sandy loam, pg—clay sand, pl—loose sand, ps—light clay sand, płp—sandy silt, m—alluvia, tn—turf.</p>
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<p>Correlation between measured and predicted values of metal concentrations in the groundwater.</p>
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<p>Plot showing the importance of variables.</p>
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<p>Summarized importance of variables.</p>
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<p>Predicted concentrations of Al, Fe, and K in the groundwater.</p>
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<p>Predicted concentrations of Mn, Na, and Mg in the groundwater.</p>
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14 pages, 4426 KiB  
Article
Preparation of Alumina Oxo-Cluster/Cellulose Polymers and Dye Adsorption Application
by Henglong Tang, Simeng Yao, Zhu Long, Xuefei Yang, Pengxiang Si, Chang Sun and Dan Zhang
Materials 2024, 17(23), 6023; https://doi.org/10.3390/ma17236023 - 9 Dec 2024
Viewed by 621
Abstract
Aluminum oxide clusters (AlOCs) possess high surface areas and customizable pore structures, making them applicable in the field of environmental remediation. However, their practical use is hindered by stability issues, aggregation tendencies, and recycling challenges. This study presents an in -situ synthesis of [...] Read more.
Aluminum oxide clusters (AlOCs) possess high surface areas and customizable pore structures, making them applicable in the field of environmental remediation. However, their practical use is hindered by stability issues, aggregation tendencies, and recycling challenges. This study presents an in -situ synthesis of AlOCs on cellulose using a solvent thermal method. The resulting adsorbent’s structural and property profiles were thoroughly characterized using multiple analytical techniques. Batch adsorption experiments were performed to assess the adsorbent’s capacity and kinetics in removing selected dyes from aqueous solutions. Additionally, both real-environment simulation and regeneration experiments have been conducted to thoroughly assess the adsorbent’s reliability, stability, and practical applicability. The aim was to engineer an effective and recyclable adsorbent specifically tailored for dye-contaminated wastewater treatment. Full article
(This article belongs to the Special Issue Construction and Applications in Functional Polymers)
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<p>SEM images of the longitudinal sections (<b>a</b>) and cross-sections (<b>b</b>) of AlOC-15/Cellulose, as well as its EDX image (<b>c</b>); SEM images of the longitudinal sections (<b>d</b>) and cross-sections (<b>e</b>) of AlOC-20/Cellulose, along with its EDX image (<b>f</b>); SEM images of the longitudinal sections (<b>g</b>) and cross-sections (<b>h</b>) of AlOC-22/Cellulose, and its EDX image (<b>i</b>); SEM images of the longitudinal sections (<b>j</b>) and cross-sections (<b>k</b>) of AlOC-26-NC/Cellulose, as well as its EDX image (<b>l</b>).</p>
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<p>(<b>a</b>) BET analysis of the adsorbents, and (<b>b</b>) FT-IR spectra of natural balsa wood, TEMPO-oxidized wood, and the AlOCs/Cellulose.</p>
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<p>TG curves of AlOCs/Cellulose.</p>
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<p>The adsorption effects of (<b>a</b>) natural balsa wood and TEMPO-oxidized wood, and (<b>b</b>) AlOCs/Cellulose (pH 7, <span class="html-italic">m</span> = 10 mg, CV: 204.00 mg/L, MB: 159.93 mg/L, TB: 233.30 mg/L, RRB: 239.51 mg/L, CBK: 293.20 mg/L, MO: 163.67 mg/L, CR: 348.34 mg/L, and CLR: 191.22 mg/L, 298 K, 24 h).</p>
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<p>(<b>a</b>) the influence of solution pH on adsorption capacity (<span class="html-italic">m</span> = 10 mg, <span class="html-italic">C</span><sub>0</sub> = 491.00 mg/L, 298 K, 24 h); (<b>b</b>) Zeta potential of adsorbent at different pH.</p>
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<p>(<b>a</b>) Influence of contact time on the adsorption properties; (<b>b</b>) PFO and (<b>c</b>) PSO models for MO adsorption (pH 5, <span class="html-italic">m</span> = 10 mg, <span class="html-italic">C</span><sub>0</sub> = 3600.63 mg/L, 298 K, 24 h).</p>
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<p>(<b>a</b>) Influences of concentration on the adsorption properties of MO; (<b>b</b>) Langmuir and (<b>c</b>) Freundlich adsorption isotherm models for MO adsorption (pH 5, <span class="html-italic">m</span> = 10 mg, 298 K, 1230 min).</p>
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<p>(<b>a</b>) Effect of ionic strength on MO dye removal of AlOC-26-NC/Cellulose; (<b>b</b>) Effect of competing ions on MO dye removal and (<b>c</b>) Effect of humic acid on MO dye removal (pH 5, <span class="html-italic">m</span> = 10 mg, <span class="html-italic">C</span><sub>0</sub> = 163.67 mg/L, 298 K, 24 h).</p>
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<p>Reusability study of AlOC-26-NC/Cellulose (pH 5, <span class="html-italic">m</span> = 10 mg, <span class="html-italic">C</span><sub>0</sub> = 491.00 mg/L, 298 K, 24 h).</p>
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<p>Preparation of AlOCs modified wood.</p>
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11 pages, 4179 KiB  
Article
Water Sorption Properties and Hydrothermal Stability of Al-Containing Metal–Organic Frameworks CAU-10 and MIL-96 Studied Using Quasi-Equilibrated Thermodesorption
by Waclaw Makowski, Patrycja Gryta, Gabriela Jajko-Liberka, Monika Cieślik-Górna and Aleksandra Korzeniowska
Molecules 2024, 29(23), 5625; https://doi.org/10.3390/molecules29235625 - 28 Nov 2024
Viewed by 479
Abstract
A novel experimental technique, quasi-equilibrated temperature-programmed desorption and adsorption (QE-TPDA), was used to study the water sorption properties and hydrothermal stability of aluminum trimesate MIL-96 and aluminum isophthalate CAU-10, which have been selected due to their remarkable sorption properties. The QE-TPDA profiles of [...] Read more.
A novel experimental technique, quasi-equilibrated temperature-programmed desorption and adsorption (QE-TPDA), was used to study the water sorption properties and hydrothermal stability of aluminum trimesate MIL-96 and aluminum isophthalate CAU-10, which have been selected due to their remarkable sorption properties. The QE-TPDA profiles of water observed for MIL-96 and CAU-10 confirmed the hydrophilic nature of these materials. Complex QE-TPDA profiles indicate that water sorption in MIL-96 follows a three-step pore filling mechanism. The shape of single desorption peaks in the QE-TPDA profiles for CAU-10 confirms that water sorption involves a reversible phase transition. Based on the QE-TPDA profiles, the water adsorption heat was determined: 45–46 kJ/mol for CAU-10 and 43–56 kJ/mol for MIL-96, in the latter case depending on the adsorption extent. Hydrothermal stability tests revealed that MIL-96 retained its stable porosity-related sorption capacity for water after hydrothermal treatment up to 290 °C. Gradual changes in the QE-TPDA profiles due to the hydrothermal treatment above 290 °C, with decreasing the high-temperature desorption peak and increasing the low-temperature one, indicate minor structural changes occurring in this material. Only after 410 °C treatment was fast degradation of MIL-96 observed. CAU-10 exhibited high and unchanged hydrothermal stability up to 400 °C. Full article
(This article belongs to the Special Issue Porous Organic Materials: Design and Applications: Volume II)
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<p>The isotherms of water adsorption and desorption measured at 25 °C (<b>A</b>) and QE-TPDA profiles (<b>B</b>) of water observed for CAU-10, as well as the integral adsorption and desorption curves (<b>C</b>), based on the thermodesorption profiles. Experimental details of QE-TPDA: inlet partial pressure of water p<sub>in</sub> = 1.9 kPa, sample mass m = 3.3 mg, carrier gas (He) flowrate F = 7.2 cm<sup>3</sup>/min.</p>
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<p>The QE-TPDA profiles from <a href="#molecules-29-05625-f001" class="html-fig">Figure 1</a>B transformed according to the van’t Hoff equation. The formulae in the insets indicate the values of the adsorption enthalpy and entropy and correlation coefficients obtained by linear regression of overlapping fragments of the profiles.</p>
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<p>The isotherms of water adsorption and desorption (<b>A</b>) and QE-TPDA profiles (<b>B</b>) of water observed for MIL-96, as well as the integral adsorption and desorption curves (<b>C</b>), based on the QE-TPDA profiles from B. Experimental details of QE-TPDA: inlet partial pressure of water p<sub>in</sub> = 2.4 kPa, sample mass m = 5.7 mg, carrier gas (He) flowrate F = 7.2 cm<sup>3</sup>/min.</p>
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<p>The QE-TPDA profiles (<b>A</b>) of water observed in the new experimental system for MIL-96 at a heating/cooling rate of 2 °C/min at different inlet partial pressures, and the corresponding integral desorption curves (<b>B</b>). The points indicate data found for the preset adsorbed amount values (from 25.5 to 209.5 mg/g, with 11.5 mg/g interval). Experimental details: sample mass m = 5.5 mg, carrier gas (N<sub>2</sub>) flowrate F = 8.0 cm<sup>3</sup>/min.</p>
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<p>(<b>A</b>) The transformed adsorption isosteres of water on MIL-96 calculated from data indicated as points in <a href="#molecules-29-05625-f004" class="html-fig">Figure 4</a>. (<b>B</b>) Isosteric adsorption heat of water on MIL-96 obtained from analysis of the adsorption isosteres. The blue line indicates the values of the condensation heat of water, corresponding to the average temperatures of particular isosteres.</p>
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<p>Illustration of the principle of the hydrothermal stability test: the evolution of the sample temperature and the detector signal during a single desorption–adsorption cycle. This example corresponds to the first cycle recorded for MIL-96 (see <a href="#molecules-29-05625-f007" class="html-fig">Figure 7</a>). The diagnostic segment and the hydrothermal treatment segment are indicated by thick black and dark red lines, respectively.</p>
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<p>Results of the hydrothermal stability test for MIL-96: selected QE-TPD profiles corresponding to the last cycle in the 3-cycle sequences (<b>A</b>) and evolution of the hydrothermal treatment temperature and sorption capacity with the cycle number (<b>B</b>). Experimental details: heating rate β = 2 °C/min, inlet partial pressure of water p<sub>in</sub> = 2.8 kPa, sample mass m = 3.0 mg, carrier gas (N<sub>2</sub>) flowrate F = 8.0 cm<sup>3</sup>/min.</p>
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<p>Powder XRD patterns of MIL-96 samples after the QE-TPDA hydrothermal stability tests interrupted at different temperatures compared with the pattern recorded for the as-synthesized sample.</p>
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<p>Results of the hydrothermal stability test for CAU-10: selected QE-TPD profiles corresponding to the last cycle in the 3-cycle sequence (<b>A</b>) and evolution of the hydrothermal treatment temperature and sorption capacity with the cycle number (<b>B</b>). Experimental details: heating rate β = 1 °C/min, inlet partial pressure of water p<sub>in</sub> = 2.8 kPa, sample mass m = 3.0 mg, carrier gas flowrate F = 8.0 cm<sup>3</sup>/min.</p>
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<p>Powder XRD patterns of CAU-10 samples before and after the QE-TPDA of H<sub>2</sub>O measurements.</p>
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15 pages, 3074 KiB  
Article
A Case Study on Integrating an Eco-Design Tool into the Construction Decision-Making Process
by Kétlin Cornely, Guilherme Ascensão and Victor M. Ferreira
Appl. Sci. 2024, 14(22), 10583; https://doi.org/10.3390/app142210583 - 16 Nov 2024
Viewed by 1159
Abstract
To enhance the sustainability of construction and meet the sector’s environmental agenda, it is essential to comprehensively scrutinize the environmental, social, and economic impacts of construction projects from the project’s design stage. Such assessment is of utmost importance to minimize the impacts of [...] Read more.
To enhance the sustainability of construction and meet the sector’s environmental agenda, it is essential to comprehensively scrutinize the environmental, social, and economic impacts of construction projects from the project’s design stage. Such assessment is of utmost importance to minimize the impacts of both new construction and rehabilitation projects and is particularly critical during the selection of building materials and construction solutions. This work reports improvements in functionality and user-friendliness of an eco-design tool (UAveiroGreenBuilding) targeting the construction/rehabilitation sector and previously developed within our research group. The optimized version of the eco-design tool underwent validation through the assessment of competitive window frame materials (e.g., wood, PVC, and aluminum) for potential implementation in a rehabilitation project. Windows with PVC frames were identified as the preferred window configuration due to their superior environmental performance and favorable economic profile. Additionally, a digital communication interface was developed to connect the eco-design tool with building information modeling (BIM) projects, achieved through a routine integrated using a Dynamo application. Such successful integration not only streamlined and expedited the data transfer process by obviating the need for manual input but it also enabled the storage of environmental data throughout the life cycle of the project using a simple and reliable data storage protocol. Full article
(This article belongs to the Section Civil Engineering)
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<p>University of Aveiro Campus. (<b>a</b>) The red line highlights the Central Technical Area and (<b>b</b>) the plant of the Central Technical Area.</p>
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<p>Normalized environmental impact of different window frame materials.</p>
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<p>Normalized resource consumption of different window frame materials’ (<b>a</b>) consumption of non-renewable resources and (<b>b</b>) consumption of renewable resources.</p>
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<p>Economic assessment of different window frame solutions.</p>
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<p>Dynamo routine structure.</p>
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<p>Parameters entered into BIM (<b>a</b>) and imported data after executing the developed Dynamo routine (<b>b</b>).</p>
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17 pages, 4492 KiB  
Article
Advanced Numerical Modeling and Experimental Analysis of Thermal Gradients in Gleeble Compression Configuration for 2017-T4 Aluminum Alloy
by Olivier Pantalé, Yannis Muller and Yannick Balcaen
Appl. Mech. 2024, 5(4), 839-855; https://doi.org/10.3390/applmech5040047 - 13 Nov 2024
Viewed by 914
Abstract
Gleeble thermomechanical simulators are widely utilized tools for the investigation of high-temperature deformation behavior in materials. However, temperature gradients that develop within the specimen during Gleeble compression tests have the potential to result in non-uniform deformation, which may subsequently impact the accuracy of [...] Read more.
Gleeble thermomechanical simulators are widely utilized tools for the investigation of high-temperature deformation behavior in materials. However, temperature gradients that develop within the specimen during Gleeble compression tests have the potential to result in non-uniform deformation, which may subsequently impact the accuracy of the measured mechanical properties. This study presents an experimental and numerical investigation of the temperature fields in 2017-T4 aluminum alloy specimens prior to Gleeble compression tests at temperatures ranging from 300 °C to 500 °C utilizing uniform temperature distribution (ISO-T) tungsten carbide anvils. The use of multiple thermocouples, welded to both the specimen and anvils, offers valuable insights into the temperature gradients and their evolutions. A coupled thermal–electrical finite-element model was developed in Abaqus for the purpose of simulating the resistive heating process. A user amplitude subroutine (UAMP) is implemented to regulate the heating based on a proportional–integral–derivative (PID) algorithm that modulates the current density to follow the specified temperature profile. The numerical results demonstrate that the temperature gradients within the specimen at the end of the heating process, reaching a temperature of 400 °C, are minimal, with values below 1.9 °C. This is in accordance with the experimental observations. The addition of graphite foils between the specimen and anvils has been shown to effectively reduce the gradients. The use of the measured anvil temperature as a boundary condition, rather than a constant value of 20 °C, has been demonstrated to improve the agreement between the simulated and experimental cooling curves. The modeling approach provides a framework for quantifying temperature gradients in Gleeble compression specimens and for assessing their impact on the measured constitutive response of materials at elevated temperatures. Full article
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<p>Closed view of the specimen inside the Gleeble thermomechanical simulator.</p>
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<p>Gleeble compression test configuration: (<b>left</b>) global view and (<b>right</b>) closed view of the specimen and the anvils.</p>
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<p>Experimental results extracted from the Gleeble.</p>
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<p>Overshoots extracted from the Gleeble (zoom).</p>
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<p>Electro-thermal axi-symmetric model used for the numerical simulations. Where <math display="inline"><semantics> <mrow> <mi>i</mi> <mo>(</mo> <mi>t</mi> <mo>)</mo> </mrow> </semantics></math>: applied current density, <math display="inline"><semantics> <mrow> <mi>T</mi> <msub> <mi>c</mi> <mn>1</mn> </msub> </mrow> </semantics></math>: monitored and regulated temperatures using control thermocouple, <math display="inline"><semantics> <mrow> <mi>T</mi> <msub> <mi>c</mi> <mn>2</mn> </msub> </mrow> </semantics></math>: the axial thermal gradient within the specimen during the experiment, <math display="inline"><semantics> <mrow> <mi>T</mi> <msub> <mi>c</mi> <mn>3</mn> </msub> </mrow> </semantics></math>: K thermocouple, positioned on the rear surface of the anvil backer.</p>
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<p>The UAMP F77 subroutine used to compute the current density <math display="inline"><semantics> <mrow> <mi>i</mi> <mo>(</mo> <mi>t</mi> <mo>)</mo> </mrow> </semantics></math> for <math display="inline"><semantics> <mrow> <mn>400</mn> <mo> </mo> <mo>°</mo> <mi mathvariant="normal">C</mi> </mrow> </semantics></math>.</p>
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<p>Temperature contourplot in the anvil and the sample at the end of the heating phase (<math display="inline"><semantics> <mrow> <mi>t</mi> <mo>=</mo> <mn>1100</mn> <mspace width="3.33333pt"/> <mi mathvariant="normal">s</mi> <mspace width="0.277778em"/> </mrow> </semantics></math>) for the constant cooling condition.</p>
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<p>Temperature contourplot in the sample and a portion of the anvil at the end of the heating phase (<math display="inline"><semantics> <mrow> <mi>t</mi> <mo>=</mo> <mn>1100</mn> <mspace width="3.33333pt"/> <mi mathvariant="normal">s</mi> </mrow> </semantics></math>) for the constant cooling condition.</p>
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<p>Temporal evolution of the numerically calculated and experimentally measured temperatures <math display="inline"><semantics> <mrow> <mi>T</mi> <msub> <mi>c</mi> <mn>1</mn> </msub> </mrow> </semantics></math>, the current density <span class="html-italic">i</span>, and the heating power <math display="inline"><semantics> <msup> <mi>P</mi> <mi>exp</mi> </msup> </semantics></math> for the constant cooling condition.</p>
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<p>Temperature contourplot in the sample and a portion of the anvil at the end of the heating phase (<math display="inline"><semantics> <mrow> <mi>t</mi> <mo>=</mo> <mn>1100</mn> <mspace width="3.33333pt"/> <mi mathvariant="normal">s</mi> <mspace width="0.277778em"/> </mrow> </semantics></math>) for the variable cooling condition.</p>
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<p>Temporal evolution of the numerically calculated and experimentally measured temperatures <math display="inline"><semantics> <mrow> <mi>T</mi> <msub> <mi>c</mi> <mn>1</mn> </msub> </mrow> </semantics></math>, the current density <span class="html-italic">i</span>, and the heating power <math display="inline"><semantics> <msup> <mi>P</mi> <mi>exp</mi> </msup> </semantics></math> for the variable cooling condition.</p>
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17 pages, 2983 KiB  
Article
Hard-Anodized Aluminum Alloy: Wear Properties in Vegetable Oils
by Chiara Soffritti, Annalisa Fortini, Enrico Baroni, Mattia Merlin and Gian Luca Garagnani
Lubricants 2024, 12(11), 383; https://doi.org/10.3390/lubricants12110383 - 5 Nov 2024
Viewed by 765
Abstract
The present study examines the tribological behavior of an EN AW-4006 aluminum alloy subjected to two innovative hard anodizing processes involving the sealing of anodic oxide pores with Ag+ ions and tested in lubricated conditions. Four plant-based lubricants with different concentrations of [...] Read more.
The present study examines the tribological behavior of an EN AW-4006 aluminum alloy subjected to two innovative hard anodizing processes involving the sealing of anodic oxide pores with Ag+ ions and tested in lubricated conditions. Four plant-based lubricants with different concentrations of fatty acids were considered. Wear tests were conducted using a ball-on-disk tribometer, employing a constant frequency oscillatory motion at 2 Hz and a maximum linear speed of 0.1 m/s. The investigation explores the influence of applied loads (5 N, 10 N, and 15 N) on the resulting coefficient of friction. Through a Design of Experiments methodology, the most influential factors affecting the coefficient of friction are identified. The results indicate that hard anodizing processes and applied load affect the coefficient of friction during wear testing as the main factor of influence. High values of the Unsaturation Number led to a high coefficient of friction at 5 N. Wavy-shaped profile tracks were detected at 10 and 15 N, leading to high specific wear rate values and the failure of the anodized layer. Full article
(This article belongs to the Special Issue Friction and Wear of Alloys)
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<p>Optical micrographs in the cross-section of the anodized layers before wear tests. The yellow arrows indicate uniformly distributed voids and macro-pores.</p>
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<p>Dynamic viscosity of the vegetable oils at the three different temperatures: (<b>a</b>) 25 °C, (<b>b</b>) 40 °C, and (<b>c</b>) 100 °C.</p>
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<p>Representative COF evolution against sliding distance at the different applied loads and for a G sample lubricated with (<b>a</b>) olive oil and (<b>b</b>) peanut oil.</p>
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<p>Relationship between COF and their respective WR values for (<b>a</b>) G and (<b>b</b>) GP anodized layers.</p>
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<p>Representative VPSEM micrographs of the wear tracks on the anodized layers after wear tests at applied loads of 5 N for (<b>a</b>) G and (<b>b</b>) GP samples. The white arrows show wide cracks alongside the sliding direction.</p>
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<p>Representative VPSEM micrographs of the wear tracks on the anodized layers after wear tests at applied loads of (<b>a</b>,<b>b</b>) 10 N and (<b>c</b>,<b>d</b>) 15 N. (<b>a</b>,<b>c</b>) refer to G wear tracks obtained under sunflower oil lubrication. (<b>b</b>,<b>c</b>) refer to GP wear tracks obtained under sunflower oil lubrication. The white arrows in (<b>a</b>,<b>b</b>) show wide cracks alongside the sliding direction. In (<b>c</b>,<b>d</b>), the yellow arrows indicate cracked junctions between depression zones, whereas the red circle shows thick cracks longitudinal and transverse to the sliding direction.</p>
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<p>Representative VPSEM micrograph showing the detail of the cracked wavy-shaped profile of the worn anodized layers after wear tests at the highest loads, together with semi-quantitative EDS analysis at different positions (blue and red arrows) of the wear track.</p>
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15 pages, 4061 KiB  
Article
A Viability Study of Thermal Pre-Treatment for Recycling of Pharmaceutical Blisters
by Mertol Gökelma, Fabian Diaz, İrem Yaren Çapkın and Bernd Friedrich
Sustainability 2024, 16(20), 8968; https://doi.org/10.3390/su16208968 - 16 Oct 2024
Cited by 1 | Viewed by 1019
Abstract
Pharmaceutical packaging is one of the most used packaging types which contains aluminum and plastics. Due to increasing amounts of waste and rising environmental concerns, recycling approaches are being investigated. Since blisters usually contain a balanced amount of plastics and metals, most of [...] Read more.
Pharmaceutical packaging is one of the most used packaging types which contains aluminum and plastics. Due to increasing amounts of waste and rising environmental concerns, recycling approaches are being investigated. Since blisters usually contain a balanced amount of plastics and metals, most of the approaches focus on recycling only one material. Therefore, more sustainable recycling approaches which recover both plastic and aluminum fractions are needed. This study investigates the thermal behavior and degradation mechanisms of plastic-rich and aluminum-rich pharmaceutical blisters using various analytical techniques. Structural characterization revealed that plastic-rich blisters have a thicker profile with plastic and aluminum layers, while aluminum-rich blisters consist of plastic layers between aluminum sheets. Thermal degradation analysis showed two main stages for both types: plastic-rich blisters (polyvinyl chloride) exhibited significant weight loss and long-chain hydrocarbon formation between 210 and 285 °C, and aluminum-rich blisters (polyamide/nylon) degraded from 240 to 270 °C. Differential Scanning Calorimetry and Fourier Transform Infrared Spectroscopy analyses confirmed the endothermic behavior of such a transformation. The gas emissions analysis indicated an increased formation of gasses from the thermal treatment of plastic-rich blisters, with the presence of oxygen leading to the formation of carbon dioxide, water, and carbon monoxide. Thermal treatment with 5% O2 in the carrier gas benefited plastic-rich blister treatment, reducing organic waste by up to 80% and minimizing burning risk, leveraging pyrolytic carbon for protection. This method is unsuitable for aluminum-rich blisters, requiring reduced oxygen or temperature to prevent pyrolytic carbon combustion and aluminum oxidation. Full article
(This article belongs to the Section Waste and Recycling)
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<p>Types of pharmaceutical blisters: (<b>a</b>) plastic-rich, (<b>b</b>) aluminum-rich.</p>
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<p>Schematic of the furnace used for laboratory-scale thermal pre-treatment trials.</p>
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<p>SEM images and EDS mapping of the blisters from the cross-sections of (<b>a</b>) plastic-rich and (<b>b</b>) aluminum-rich blisters.</p>
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<p>Weight loss, derivative thermogravimetry (DTG), and heat flow during TGA-DSC analysis of thermal pre-treatment of (<b>A</b>) plastic-rich blisters and (<b>B</b>) aluminum-rich blisters.</p>
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<p>FTIR analysis of plastic fractions of plastic-rich and aluminum-rich blisters.</p>
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<p>Temperature profile and main species concentration (ppm) during thermal treatment of plastic-rich blisters using 0%, 5%, and 20% oxygen heated at temperatures ranging from 600 °C/h to 800 °C.</p>
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<p>Temperature profile and main species concentration (ppm) during thermal treatment of aluminum-rich blisters using 0%, 5%, and 20% oxygen heated at temperatures ranging from 600 °C/h to 800 °C.</p>
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<p>Weight loss after thermal treatment of (<b>a</b>) plastic-rich and (<b>b</b>) aluminum-rich blisters with 0, 5, and 20% O<sub>2</sub>.</p>
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17 pages, 7147 KiB  
Article
Non-Destructive Testing of Joints Used in Refrigerated Vehicle Bodies
by Jakub Kowalczyk and Przemysław Tyczewski
Appl. Sci. 2024, 14(20), 9364; https://doi.org/10.3390/app14209364 - 14 Oct 2024
Viewed by 653
Abstract
This paper focuses on the non-destructive evaluation of adhesive joints used in vehicles designed for transporting food products. The research and analysis were limited to the joints used in connecting elements of the cargo space. Two non-destructive methods were employed in the study: [...] Read more.
This paper focuses on the non-destructive evaluation of adhesive joints used in vehicles designed for transporting food products. The research and analysis were limited to the joints used in connecting elements of the cargo space. Two non-destructive methods were employed in the study: ultrasonic and thermographic techniques. Both methods confirmed the feasibility of evaluating adhesive joints in the construction of food transport vehicles, with the thermographic method proving to be much faster in identifying large areas of deadhesion in the plating. The ultrasonic method, on the other hand, allows for the inspection of sheathing and aluminum profiles. The predefined decibel drop in the height of the first two pulses on the ultrasonic defectoscope screen for areas with high-quality joints was less than 3.5 dB. In contrast, for areas with adhesion-related damage, the decibel drop in the first two pulses exceeded 4.5 dB. Full article
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<p>Research plan.</p>
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<p>Areas selected for study.</p>
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<p>The dimensions of the sample along with the plotting of the measurement points (red circle—the area in which the simulation of the separation of insulation from the sheet was performed).</p>
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<p>View of the sample: (<b>a</b>) model, (<b>b</b>) photo of the sample.</p>
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<p>View of the specimen (<b>a</b>) after removing some of the of the plating and insulation; (<b>b</b>) after the insulation layer was pasted in place.</p>
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<p>Sample used in the study: 1—aluminum alloy, 2—anodized aluminum alloy, and 3—additional profile for calibration of apparatus and pilot studies.</p>
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<p>Sample used in the study: (<b>a</b>) dimensions, (<b>b</b>) model.</p>
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<p>Evaluation of the feasibility of using ultrasonic probes: (<b>a</b>) test bench view—CUD ultrasonic flaw detector, (<b>b</b>) test bench view—USM35XS ultrasonic flaw detector, (<b>c</b>) display view of the CUD, (<b>d</b>) display view of the USM35XS.</p>
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<p>The idea of determining an ultrasonic measure.</p>
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<p>Assessing the effect of thickness on the ultrasonic measure of joint quality (<span style="color:red">•</span> measurement point).</p>
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<p>Effect of insulation layer thickness on ultrasonic measure.</p>
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<p>Results of fundamental tests on the plating of a temperature-controlled transport vehicle.</p>
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<p>Thermal imaging test results for sheathing.</p>
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<p>Thermal imaging test results for profiles.</p>
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12 pages, 1743 KiB  
Article
Protective Effects of Wild Sulla coronaria (Fabaceae) Flowers Phytocomplex in Human Dermal Fibroblasts Stimulated with Interleukin-1β
by Giuseppe Antonio Malfa, Simone Bianchi, Vivienne Spadaro, Ekaterina Kozuharova, Pasquale Marino, Francesco Pappalardo, Claudia Di Giacomo and Rosaria Acquaviva
Plants 2024, 13(19), 2748; https://doi.org/10.3390/plants13192748 - 30 Sep 2024
Viewed by 884
Abstract
Sulla coronaria is indigenous to the Mediterranean region. It is grown as fodder in southern Italy because it contains various secondary metabolites with beneficial activities on animals. Recently, its potential use in cosmeceutical treatments for skin problems was reported. In this scenario, to [...] Read more.
Sulla coronaria is indigenous to the Mediterranean region. It is grown as fodder in southern Italy because it contains various secondary metabolites with beneficial activities on animals. Recently, its potential use in cosmeceutical treatments for skin problems was reported. In this scenario, to contribute to a possible cosmeceutical application, we characterized the phytochemical profile of Sulla coronaria flowers’ hydroalcoholic extract by HPLC-DAD, Folin-Ciocalteu, Aluminum Chloride methods, DPPH assay, and, for the first time, we evaluated the antioxidant and anti-inflammatory activities on dermal fibroblasts. The phytochemical analysis confirmed the significant content of phenolic compounds (TPC 69.8 ± 0.6 mg GAE/g extract, TFC 15.07 mg CE/g extract) and the remarkable presence of rutin, quercetin, and isorhamnetin derivatives that give to the phytocomplex a good antioxidant activity as highlighted by the DPPH assay (IC50 of 8.04 ± 0.5 µg/mL). Through the reduction in NO• and ROS levels in human dermal fibroblasts, the biological tests demonstrated both the safety of the extract and its ability to counteract the inflammatory state generated by Interleukin-1β exposure. Our findings indicate that the antioxidant activities of the phytocomplex are strictly related to the anti-inflammatory action of the Sulla coronaria flowers extract, confirming that this plant could be a valuable source of bioactive molecules for cosmeceutical and nutraceutical applications. Full article
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<p>Blooming of wild <span class="html-italic">Sulla coronaria</span> plant at the collection site (Corleone, Palermo, Italy).</p>
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<p>HPLC-DAD phytochemical fingerprint of <span class="html-italic">Sulla coronaria</span> flower hydroalcoholic extract. Column: Ascentis Express C18, 15 cm × 4.6 mm, 2.7 µm d.p. The numbers indicating peaks refer to the identified compounds reported in <a href="#plants-13-02748-t002" class="html-table">Table 2</a>.</p>
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<p>Aglycone chemical structures of the identified compounds in <span class="html-italic">Sulla coronaria</span> flower hydroalcoholic extract.</p>
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<p>Cytotoxic effect of <span class="html-italic">Sulla coronaria</span> flower hydroalcoholic extract on HDF cells. An MTT test was performed on HDFs treated with different concentrations of extract (from 10 to 1000 µg/mL) for 24 h. Data are represented as the means ± S.D. of three independent experiments. Confidence intervals calculated by one-way ANOVA test: * Significant vs. untreated control cells.</p>
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<p>ROS production in HDF untreated cells (Ctr), treated for 12 h with IL-1β (10 ng/mL), and pre-treated for 24 h with the extract (50–100–200 μg/mL). Results are expressed as the percentage of the intensity of fluorescence (I.F.) <span class="html-italic">vs</span> Ctr. Values are the mean ± S.D. of three experiments in triplicate. Confidence intervals calculated by one-way ANOVA test: * Significant vs. untreated control cells: <span class="html-italic">p</span> &lt; 0.05; # Significant vs. IL-1β-Stimulated cells: <span class="html-italic">p</span> &lt; 0.05.</p>
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<p>Effect of <span class="html-italic">Sulla coronaria</span> flower extract on NO• production in HDF cells. A Griess assay was performed on the supernatant of IL-1β-stimulated cells non-treated and treated with the extract (50, 100, and 200 µg/mL) for 24 h. Data are represented as the means ± SD of three independent experiments. Confidence intervals calculated by one-way ANOVA test: * Significant vs. untreated control cells: <span class="html-italic">p</span> &lt; 0.05; # Significant vs. IL-1β-Stimulated cells: <span class="html-italic">p</span> &lt; 0.05.</p>
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