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20 pages, 3992 KiB  
Article
Encapsulation of Inositol Hexakisphosphate with Chitosan via Gelation to Facilitate Cellular Delivery and Programmed Cell Death in Human Breast Cancer Cells
by Ilham H. Kadhim, Adeolu S. Oluremi, Bijay P. Chhetri, Anindya Ghosh and Nawab Ali
Bioengineering 2024, 11(9), 931; https://doi.org/10.3390/bioengineering11090931 (registering DOI) - 17 Sep 2024
Abstract
Inositol hexakisphosphate (InsP6) is the most abundant inositol polyphosphate both in plant and animal cells. Exogenous InsP6 is known to inhibit cell proliferation and induce apoptosis in cancerous cells. However, cellular entry of exogenous InsP6 is hindered due to [...] Read more.
Inositol hexakisphosphate (InsP6) is the most abundant inositol polyphosphate both in plant and animal cells. Exogenous InsP6 is known to inhibit cell proliferation and induce apoptosis in cancerous cells. However, cellular entry of exogenous InsP6 is hindered due to the presence of highly negative charge on this molecule. Therefore, to enhance the cellular delivery of InsP6 in cancerous cells, InsP6 was encapsulated by chitosan (CS), a natural polysaccharide, via the ionic gelation method. Our hypothesis is that encapsulated InsP6 will enter the cell more efficiently to trigger its apoptotic effects. The incorporation of InsP6 into CS was optimized by varying the ratios of the two and confirmed by InsP6 analysis via polyacrylamide gel electrophoresis (PAGE) and atomic absorption spectrophotometry (AAS). The complex was further characterized by Scanning Electron Microscopy (SEM) and Fourier Transform Infrared Spectroscopy (FTIR) for physicochemical changes. The data indicated morphological changes and changes in the spectral properties of the complex upon encapsulation. The encapsulated InsP6 enters human breast cancer MCF-7 cells more efficiently than free InsP6 and triggers apoptosis via a mechanism involving the production of reactive oxygen species (ROS). This work has potential for developing cancer therapeutic applications utilizing natural compounds that are likely to overcome the severe toxic effects associated with synthetic chemotherapeutic drugs. Full article
(This article belongs to the Special Issue Advances in Hydrogels for Tissue Engineering Applications)
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Graphical abstract

Graphical abstract
Full article ">Figure 1
<p>Schematic depiction of the concept of cellular entry of exogenously administered InsP<sub>6</sub> after encapsulation with chitosan by ionic gelation to shield off the negative charge. Note that the encapsulated InsP<sub>6</sub> enters the cell through cell membrane, whereas negatively charged free InsP<sub>6</sub> is unable to enter the cell membrane.</p>
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<p>Schematic illustration of the preparation of the CS:InsP<sub>6</sub> nanomaterial complex by ionic gelation. Chitosan dissolved in acetic acid (5.0 mg/mL) and InsP<sub>6</sub> dissolved in deionized water (5.0 mg/mL) were mixed in varying proportions and stirred for 30 min followed by pH adjustment. The CS:InsP<sub>6</sub> complex was purified by centrifugation and washing with ethanol and lyophilized to dry powder.</p>
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<p>Detection of InsP<sub>6</sub> contents in the CS:InsP<sub>6</sub> complex by PAGE. Optimization of InsP<sub>6</sub> incorporation in chitosan was carried out by varying the ratios of CS:InsP<sub>6</sub> (<b>B</b>). Standard InsP<sub>6</sub> with known concentrations were also run in parallel to establish the linearity of detection (<b>A</b>). Band densities were analyzed by image J software. (<b>B</b>) shows the amounts of InsP<sub>6</sub> detected in the samples with various ratios of CS:InsP<sub>6</sub> applied on the gel. The maximum amount of InsP<sub>6</sub> (0.49 μg) was detected in the sample with a CS:InsP<sub>6</sub> ratio of 2.5:1.0. This amount (0.49 μg), when calculated using the dilution factor of the samples loaded on the gel, provides a total incorporation of 49 ug InsP<sub>6</sub> per mg CS. Data shown are a representative of at least three independent experiments with similar results. The error bars are not shown as the data shown are from a single experiment repeated at least three times.</p>
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<p>SEM images of CS (<b>A</b>) and the CS:InsP<sub>6</sub> complex (<b>B</b>). Arrows point to the empty spaces in CS (<b>A</b>) that were perhaps filled by InsP<sub>6</sub> (<b>B</b>), showing morphological changes following encapsulation. The CS:InsP<sub>6</sub> complex at a ratio of 2.5:1.0 was used for SEM analysis in (<b>B</b>). Electron micrographs shown are representative images seen in replicate experiments with similar results.</p>
Full article ">Figure 5
<p>FTIR spectra of (<b>a</b>) InsP<sub>6</sub>, (<b>b</b>) CS, and (<b>c</b>) encapsulated complex with a CS:InsP<sub>6</sub> ratio of 2.5:1.0. Note that the spectral properties of the characteristic bands at specific wavenumbers in InsP<sub>6</sub> (<b>a</b>) and CS (<b>b</b>) are changed upon encapsulation (<b>c</b>).</p>
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<p>Cellular uptake of encapsulated InsP<sub>6</sub>. Band intensity was analyzed by image J software. (<b>A</b>) shows quantitative detection of InsP<sub>6</sub> in the CS:IsP<sub>6</sub> complex with a CS:InsP<sub>6</sub> ratio of 2.5:1.0. A volume of 5, 10, and 20 µL of the complex loaded on the gel gave 0.15, 0.36, and 0.64 µg InsP<sub>6</sub>, respectively, showing a concentration-dependent linear increase in the detection of InsP<sub>6</sub> in the complex. (<b>B</b>) shows a significant increase in InsP<sub>6</sub> uptake by MCF-7 cells using the encapsulated complex with a CS:InsP<sub>6</sub> ratio of 2.5:1.0 as compared to corresponding free InsP<sub>6</sub> and CS. Data shown are representative of experiments performed independently at least three times with similar results. Statistical analysis is not shown as the data are from a representative experiment.</p>
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<p>Dose- and time-dependent induction of cell viability in MCF-7 cells by encapsulated InsP<sub>6</sub> treatment. Cell viability was determined at 24 h (<b>A</b>), 48 h (<b>B</b>), and 72 h (<b>C</b>) by MTT assay using the given doses of free InsP<sub>6</sub> (1.0–4.0 µM) and equivalent amounts of the CS: InsP<sub>6</sub> complex that would give similar doses of free InsP<sub>6</sub>. Data are shown as means ± SD from three independent experiments. All experimental values were statistically compared with their respective controls to determine any significant differences. Only treatment with 4 µM encapsulated InsP<sub>6</sub> gave a significant difference as compared with 4 µM free InsP<sub>6</sub>. * <span class="html-italic">p</span> value ≤ 0.001 or ** <span class="html-italic">p</span> ≤ 0.0001 show significantly different values as compared to the respective controls.</p>
Full article ">Figure 8
<p>Effect of encapsulated InsP<sub>6</sub> on apoptosis. MCF-7 cells were incubated with 4 µM of encapsulated InsP<sub>6</sub> for 72 h to induce apoptosis. Etoposide (100 µM) was used as a positive control. (<b>A</b>) MCF-7 cells were stained with acridine orange/ethidium bromide and visualized under UV light using a fluorescent microscope. (<b>B</b>) The percentage of apoptosis was determined by counting 200–300 live (green) and/or dead (red) cells. Values shown are mean ±SD from three experiments, each performed in triplicate. ** <span class="html-italic">p</span> value ≤ 0.001 as compared to the control.</p>
Full article ">Figure 9
<p>Effect of encapsulated InsP<sub>6</sub> on ROS generation. MCF-7 cells were treated with 4 µM free InsP<sub>6</sub> equivalent of the encapsulated CS:InsP<sub>6</sub> complex for 72 h in a 96-well microplate. Etoposide (100 µM) was used as a positive control. Cells were then stained with 10 µM DCFH-DA and fluorescence intensity was recorded using a fluorescence microplate reader. Values shown are mean ± SD from three independent experiments, each performed in triplicate. * <span class="html-italic">p</span> value of ≤0.0001 was considered significantly different compared to the control.</p>
Full article ">Figure 10
<p>Determination of specificity of encapsulated InsP<sub>6</sub>-induced apoptosis by flow cytometry (<b>A</b>). Apoptosis was measured by using a commercially available Vybrant apoptosis assay kit #4. Live cells - are shown as green in lower left quadrant and apoptotic cells are shown as blue in <b>lower and upper right</b> quadrant. Necrotic cells give a red color which are expected to show up in upper left quadrant. The data shown are representative of an experiment repeated at least three times with similar results. (<b>B</b>) shows statistical analysis results of the flow cytometry data showing mean ± standard deviation (SD) from three independent experiments. The % apoptosis values were obtained by combining early and late apoptosis values from the lower and upper right quadrants, respectively. One-way ANOVA with multiple comparisons was used to determine values that were statistically significant. **** <span class="html-italic">p</span> &lt; 0.0001 was considered statistically significant values compared with their respective controls.</p>
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25 pages, 6904 KiB  
Article
Housing Market Segmentation as a Driver of Urban Micro-Segregation? An In-Depth Analysis of Two Viennese Districts
by Robert Musil and Jiannis Kaucic
Land 2024, 13(9), 1507; https://doi.org/10.3390/land13091507 (registering DOI) - 17 Sep 2024
Abstract
The concept of segregation analyses the unequal distribution of social groups between neighbourhoods. It rests on two assumptions: that of homogeneous neighbourhoods and of a market liberal housing system. Both assumptions are applicable the context of American cities, but they display severe limitations [...] Read more.
The concept of segregation analyses the unequal distribution of social groups between neighbourhoods. It rests on two assumptions: that of homogeneous neighbourhoods and of a market liberal housing system. Both assumptions are applicable the context of American cities, but they display severe limitations when applied to the European context. Vienna’s housing market is particularly highly segmented, not only throughout the city as a whole but also within neighbourhoods. In the densely built-up area, residential buildings of different segments with different underlying rent regulations and entry barriers can be found side by side. Therefore, buildings are expected to show varying tenant and owner structures, which undermines the idea of a homogeneous neighbourhood. Against this background, we analyse at the micro scale small neighbourhoods defined by 100 m grid cells in a case study of two inner-city Viennese districts (districts 6 and 7) characterised by a particularly vivid housing-transformation and commodification dynamic. Using a novel and fine-grained dataset combining building information with the socio-economic data of households, we investigate the patterns and dynamics of income inequality and income segregation, as well as the relationship between housing market segments and socio-economic patterns. As data comprise two cross-sections for the years 2011 and 2020/21, changes in the neighbourhoods during the house-price boom period are also considered. This leads us to ask the question: How do housing market segmentation and its related changes affect income inequality and segregation at the micro scale? Our analysis delivers two main results: Firstly, we show the existence of marked social variation and related dynamics at the micro scale, even within a small urban area. Secondly, we show that the spatial distribution of housing market segments has a strong impact on income inequality in the neighbourhood. Full article
(This article belongs to the Special Issue Urban Micro-Segregation)
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Figure 1

Figure 1
<p>The location of the study area within the city of Vienna. Note: BR = Belt Road; MH = Mariahilfer Straße; RR = Ring Road; WZ = Linke Wienzeile. Numbers denote the 23 Viennese districts.</p>
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<p>Household income segregation for 2011 and 2020 across 100 × 100 m grid cells by income percentile, as measured by the information theory index H.</p>
Full article ">Figure 3
<p>Spatial distribution of indices for 2011 (<b>left</b>) and 2020 (<b>right</b>) in 100 × 100 m grid cells. Panels (<b>a</b>,<b>b</b>) contain the median equivalised household income, panels (<b>c</b>,<b>d</b>) show the Gini coefficient of average equivalised household income, and panels (<b>e</b>,<b>f</b>) present the local segregation scores of the multi-group Mutual Information segregation index M of the equivalised household income quintiles.</p>
Full article ">Figure 4
<p>Main housing market segments in 100 × 100 m grid cells for 2011 (panel <b>a</b>) and 2020/21 (panel <b>b</b>).</p>
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<p>Distribution of equivalised household income by housing market segment, distance to the city centre, and educational attainment for the years 2011 (<b>top</b> panel) and 2020/21 (<b>bottom</b> panel). Note: For the calculation of household income, personal incomes were bottom-coded at 1000 EUR and top-coded at 100,000 EUR to safeguard data protection and improve data structure. The axis was capped at 125,000 EUR.</p>
Full article ">
15 pages, 3030 KiB  
Article
Agroecological Assessment of Arable Lands in the Leningrad Region of Russia under the Influence of Climate Change
by Ekaterina Yu. Chebykina and Evgeny V. Abakumov
Agronomy 2024, 14(9), 2113; https://doi.org/10.3390/agronomy14092113 (registering DOI) - 17 Sep 2024
Abstract
The paper presents an analysis of the influence of climatic characteristics on the rating of land suitability for agricultural use. Soil fertility is one of the most important factors in land productivity and crop capacity; it is a complex value that depends not [...] Read more.
The paper presents an analysis of the influence of climatic characteristics on the rating of land suitability for agricultural use. Soil fertility is one of the most important factors in land productivity and crop capacity; it is a complex value that depends not only on agrophysical and agrochemical soil properties but also on other natural factors, such as climate. There are different methodical approaches for a quantitative assessment of fertility level. The objectives of the research were to understand whether the distributions of active temperature sums and annual precipitation sums have a significant effect on the spatial and temporal heterogeneity of the rating assessment of land suitability for agricultural use in the example of the Leningrad region. The estimation and comparison between Semenov–Blagovidov’s method of quality land estimation and Karmanov’s method of appraisal of soils are given in this article. Karmanov’s method is highlighted in this paper for its ability to assess soil’s ecological indices more effectively than traditional methods. The research suggested that climate change may lead to increased variability in soil quality, with potential benefits for agriculture under certain climate scenarios, but at the same time, excessive temperatures in summer and precipitations might become a limiting factor, pushing down yields. The results of such assessment show that the performed calculation models can be used to forecast crop yields for future periods. Full article
(This article belongs to the Special Issue Crop Models for Agricultural Yield Prediction under Climate Change)
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Figure 1

Figure 1
<p>Locations of the studied farms in the Leningrad region. Numbers at the right figure are numbers of farms according to table in <a href="#sec3dot1-agronomy-14-02113" class="html-sec">Section 3.1</a>.</p>
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<p>Soil bonitet quality for agricultural crops of the Leningrad region according to Semenov–Blagovidov’s formula.</p>
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<p>SEI and soil bonitet quality (B) for cereal crops of the Leningrad region according to Karmanov’s formula.</p>
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<p>The relative increase in soil bonitet quality for cereal crops according to two scenarios (the ratio of soil bonitet quality under predicted conditions to that calculated for the present): (<b>a</b>)—according to the arid (A1F1) scenario; (<b>b</b>)—according to the humid (B2) scenario; ♦—data for 2030; ■—data for 2050.</p>
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<p>The yield of cereal crops according to the formula of Semenov–Blagovidov/Karmanov.</p>
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16 pages, 10090 KiB  
Article
Gestational Interrelationships among Gut–Metabolism–Transcriptome in Regulating Early Embryo Implantation and Placental Development in Mice
by Shuai Lin, Yuqi Liang, Jingqi Geng, Yunfei Yan, Ruipei Ding and Maozhang He
Microorganisms 2024, 12(9), 1902; https://doi.org/10.3390/microorganisms12091902 (registering DOI) - 17 Sep 2024
Abstract
Decidualization of the uterine endometrium is a critical process for embryo implantation in mammals, primarily occurring on gestational day 8 in pregnant mice. However, the interplay between the maternal gut microbiome, metabolism, and the uterus at this specific time point remains poorly understood. [...] Read more.
Decidualization of the uterine endometrium is a critical process for embryo implantation in mammals, primarily occurring on gestational day 8 in pregnant mice. However, the interplay between the maternal gut microbiome, metabolism, and the uterus at this specific time point remains poorly understood. This study employed a multi-omics approach to investigate the metabolic, gut microbiome, and transcriptomic changes associated with early pregnancy (gestational day 8 (E8)) in mice. Serum metabolomics revealed a distinct metabolic profile at E8 compared to controls, with the differential metabolites primarily enriched in amino acid metabolism pathways. The gut microbial composition showed that E8 mice exhibited higher alpha-diversity and a significant shift in beta-diversity. Specifically, the E8 group displayed a decrease in pathogenic Proteobacteria and an increase in beneficial Bacteroidetes and S24-7 taxa. Transcriptomics identified myriads of distinct genes between the E8 and control mice. The differentially expressed genes were enriched in pathways involved in alanine, aspartate, and glutamate metabolism, PI3K-Akt signaling, and the PPAR signaling pathway. Integrative analysis of the multi-omics data uncovered potential mechanistic relationships among the differential metabolites, gut microbiota, and uterine gene expression changes. Notably, the gene Asns showed strong correlations with specific gut S24-7 and metabolite L-Aspartatic acid, suggesting its potential role in mediating the crosstalk between the maternal environment and embryo development during early pregnancy. These findings provide valuable insights into the complex interplay between the maternal metabolome, the gut microbiome, and the uterine transcriptome in the context of early pregnancy, which may contribute to our understanding of the underlying mechanisms of embryo implantation and development. Full article
(This article belongs to the Special Issue Advances in Host-Gut Microbiota)
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Figure 1

Figure 1
<p>Serum metabolites were significantly changed in E8 group as compared to sham group. (<b>A</b>,<b>B</b>) Principal coordinate analysis (PCoA) based on Bray–Curtis dissimilarity calculated by metabolite features in ESI<sup>+</sup> and ESI<sup>−</sup> mode indicating an obvious shift in mice of E8 group from that in sham group. (<b>C</b>) Heatmap clustering of distinct serum metabolites from the comparison between E8 and sham groups. (<b>D</b>) KEGG pathway analysis was performed based on differentially expressed metabolites between E8 and sham groups. The color of bubbles represents the value of adjusted <span class="html-italic">p</span> value, and the size of bubbles represents the number of counts (sorted by enrichment ratio). (<b>E</b>) Schematic diagram of 3 E8-depleted metabolites participating in the alanine, aspartate, and glutamate metabolism KEGG pathways. (Asterisk indicates statistical significance, ‘**’ represents <span class="html-italic">p</span> &lt; 0.01).</p>
Full article ">Figure 2
<p>Compositional analysis of gut microbiota in mice between sham and E8 groups. (<b>A</b>) Faecal alpha diversity analysis estimated by Chao1 and Shannon indexes between mice in sham and E8 groups. (<b>B</b>) Principal coordination analysis (PCoA) and analysis of similarities (anosim) were calculated based on Bray–Curtis matrix. (<b>C</b>,<b>D</b>) The taxonomic composition distribution between two groups on the phylum and genus levels of gut microbiota. (<b>E</b>) Log10-transformed relative abundance of significantly different ASVs between sham and E8. (<b>F</b>) The ratio of Firmicutes compared to Bacteroidota in E8 mice compared with sham mice.</p>
Full article ">Figure 3
<p>Analysis of differentially expressed genes in E8 and sham groups. (<b>A</b>) PCA score plot indicating an obvious separation of the transcriptomic profile between E8 and sham groups. (<b>B</b>) Volcano plot showing differential genes (top 20 upregulated and top 20 downregulated genes in E8 and sham mice). Criteria for significant differences (VIP &gt; 1, adjusted <span class="html-italic">p</span> &lt; 0.05 and fold change ≥ 2). (<b>C</b>) KEGG enrichment analysis of the DEGs in the E8 versus sham comparison. The red column represents the top 15 KEGG pathways in E8 and blue column represents the top 15 downregulated KEGG pathways. (<b>D</b>,<b>E</b>) The bar plot for the top 15 significant enrichment annotations for biological process (BP) of all upregulated genes (<b>D</b>) and downregulated genes (<b>E</b>).</p>
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<p>Associations between differentially expressed metabolites and gut microbiota. (<b>A</b>) Chord diagram displaying the significant associations between differentially expressed metabolites and ASVs. The associated metabolites are colored gray, and the associated ASVs are colored successively. Each line indicates a significant correlation between a bacterium and a metabolite, with the red color corresponding to a positive association (<span class="html-italic">p</span> value &lt; 0.05) and the blue color representing a negative association (<span class="html-italic">p</span> value &lt; 0.05). (<b>B</b>) Correlations between metabolite modules and ASVs. The absolute correlation coefficient (|r|) corresponds to the size of the circle, and the <span class="html-italic">p</span> value is indicated by asterisk (“*”, <span class="html-italic">p</span> &lt; 0.05; “**”, <span class="html-italic">p</span> &lt; 0.01).</p>
Full article ">Figure 5
<p>Variations in serum metabolites and gut microbiota have extensive relationship with pregnancy-related KEGG pathways. (<b>A</b>) Heatmap shows differentially expressed genes in the alanine, aspartate, and glutamate metabolism pathways. (<b>B</b>) 16S rRNA gene sequencing based on ASVs composition and metabolites composition was related to each of 16 significantly differential genes in the alanine, aspartate, and glutamate metabolism pathways using Mantel-test analysis. Edge width corresponds to the Mantel’s r statistic for the corresponding distance correlations, and edge color denotes the statistical significance. Pairwise comparisons of genes are shown, with a color gradient denoting Spearman’s correlation coefficient (Asterisks in the cells indicate statistical significance of the pairwise correlation, ‘*’ represents <span class="html-italic">p</span> &lt; 0.05, ‘**’ represents <span class="html-italic">p</span> &lt; 0.01, ‘***’ represents <span class="html-italic">p</span> &lt; 0.001). (<b>C</b>) Chord diagram displays the significant associations between each ASV and gene in the alanine, aspartate, and glutamate metabolism pathway. The associated genes are colored gray, and the associated ASVs are colored successively. Each line indicates a significant correlation between a bacterium and a metabolite, with the red color corresponding to a positive association (<span class="html-italic">p</span> value &lt; 0.05) and the blue color representing a negative association (<span class="html-italic">p</span> value &lt; 0.05). (<b>D</b>) Chord diagram displays the significant associations between each metabolite and gene in the alanine, aspartate and glutamate metabolism pathway. The associated genes are colored gray, and the associated metabolites are colored successive. Each line indicates a significant correlation between a bacterium and a metabolite, with the red color corresponding to a positive association (<span class="html-italic">p</span> value &lt; 0.05) and the blue color representing a negative association (<span class="html-italic">p</span> value &lt; 0.05).</p>
Full article ">
13 pages, 278 KiB  
Article
A Study of Factors Contributing to the Nutritional Status of Elderly People Receiving Home Care
by Eirini Stratidaki, Enkeleint A. Mechili, Christina Ouzouni, Athina E. Patelarou, Konstantinos Giakoumidakis, Aggelos Laliotis and Evridiki Patelarou
Nutrients 2024, 16(18), 3135; https://doi.org/10.3390/nu16183135 (registering DOI) - 17 Sep 2024
Abstract
(1) Background: Nutrition is a critical aspect of health and well-being in the elderly population, as physiological changes associated with aging can impact nutrient utilization and dietary needs. The aim of this study was the assessment of nutritional screening and associated factors among [...] Read more.
(1) Background: Nutrition is a critical aspect of health and well-being in the elderly population, as physiological changes associated with aging can impact nutrient utilization and dietary needs. The aim of this study was the assessment of nutritional screening and associated factors among community-dwelling elderly people. (2) Methods: This study is the first phase of an intervention trial of people aged 65 years and over who received primary health services and resided in the municipality of Archanes Asterousia in Crete, Greece. Nutritional risk was assessed using the Mini Nutritional Assessment. Diet-related factors were analyzed, including health status (oral hygiene, depression, cognitive decline, impaired functioning, quality of life), social factors (educational attainment, marital status, type of work before 60 years), and lifestyle factors (smoking, drinking, diet). (3) Results: A total of 730 elderly people were evaluated (males, 31.5%), with an average age (±SD) of 76.83 (±6.68) years. MNA was found to have a statistically significant connection with assessment of oral hygiene, mental state, Charlson comorbidity, functional independence (assessed with the Barthel scale), and quality of life. The exception was geriatric depression (GDS), with which no statistically significant association was found (p > 0.05). Nutritional risk analysis revealed 379 participants (51.9%) to be adequately nourished, 205 (28.1%) to be at risk of malnutrition, and 146 (20.0%) to be malnourished. (4) Conclusions: These results clearly demonstrated the key factors that contribute to the nutritional screening of elderly people and need to be addressed by health authorities and social services. Full article
31 pages, 3833 KiB  
Article
Transition Metal-Promoted LDH-Derived CoCeMgAlO Mixed Oxides as Active Catalysts for Methane Total Oxidation
by Marius C. Stoian, Cosmin Romanitan, Katja Neubauer, Hanan Atia, Constantin Cătălin Negrilă, Ionel Popescu and Ioan-Cezar Marcu
Catalysts 2024, 14(9), 625; https://doi.org/10.3390/catal14090625 (registering DOI) - 17 Sep 2024
Abstract
A series of M(x)CoCeMgAlO mixed oxides with different transition metals (M = Cu, Fe, Mn, and Ni) with an M content x = 3 at. %, and another series of Fe(x)CoCeMgAlO mixed oxides with Fe contents x ranging from 1 to 9 at. [...] Read more.
A series of M(x)CoCeMgAlO mixed oxides with different transition metals (M = Cu, Fe, Mn, and Ni) with an M content x = 3 at. %, and another series of Fe(x)CoCeMgAlO mixed oxides with Fe contents x ranging from 1 to 9 at. % with respect to cations, while keeping constant in both cases 40 at. % Co, 10 at. % Ce and Mg/Al atomic ratio of 3 were prepared via thermal decomposition at 750 °C in air of their corresponding layered double hydroxide (LDH) precursors obtained by coprecipitation. They were tested in a fixed bed reactor for complete methane oxidation with a gas feed of 1 vol.% methane in air to evaluate their catalytic performance. The physico-structural properties of the mixed oxide samples were investigated with several techniques, such as powder X-ray diffraction (XRD), scanning electron microscopy (SEM) coupled with energy dispersive X-ray spectroscopy (EDX), elemental mappings, inductively coupled plasma optical emission spectroscopy (ICP-OES), X-ray photoelectron spectroscopy (XPS), temperature-programmed reduction under hydrogen (H2-TPR) and nitrogen adsorption–desorption at −196 °C. XRD analysis revealed in all the samples the presence of Co3O4 crystallites together with periclase-like and CeO2 phases, with no separate M-based oxide phase. All the cations were distributed homogeneously, as suggested by EDX measurements and elemental mappings of the samples. The metal contents, determined by EDX and ICP-OES, were in accordance with the theoretical values set for the catalysts’ preparation. The redox properties studied by H2-TPR, along with the surface composition determined by XPS, provided information to elucidate the catalytic combustion properties of the studied mixed oxide materials. The methane combustion tests showed that all the M-promoted CoCeMgAlO mixed oxides were more active than the M-free counterpart, the highest promoting effect being observed for Fe as the doping transition metal. The Fe(x)CoCeMgAlO mixed oxide sample, with x = 3 at. % Fe displayed the highest catalytic activity for methane combustion with a temperature corresponding to 50% methane conversion, T50, of 489 °C, which is ca. 40 °C lower than that of the unpromoted catalyst. This was attributed to its superior redox properties and lowest activation energy among the studied catalysts, likely due to a Fe–Co–Ce synergistic interaction. In addition, long-term tests of Fe(3)CoCeMgAlO mixed oxide were performed, showing good stability over 60 h on-stream. On the other hand, the addition of water vapors in the feed led to textural and structural changes in the Fe(3)CoCeMgAlO system, affecting its catalytic performance in methane complete oxidation. At the same time, the catalyst showed relatively good recovery of its catalytic activity as soon as the water vapors were removed from the feed. Full article
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<p>Diffractograms of (<b>a</b>) M(3)CoCeMgAl, and (<b>b</b>) Fe(x)CoCeMgAl LDH-based precursors compared to that of undoped CoCeMgAl LDH. Symbols: #—LDH phase; ∗—boehmite (AlOOH) phase.</p>
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<p>Diffractograms of (<b>a</b>) M(3)CoCeMgAlO and (<b>b</b>) Fe(x)CoCeMgAlO mixed oxides calcined at 750 °C compared to their unpromoted CoCeMgAlO counterpart. Symbols: Δ—Co<sub>3</sub>O<sub>4</sub> phase; ∗—CeO<sub>2</sub> phase; #—Mg(Al)O phase.</p>
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<p>(<b>a</b>) High-resolution O 1s core level and (<b>b</b>) C 1s core level X-ray photoelectron profiles of the Fe(x)CoCeMgAlO mixed oxide samples: CoCeMgAlO (A); Fe(1)CoCeMgAlO (B); Fe(3)CoCeMgAlO (C); Fe(6)CoCeMgAlO (D); Fe(9)CoCeMgAlO (E).</p>
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<p>(<b>a</b>) High-resolution Co 2p core level and (<b>b</b>) Ce 3d core level X-ray photoelectron profiles of the Fe(x)CoCeMgAlO mixed oxide samples: CoCeMgAlO (A); Fe(1)CoCeMgAlO (B); Fe(3)CoCeMgAlO (C); Fe(6)CoCeMgAlO (D); Fe(9)CoCeMgAlO (E).</p>
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<p>High-resolution Fe 2p core level X-ray photoelectron profiles of the Fe(x)CoCeMgAlO mixed oxide catalysts: Fe(1)CoCeMgAlO (A); Fe(3)CoCeMgAlO (B); Fe(6)CoCeMgAlO (C); Fe(9)CoCeMgAlO (D).</p>
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<p>H<sub>2</sub>-TPR profiles of CoCeMgAlO and promoted M(3)CoCeMgAlO mixed oxides.</p>
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<p>H<sub>2</sub>-TPR profiles of the promoted Fe(x)CoCeMgAlO catalysts.</p>
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<p>The light-off curves for the methane combustion reaction over (<b>a</b>) CoCeMgAlO and M(3)CoCeMgAlO and (<b>b</b>) Fe(x)CoCeMgAlO catalysts. Reaction conditions: 1 vol.% methane in air, GHSV of 16,000 h<sup>−1</sup>, 1 cm<sup>3</sup> of catalyst.</p>
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<p>Variation of the total hydrogen consumption below 750 °C in the H<sub>2</sub>-TPR measurements and of the intrinsic reaction rates at 400 and 450 °C versus Fe content in the Fe(x)CoCeMgAlO series.</p>
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<p>(<b>a</b>) Dependence of the Ce/Co surface atomic ratio and of the intrinsic reaction rates at 400 and 450 °C on the Fe content in the Fe(x)CoCeMgAlO series. (<b>b</b>) Dependence between the intrinsic reaction rate at 400 °C and the Ce<sup>4+</sup>/Ce surface atomic ratio in the Fe(x)CoCeMgAlO series.</p>
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<p>The dependence of the methane total oxidation on the gas hourly space velocity (GHSV) at constant 1 vol. % methane concentration in the feed gas for the Fe(3)CoCeMgAlO catalyst.</p>
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<p>Evolution of methane conversion at 600 °C with time over Fe(3)CoCeMgAlO catalyst. Reaction conditions: 1 vol.% CH<sub>4</sub> in air and GHSV of 16,000 h<sup>−1</sup> with 1 cm<sup>3</sup> of catalyst.</p>
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<p>Evolution of methane conversion with time on stream during combustion tests at 600 °C for the Fe(3)CoCeMgAlO catalyst in dry/humid conditions runs. Dry reaction conditions: 1 vol.% CH<sub>4</sub> in air and GHSV of 16,000 h<sup>−1</sup>, 1 cm<sup>3</sup> of catalyst. Humid reaction conditions were obtained by adding, with a peristaltic pump, a flow of 0.14 mL min<sup>−1</sup> of deionized liquid water to the dry mixture, corresponding to a water vapor content of around 40 vol. %.</p>
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<p>The scheme for methane catalytic oxidation reaction on the active phase of Co<sub>3</sub>O<sub>4</sub> spinel oxide.</p>
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14 pages, 7608 KiB  
Case Report
Peri-Implant Tissue Stability: A Series of Five Case Reports on an Innovative Implant Design
by Marco Aurélio Bianchini, Mario Escobar, Maria Elisa Galarraga-Vinueza, Thalles Yurgen Balduino and Sergio Alexandre Gehrke
Appl. Sci. 2024, 14(18), 8354; https://doi.org/10.3390/app14188354 (registering DOI) - 17 Sep 2024
Abstract
Background/Aim: The stability of peri-implant tissues is crucial for the long-term success of dental implant treatments. A new cervical implant design has been developed to address the challenges associated with peri-implant tissue stability, featuring a concave cervical portion to increase tissue volume in [...] Read more.
Background/Aim: The stability of peri-implant tissues is crucial for the long-term success of dental implant treatments. A new cervical implant design has been developed to address the challenges associated with peri-implant tissue stability, featuring a concave cervical portion to increase tissue volume in this area. The present study aimed to clinically evaluate the effectiveness of the new cervical implant design in maintaining peri-implant tissue stability. Materials and Methods: Five clinical cases involving completely edentulous patients were selected, in which 25 implants were installed. The marginal bone level around each implant was assessed at three different time points—T0: immediately after the prosthesis installation, T1: 6 months post installation, and T2: at the last control visit, up to 38 months later. Measurements were taken to analyze changes in marginal bone levels (MBLs) and the keratinized mucosa (KM) over time. Furthermore, the keratinized mucosa (KM) around the implants was evaluated. Results: The mean and standard deviation values of the marginal bone levels at each time point were as follows—T0: 0.59 ± 0.55 mm; T1: 1.41 ± 0.59 mm; T2: 1.76 ± 0.69 mm. Statistical analysis showed significant differences across the time points (ANOVA p < 0.0001). The overall mean KM values were 3.85 mm for T1 and T2, showing the stability of the peri-implant soft tissues at ≥1-year controls. Conclusion: Within the limitations of the present study, the results showed that the Collo implants presented measured MBL values increasing within the time range analyzed in each case but within the normal values cited in the literature for these types of rehabilitation treatments. However, the measured KM values presented, in all cases, an average above the values referenced in the literature as a minimum for maintaining the health of the peri-implant tissues. Full article
(This article belongs to the Special Issue Implant Dentistry: Advanced Materials, Methods and Technologies)
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<p>Schematic image of the innovative new design of the Collo implant inserted into the bone tissue. The figure provides a visual representation of how this novel implant design may contribute to the stability and sealing of peri-implant tissues, particularly highlighting the intricate details of the cervical portion of the implant.</p>
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<p>Image of implant placement positioned at bone level.</p>
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<p>Polymeric acrylic resin implant-supported fixed prostheses with cobalt–chrome sub-structure, acrylic resin prosthetic teeth, and pink acrylic resin gingiva.</p>
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<p>Mesial MBL measurement with periapical radiography using Image J software 2.1.4.7.</p>
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<p>Maxilla full-arch implant-supported rehabilitation with Collo implants. (<b>A</b>) Clinical photo showing the peri-implant tissue adapted surrounding the multiunit abutments; (<b>B</b>) radiographical assessment at the immediate loading implant placement and at (<b>C</b>) 6 months and (<b>D</b>) 12 months.</p>
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<p>Mandible full-arch implant-supported rehabilitation with Collo implants. (<b>A</b>) Clinical photo showing the peri-implant tissue adapted surrounding the multiunit abutments; (<b>B</b>) radiographical assessment at the immediate loading implant placement and at (<b>C</b>) 6 months and (<b>D</b>) 38 months.</p>
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<p>Maxilla full-arch implant-supported rehabilitation with Collo implants. (<b>A</b>) Clinical photo showing the peri-implant tissue adapted surrounding the multiunit abutments; (<b>B</b>) radiographical assessment at the immediate loading implant placement and at (<b>C</b>) 6 months and (<b>D</b>) 24 months.</p>
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<p>Mandible full-arch implant-supported rehabilitation with Collo implants. (<b>A</b>) Clinical photo showing the peri-implant tissue adapted surrounding the multiunit abutments; (<b>B</b>) radiographical assessment at the immediate loading implant placement and at (<b>C</b>) 6 months and (<b>D</b>) 36 months.</p>
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<p>Mandible full-arch implant-supported rehabilitation with Collo implants. (<b>A</b>) Clinical photo showing the peri-implant tissue adapted surrounding the multiunit abutments; (<b>B</b>) radiographical assessment at the immediate loading implant placement and at (<b>C</b>) 6 months and (<b>D</b>) 12 months.</p>
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<p>Occlusal and buccal view of the peri-implant soft tissue showing a healthy aspect surrounding the multiunit implant component.</p>
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<p>Graph distribution of the data collected at each time point: (T0) immediately after installation of the prosthesis, (T1) 6 months later, and (T2) at the time of the last control visit.</p>
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30 pages, 8586 KiB  
Review
Unraveling the Dynamic Properties of New-Age Energy Materials Chemistry Using Advanced In Situ Transmission Electron Microscopy
by Subramaniyan Ramasundaram, Sampathkumar Jeevanandham, Natarajan Vijay, Sivasubramani Divya, Peter Jerome and Tae Hwan Oh
Molecules 2024, 29(18), 4411; https://doi.org/10.3390/molecules29184411 (registering DOI) - 17 Sep 2024
Abstract
The field of energy storage and conversion materials has witnessed transformative advancements owing to the integration of advanced in situ characterization techniques. Among them, numerous real-time characterization techniques, especially in situ transmission electron microscopy (TEM)/scanning TEM (STEM) have tremendously increased the atomic-level understanding [...] Read more.
The field of energy storage and conversion materials has witnessed transformative advancements owing to the integration of advanced in situ characterization techniques. Among them, numerous real-time characterization techniques, especially in situ transmission electron microscopy (TEM)/scanning TEM (STEM) have tremendously increased the atomic-level understanding of the minute transition states in energy materials during electrochemical processes. Advanced forms of in situ/operando TEM and STEM microscopic techniques also provide incredible insights into material phenomena at the finest scale and aid to monitor phase transformations and degradation mechanisms in lithium-ion batteries. Notably, the solid–electrolyte interface (SEI) is one the most significant factors that associated with the performance of rechargeable batteries. The SEI critically controls the electrochemical reactions occur at the electrode–electrolyte interface. Intricate chemical reactions in energy materials interfaces can be effectively monitored using temperature-sensitive in situ STEM techniques, deciphering the reaction mechanisms prevailing in the degradation pathways of energy materials with nano- to micrometer-scale spatial resolution. Further, the advent of cryogenic (Cryo)-TEM has enhanced these studies by preserving the native state of sensitive materials. Cryo-TEM also allows the observation of metastable phases and reaction intermediates that are otherwise challenging to capture. Along with these sophisticated techniques, Focused ion beam (FIB) induction has also been instrumental in preparing site-specific cross-sectional samples, facilitating the high-resolution analysis of interfaces and layers within energy devices. The holistic integration of these advanced characterization techniques provides a comprehensive understanding of the dynamic changes in energy materials. This review highlights the recent progress in employing state-of-the-art characterization techniques such as in situ TEM, STEM, Cryo-TEM, and FIB for detailed investigation into the structural and chemical dynamics of energy storage and conversion materials. Full article
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<p>In situ solid-state/electrochemical biasing TEM characterization for energy materials. (<b>A</b>) Single-particle-level characterization of (<b>a</b>) graphene cage-like layer covering connected with the electrical circuit for external load test analysis, and (<b>b</b>) current-voltage measurements of graphene-encapsulated and amorphous-carbon-coated SiMPs [<a href="#B32-molecules-29-04411" class="html-bibr">32</a>]. (<b>B</b>) Experimental set-up of (<b>a</b>) in situ bias arrangements of tungsten tip and Cu wire inside TEM, (<b>b</b>) low-magnification TEM showing the contact, (<b>c</b>) high-magnification TEM showing the contact between tip, wire, and SEI layer, and (<b>d</b>) TEM showing the surface SEI layer assembly of the integrated set-up, and (<b>e</b>) current-voltage plot indicating critical voltage [<a href="#B33-molecules-29-04411" class="html-bibr">33</a>]. (<b>C</b>) Lithiation of electrochemically biased and (<b>a</b>) arc-discharged MWCNT which is glued to an Al rod (working electrode), Li<sub>2</sub>O grown on Li surface acts as a solid electrolyte, bulk Li metal scratched from tungsten rod acts as counter electrode, (<b>b</b>) pristine MWCNT before coming in contact with Li<sub>2</sub>O/Li electrode, (<b>c</b>) lithiated MWCNT showing uniform Li<sub>2</sub>O layer formation on the surface, and (<b>d</b>–<b>f</b>) corresponding EELS mapping of C, Li, and O, respectively, indicating the nanotube lithiation [<a href="#B34-molecules-29-04411" class="html-bibr">34</a>]. (<b>D</b>) Crack formation in the lithiated Si NWs, (<b>a</b>–<b>i</b>) morphological evolution showing anisotropic elongation and crack during the lithiation of solid cells after contacting the Li<sub>2</sub>O/Li electrode. Red arrows in the panel indicate the propagation of reaction front [<a href="#B38-molecules-29-04411" class="html-bibr">38</a>]. (<b>E</b>) In situ electrochemical functional cell for operando TEM characterization of battery materials [<a href="#B41-molecules-29-04411" class="html-bibr">41</a>]. Figures reproduced with permission from [<a href="#B32-molecules-29-04411" class="html-bibr">32</a>,<a href="#B33-molecules-29-04411" class="html-bibr">33</a>,<a href="#B34-molecules-29-04411" class="html-bibr">34</a>,<a href="#B38-molecules-29-04411" class="html-bibr">38</a>,<a href="#B41-molecules-29-04411" class="html-bibr">41</a>].</p>
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<p>In situ thermal-induced TEM characterization of energy materials. (<b>A</b>) Thermal welding type experiment of nano solder Sn sheet and Cu structure, showing (<b>a</b>) TEM images of their interface at room temperature (Red, and green parts represent Sn, and Cu, respectively) and (<b>d</b>) after heating (enlarged version (<b>b</b>,<b>e</b>) and HRTEM images (<b>c</b>,<b>f</b>) before and after heating, respectively) [<a href="#B50-molecules-29-04411" class="html-bibr">50</a>]. (<b>B</b>) STEM-HAADF images of samples at all four conditions of the perovskite layer (varying the temperature from 50 to 250 °C) showed no visible changes until 150 °C [<a href="#B1-molecules-29-04411" class="html-bibr">1</a>]. (<b>C</b>) Direct transitions of perovskite structures from tetragonal to trigonal crystalline structure, (<b>a</b>–<b>c</b>) degradation process focusing on single MAPbI<sub>3</sub> grains (scale bar = 2 nm), and (<b>d</b>) MAPbI<sub>3</sub> transition from tetragonal phase to PbI<sub>2</sub> with a trigonal configuration [<a href="#B51-molecules-29-04411" class="html-bibr">51</a>]. (<b>D</b>) Cross-sectional view of in situ analysis showing HAADF images of a perovskite solar cell with a device structure of glass/ITO/TiO<sub>2</sub>/CH<sub>3</sub>NH<sub>3</sub>PbI<sub>3</sub>/spiro-OMeTAD/Ag, and stability check: day 1 shows bright images due to FIB beam focus damage, day 2 shows beam-sensitiveness slowly disappeared, days 7–15 show growth of electron-beam damaged area, and days 20–30 show no further changes (later day-30 samples underwent heating-induced degradation at different time intervals as shown by arrows) [<a href="#B52-molecules-29-04411" class="html-bibr">52</a>]. Figures reproduced with permission from [<a href="#B1-molecules-29-04411" class="html-bibr">1</a>,<a href="#B50-molecules-29-04411" class="html-bibr">50</a>,<a href="#B51-molecules-29-04411" class="html-bibr">51</a>,<a href="#B52-molecules-29-04411" class="html-bibr">52</a>].</p>
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<p>In situ gas-cell type TEM characterization for energy materials. (<b>A</b>) Schematic demonstration of operando ETEM equipped with windowed gas cell. (<b>B</b>) HAADF-STEM characterization depicting the atomic orientation of Ni/TiO<sub>2</sub> (<b>a</b>) catalyst (exposed to H<sub>2</sub>) prepared under in situ conditions at 400 °C (white arrow: Ni NPs of TiO<sub>2</sub> support, solid lines: TiO<sub>x</sub>-covered Ni atomic planes, and dashed lines: unoccupied facets), (<b>b</b>) strain maps showing atomic displacements, (<b>c</b>) catalyst (exposed to CO<sub>2</sub>:H<sub>2</sub> (0.25 bar:0.75 bar) mixture) at 400 °C showing complete re-exposure of Ni and NPs restructuring, and (<b>d</b>) estimated atomic displacements/reorientations [<a href="#B59-molecules-29-04411" class="html-bibr">59</a>]. (<b>C</b>) Concept of loading ZnO nanowires onto SiN<sub>x</sub> observing windows in a gas-cell setup with built-in MEMS chip (SO<sub>2</sub> atm conditions). (<b>D</b>) In situ TEM imaging taken after exposure to SO<sub>2</sub> gaseous conditions shows (<b>a</b>–<b>h</b>) the nanostructure’s morphological evolution, and (<b>i</b>) its corresponding EDS mapping [<a href="#B61-molecules-29-04411" class="html-bibr">61</a>]. (<b>E</b>) The concept of particle formation and growth observed during the reduction of nickel-phyllosilicate-based catalyst precursor was investigated in an in situ gaseous state. (<b>F</b>) In situ TEM images were observed at different time intervals during the reduction of nickel-phyllosilicates under 1 bar pressure (0.1 sccm gas flow rate at 425 °C) with an electron imaging dose of 30 e<sup>−</sup>·A<sup>−2</sup>·s<sup>−1</sup> showing the nucleation and growth of nanoparticles only in the presence of the electron beam [<a href="#B63-molecules-29-04411" class="html-bibr">63</a>]. Figures reproduced with permission from [<a href="#B59-molecules-29-04411" class="html-bibr">59</a>,<a href="#B61-molecules-29-04411" class="html-bibr">61</a>,<a href="#B63-molecules-29-04411" class="html-bibr">63</a>].</p>
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<p>In situ liquid-cell/electrochemistry integrated TEM characterization for energy materials. (<b>A</b>) Schematic diagram showing a cross-sectional view of TEM holder, (<b>a</b>) conduit-like silicon nitride membranes encapsulating fluid layer and in situ electrochemical workstation, (<b>b</b>) system of three patterned electrodes with top chip, (<b>c</b>,<b>d</b>) electrochemical activity of Pt cyclic voltammetry (CV) with thick and thin liquid (~150 nm) layers, and (<b>e</b>) Temporal evolution (<b>a</b>–<b>h</b>) occurring in LiFePO<sub>4</sub>/FePO<sub>4</sub> cluster during cycling (charge/discharge). Red, and yellow arrows indicate the propagation of delithiation in core–shell, and left to right pathways [<a href="#B75-molecules-29-04411" class="html-bibr">75</a>]. (<b>B</b>) Schematic representation of (<b>a</b>) in situ liquid-cell nanobattery setup analyzing the lithiation process, (<b>b</b>) SEM images of the electrochemically biased chip with (<b>b</b>) inner side, (<b>c</b>) its magnified view, and (<b>d</b>) Si NW electrode welded onto the Pt contact [<a href="#B76-molecules-29-04411" class="html-bibr">76</a>]. (<b>C</b>) Graphene liquid-cell (GLC) TEM illustration: (<b>a</b>) Si NPs were immersed in liquid electrolyte and placed between graphene layers in a sandwich structure, (<b>b</b>) the whole assembly was mounted on a holey amorphous carbon TEM grid (SEM image, scale bar: 1 μm), and (<b>c</b>) STEM mapping images of O, C, Si, P, and F in the GLC (scale bar: 100 nm) [<a href="#B77-molecules-29-04411" class="html-bibr">77</a>]. (<b>D</b>) Schematic diagram of in situ liquid-cell visualization of (<b>a</b>) MOS<sub>2</sub> reaction on Ti electrodes, (<b>b</b>) assembled cell window area for capturing the dynamic lithiation/de-lithiation process, (<b>c</b>) schematic diagram for nanobeam diffraction characterization on the SEI layer or residual MoS<sub>2</sub> reaction after the process, and (<b>d</b>) typical example showing bright-field or dark-field image reconstruction of the diffraction pattern [<a href="#B78-molecules-29-04411" class="html-bibr">78</a>]. Figures reproduced with permission from [<a href="#B75-molecules-29-04411" class="html-bibr">75</a>,<a href="#B76-molecules-29-04411" class="html-bibr">76</a>,<a href="#B77-molecules-29-04411" class="html-bibr">77</a>,<a href="#B78-molecules-29-04411" class="html-bibr">78</a>].</p>
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<p>In situ light-induced TEM characterization of energy materials. (<b>A</b>) Schematic representation of integrated optical fiber setup with TEM holder [<a href="#B91-molecules-29-04411" class="html-bibr">91</a>]. (<b>B</b>) Customized fiber connection with cut fiber end projecting inside the microscope vacuum with a 15° angle to avoid optical loss, and the opposite angle cut by 30° to produce a beam that can illuminate the TEM sample [<a href="#B92-molecules-29-04411" class="html-bibr">92</a>]. (<b>C</b>) Schematic representation of in situ light-induced TEM with an integrated gas flow and heating controller inside the compact sample chamber. (<b>D</b>) In situ HRTEM imaging of anatase nanocrystals at 150 °C with/without 1 Torr water pressure: (<b>a</b>–<b>f</b>) diverse experimental conditions starting from no water to fresh water presence even after 40 h in a water/gas environment before exposure to the electron beam [<a href="#B93-molecules-29-04411" class="html-bibr">93</a>]. (<b>E</b>) TEM holder modification with liquid-cell chip arrangement. (<b>a</b>,<b>c</b>,<b>d</b>) schematic representations, (<b>b</b>) liquid cell, and (<b>e</b>) real photograph. (<b>F</b>) HRTEM analysis depicting transition in the morphology of Cu<sub>2</sub>O samples observed at different (<b>a</b>–<b>c</b>) irradiation time intervals such as 1 h, 2 h, 3 h, and (<b>d</b>) schematic showing its evolution over time [<a href="#B95-molecules-29-04411" class="html-bibr">95</a>]. (<b>G</b>) Schematic diagram displaying in situ fabrication of TiO<sub>2</sub>/CdSe nanowire QD solar cell integrated with LED and electrical measurement system in the STM-TEM [<a href="#B8-molecules-29-04411" class="html-bibr">8</a>]. (<b>H</b>) Light-induced rapid phase transformation (through <span class="html-italic">α</span> phase and hydrogen-rich <span class="html-italic">β</span> phase) reaction in the antenna–reactor configuration with illumination at 690 nm (scale bars: 50 nm) visualized over different short time intervals: (<b>a</b>,<b>b</b>) phase transformation at difffernt locations., in both cases (I–V) represents snapshots taken at different time (s) interval. Figures reproduced with permission from [<a href="#B8-molecules-29-04411" class="html-bibr">8</a>,<a href="#B91-molecules-29-04411" class="html-bibr">91</a>,<a href="#B92-molecules-29-04411" class="html-bibr">92</a>,<a href="#B93-molecules-29-04411" class="html-bibr">93</a>,<a href="#B95-molecules-29-04411" class="html-bibr">95</a>,<a href="#B97-molecules-29-04411" class="html-bibr">97</a>].</p>
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<p>In situ Cryo-TEM characterization of MOF nanostructures. (<b>A</b>) Schematic representation of Cryo-TEM technique for MOF nanostructures for monitoring its dynamics under cryogenic conditions [<a href="#B100-molecules-29-04411" class="html-bibr">100</a>]. (<b>B</b>) HRTEM images of (<b>a</b>) MOF-525(Pt) and (<b>b</b>) PCN-224(Pt) (insets: FFT depicting the predominant lattice fringes) [<a href="#B102-molecules-29-04411" class="html-bibr">102</a>]. (<b>C</b>) HRTEM images of (<b>a</b>) intact MOF-5 crystals with inset FFT corresponding to [<a href="#B100-molecules-29-04411" class="html-bibr">100</a>] zone axis orientation as illustrated in (<b>b</b>); the selected inset from the filtered version (<b>c</b>) was simulated noise-free with (<b>d</b>) HRTEM image (thickness 15.5 nm, Δf = +12 nm, Cs +20 μm), and (<b>e</b>) illustrated structure of MOF-5 crystals (white stripes: terephthalate linker, grey color: pores) [<a href="#B103-molecules-29-04411" class="html-bibr">103</a>]. Figures reproduced with permission from [<a href="#B100-molecules-29-04411" class="html-bibr">100</a>,<a href="#B102-molecules-29-04411" class="html-bibr">102</a>,<a href="#B103-molecules-29-04411" class="html-bibr">103</a>].</p>
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<p>In situ Cryo-TEM characterization for SEI layer and Li metal interfaces in rechargeable batteries. (<b>A</b>) The method for preserving and stabilizing Li metal by Cryo-TEM whereby the specimen was placed onto the Cryo-TEM holder while maintaining cryogenic conditions, and during insertion of TEM column the temperature is maintained not above −170 °C. (<b>B</b>) Cryo-TEM observations (<b>a</b>) depicting kinked Li metal dendrite and SEI that changes from &lt;211&gt; to &lt;110&gt; and finally comes back to &lt;211&gt; growth lattice projection, (<b>b</b>) Li deposition on Cu TEM grid and storage under cryogenic conditions, (<b>c</b>) atomic-resolution images showing the transition from (i) &lt;211&gt; to &lt;110&gt; and (ii) &lt;110&gt; changes back to &lt;211&gt; lattice orientation, (<b>d</b>) mosaic model, and (<b>e</b>) multi-layer model of dendritic Li deposition on SEI under different carbonate electrolyte conditions [<a href="#B101-molecules-29-04411" class="html-bibr">101</a>]. (<b>C</b>) Detailed representation of Li dissolution under (<b>a</b>,<b>c</b>,<b>e</b>) mosaic SEI, and (<b>b</b>,<b>d</b>,<b>f</b>) multi-layer SEIs [<a href="#B3-molecules-29-04411" class="html-bibr">3</a>]. (<b>D</b>) Structural composition and elemental mapping of Li dendrites formed at the interface; the morphology was differentiated and analyzed under (<b>a</b>,<b>b</b>) Cryo-FIB, (<b>c</b>,<b>d</b>) Cryo-STEM, and (<b>e</b>,<b>f</b>) Cryo-EELS for type I dendrites and type II dendrites, respectively. Scale bar in (<b>a</b>,<b>b</b>), and (<b>c</b>–<b>f</b>) are equal to 1 µM, and 300 nm, respectively [<a href="#B4-molecules-29-04411" class="html-bibr">4</a>]. Figures reproduced with permission from [<a href="#B3-molecules-29-04411" class="html-bibr">3</a>,<a href="#B4-molecules-29-04411" class="html-bibr">4</a>,<a href="#B101-molecules-29-04411" class="html-bibr">101</a>].</p>
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<p>In situ Cryo-TEM characterization of electron-beam sensitive perovskites. (<b>A</b>) Schematic representation displaying (<b>a</b>) integrated galvanostatic and current-voltage measurements under Cryo-TEM conditions, and (<b>b</b>) five galvanostatic curves between mixed and only electronic states measured at the temperature range from 100 to 295 K. (<b>B</b>) Dynamic changes in optical images of perovskite films from (<b>a</b>–<b>c</b>) dark conditions to 20 mW cm<sup>−2</sup> illumination, (<b>d</b>) schematic illustration depicting the migration of cations MA<sup>+</sup> and anions I<sup>−</sup> through the film [<a href="#B105-molecules-29-04411" class="html-bibr">105</a>]. (<b>C</b>) Drop casting of (<b>a</b>) pristine or UV/moisture-exposed perovskite nanowires onto the TEM grid in nitrogen glove box conditions, in comparison with using (<b>b</b>) Cryo-TEM showing preserved structures, (<b>c</b>) conventional TEM techniques showing electron beam-damaged structures with atomic-level resolution in lattice fringes, (<b>d</b>) TEM image of MAPI<sub>3</sub> NWs after exposing to electron beam, and (<b>e</b>) decomposition of MAPI<sub>3</sub> in to PBI<sub>2</sub> [<a href="#B106-molecules-29-04411" class="html-bibr">106</a>]. Figures reproduced with permission from [<a href="#B105-molecules-29-04411" class="html-bibr">105</a>,<a href="#B106-molecules-29-04411" class="html-bibr">106</a>].</p>
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<p>Overview of diverse methodologies adapted for in situ TEM characterization of energy materials.</p>
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14 pages, 2039 KiB  
Article
Metabolomic Effects of Liraglutide Therapy on the Plasma Metabolomic Profile of Patients with Obesity
by Assim A. Alfadda, Anas M. Abdel Rahman, Hicham Benabdelkamel, Reem AlMalki, Bashayr Alsuwayni, Abdulaziz Alhossan, Madhawi M. Aldhwayan, Ghalia N. Abdeen, Alexander Dimitri Miras and Afshan Masood
Metabolites 2024, 14(9), 500; https://doi.org/10.3390/metabo14090500 (registering DOI) - 17 Sep 2024
Abstract
Background: Liraglutide, a long-acting glucagon-like peptide-1 receptor agonist (GLP1RA), is a well-established anti-diabetic drug, has also been approved for the treatment of obesity at a dose of 3 mg. There are a limited number of studies in the literature that have looked at [...] Read more.
Background: Liraglutide, a long-acting glucagon-like peptide-1 receptor agonist (GLP1RA), is a well-established anti-diabetic drug, has also been approved for the treatment of obesity at a dose of 3 mg. There are a limited number of studies in the literature that have looked at changes in metabolite levels before and after liraglutide treatment in patients with obesity. To this end, in the present study we aimed to explore the changes in the plasma metabolomic profile, using liquid chromatography-high resolution mass spectrometry (LC-HRMS) in patients with obesity. Methods: A single-center prospective study was undertaken to evaluate the effectiveness of 3 mg liraglutide therapy in twenty-three patients (M/F: 8/15) with obesity, mean BMI 40.81 ± 5.04 kg/m2, and mean age of 36 ± 10.9 years, in two groups: at baseline (pre-treatment) and after 12 weeks of treatment (post-treatment). An untargeted metabolomic profiling was conducted in plasma from the pre-treatment and post-treatment groups using LC-HRMS, along with bioinformatics analysis using ingenuity pathway analysis (IPA). Results: The metabolomics analysis revealed a significant (FDR p-value ≤ 0.05, FC 1.5) dysregulation of 161 endogenous metabolites (97 upregulated and 64 downregulated) with distinct separation between the two groups. Among the significantly dysregulated metabolites, the majority of them were identified as belonging to the class of oxidized lipids (oxylipins) that includes arachidonic acid and its derivatives, phosphorglycerophosphates, N-acylated amino acids, steroid hormones, and bile acids. The biomarker analysis conducted using MetaboAnalyst showed PGP (a21:0/PG/F1alpha), an oxidized lipid, as the first metabolite among the list of the top 15 biomarkers, followed by cysteine and estrone. The IPA analysis showed that the dysregulated metabolites impacted the pathway related to cell signaling, free radical scavenging, and molecular transport, and were focused around the dysregulation of NF-κB, ERK, MAPK, PKc, VEGF, insulin, and pro-inflammatory cytokine signaling pathways. Conclusions: The findings suggest that liraglutide treatment reduces inflammation and modulates lipid metabolism and oxidative stress. Our study contributes to a better understanding of the drug’s multifaceted impact on overall metabolism in patients with obesity. Full article
(This article belongs to the Special Issue Metabolomics in Human Diseases and Health)
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<p>(<b>A</b>) Receiver operating characteristic (ROC) curve utilizing PLS-DA as the classification and feature ranking method. The top 15 variants had an area under the curve (AUC) of 0.852. (<b>B</b>) Frequency plot showing the top 15 significantly dysregulated metabolites in the pre- and post-liraglutide treatment groups. ROC curves are shown of individual metabolite biomarkers: (<b>C</b>) N-linoleoyl tryptophan, with an AUC of 0.881, and box plot (<span class="html-italic">p</span> ≤ 0.05 and fold change ≥ 1.5), where red represents the post-liraglutide treatment group and green represents the pre-liraglutide treatment group; and (<b>D</b>) epinephrine glucuronide, with an AUC of 0.849, and box plot (<span class="html-italic">p</span> ≤ 0.05 and fold change ≥ 1.5), where red represents the post-liraglutide treatment group and green represents the pre-liraglutide treatment group.</p>
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<p>Schematic representation of the (<b>A</b>) highest scoring network pathways depicting the involvement of the differentially regulated metabolites between the pre- and post-liraglutide treatment groups. The dotted lines indicate indirect relationships, and the straight lines indicate direct relationships. The network pathways identified between the two groups were related to cell signalling, free radical scavenging, and molecular transport, with a score of 36 and 14 focus molecules (represented in bold <a href="#app1-metabolites-14-00500" class="html-app">Supplementary Table S4</a>). The interaction networks were generated through IPA (QIAGEN, Aarhus, Denmark). (<b>B</b>) The top canonical pathways dysregulated after 12 weeks of treatment with liraglutide.</p>
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<p>Schematic representation of the (<b>A</b>) highest scoring network pathways depicting the involvement of the differentially regulated metabolites between the pre- and post-liraglutide treatment groups. The dotted lines indicate indirect relationships, and the straight lines indicate direct relationships. The network pathways identified between the two groups were related to cell signalling, free radical scavenging, and molecular transport, with a score of 36 and 14 focus molecules (represented in bold <a href="#app1-metabolites-14-00500" class="html-app">Supplementary Table S4</a>). The interaction networks were generated through IPA (QIAGEN, Aarhus, Denmark). (<b>B</b>) The top canonical pathways dysregulated after 12 weeks of treatment with liraglutide.</p>
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36 pages, 4195 KiB  
Review
Artificial Intelligence Tools in Pediatric Urology: A Comprehensive Review of Recent Advances
by Adiba Tabassum Chowdhury, Abdus Salam, Mansura Naznine, Da’ad Abdalla, Lauren Erdman, Muhammad E. H. Chowdhury and Tariq O. Abbas
Diagnostics 2024, 14(18), 2059; https://doi.org/10.3390/diagnostics14182059 (registering DOI) - 17 Sep 2024
Viewed by 97
Abstract
Artificial intelligence (AI) is providing novel answers to long-standing clinical problems, and it is quickly changing pediatric urology. This thorough analysis focuses on current developments in AI technologies that improve pediatric urology diagnosis, treatment planning, and surgery results. Deep learning algorithms help detect [...] Read more.
Artificial intelligence (AI) is providing novel answers to long-standing clinical problems, and it is quickly changing pediatric urology. This thorough analysis focuses on current developments in AI technologies that improve pediatric urology diagnosis, treatment planning, and surgery results. Deep learning algorithms help detect problems with previously unheard-of precision in disorders including hydronephrosis, pyeloplasty, and vesicoureteral reflux, where AI-powered prediction models have demonstrated promising outcomes in boosting diagnostic accuracy. AI-enhanced image processing methods have significantly improved the quality and interpretation of medical images. Examples of these methods are deep-learning-based segmentation and contrast limited adaptive histogram equalization (CLAHE). These methods guarantee higher precision in the identification and classification of pediatric urological disorders, and AI-driven ground truth construction approaches aid in the standardization of and improvement in training data, resulting in more resilient and consistent segmentation models. AI is being used for surgical support as well. AI-assisted navigation devices help with difficult operations like pyeloplasty by decreasing complications and increasing surgical accuracy. AI also helps with long-term patient monitoring, predictive analytics, and customized treatment strategies, all of which improve results for younger patients. However, there are practical, ethical, and legal issues with AI integration in pediatric urology that need to be carefully navigated. To close knowledge gaps, more investigation is required, especially in the areas of AI-driven surgical methods and standardized ground truth datasets for pediatric radiologic image segmentation. In the end, AI has the potential to completely transform pediatric urology by enhancing patient care, increasing the effectiveness of treatments, and spurring more advancements in this exciting area. Full article
(This article belongs to the Section Machine Learning and Artificial Intelligence in Diagnostics)
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<p>AI for the precise identification of pediatric urology conditions.</p>
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<p>Pediatric urological disorders discussed in this review.</p>
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<p>Anatomy and urine flow in healthy versus hydronephrosis kidneys [<a href="#B14-diagnostics-14-02059" class="html-bibr">14</a>].</p>
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<p>Kidney ultrasound scans indicating different levels of hydronephrosis: (<b>a</b>) Grade 1, (<b>b</b>) Grade 2, (<b>c</b>) Grade 3, and (<b>d</b>) Grade 4. Based on SFU grading system [<a href="#B19-diagnostics-14-02059" class="html-bibr">19</a>].</p>
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<p>Normal and obstructed ureteropelvic junction (Ariyanagam, 2024) [<a href="#B29-diagnostics-14-02059" class="html-bibr">29</a>].</p>
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<p>Unenhanced abdominal CT images (kidney: yellow; kidney stone: green) [<a href="#B42-diagnostics-14-02059" class="html-bibr">42</a>].</p>
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<p>Kidney CT image in grayscale (<b>left</b>) and with overlaid mask (<b>right</b>) to highlight suspected stones or tumors [<a href="#B46-diagnostics-14-02059" class="html-bibr">46</a>].</p>
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<p>Vesicoureteral reflux (VUR) grading.</p>
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<p>Micturating cystourethrogram revealing the presence of type 1 PUV together with corresponding alterations in the bladder (trabeculation) and upper urinary system (vesicoureteral reflux) [<a href="#B63-diagnostics-14-02059" class="html-bibr">63</a>].</p>
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<p>Anatomical characteristics used to classify urethral defects. UDR is urethral defect ratio; B-B is the imaginary line between glanular knobs (<b>A</b>) Key anatomical features of hypospadias. (<b>B</b>) Hypospadias severity grading [<a href="#B76-diagnostics-14-02059" class="html-bibr">76</a>].</p>
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<p>Virtual reality surgical procedure [<a href="#B84-diagnostics-14-02059" class="html-bibr">84</a>].</p>
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20 pages, 4459 KiB  
Article
Nonlinear Perception Characteristics Analysis of Ocean White Noise Based on Deep Learning Algorithms
by Tao Qian, Ying Li and Jun Chen
Mathematics 2024, 12(18), 2892; https://doi.org/10.3390/math12182892 (registering DOI) - 17 Sep 2024
Viewed by 96
Abstract
Caused by nonlinear vibration, ocean white noise exhibits complex dynamic characteristics and nonlinear perception characteristics. To explore the potential application of ocean white noise in engineering and health fields, novel methods based on deep learning algorithms are proposed to generate ocean white noise, [...] Read more.
Caused by nonlinear vibration, ocean white noise exhibits complex dynamic characteristics and nonlinear perception characteristics. To explore the potential application of ocean white noise in engineering and health fields, novel methods based on deep learning algorithms are proposed to generate ocean white noise, contributing to marine environment simulation in ocean engineering. A comparative study, including spectrum analysis and auditory testing, proved the superiority of the generation method using deep learning networks over general mathematical or physical methods. To further study the nonlinear perception characteristics of ocean white noise, novel experimental research based on multi-modal perception research methods was carried out within a constructed multi-modal perception system environment, including the following two experiments. The first audiovisual comparative experiment thoroughly explores the system’s user multi-modal perception experience and influence factors, explicitly focusing on the impact of ocean white noise on human perception. The second sound intensity testing experiment is conducted to further explore human multi-sensory interaction and change patterns under white noise stimulation. The experimental results indicate that user visual perception ability and state reach a relatively high level when the sound intensity is close to 50 dB. Further numerical analysis based on the experimental results reveals the internal influence relationship between user perception of multiple senses, showing a fluctuating influence law to user visual concentration and a curvilinear influence law to user visual psychology from the sound intensity of ocean white noise. This study underscores ocean white noise’s positive effect on human perception enhancement and concentration improvement, providing a research basis for multiple field applications such as spiritual healing, perceptual learning, and artistic creation for human beings. Importantly, it provides valuable references and practical insights for professionals in related fields, contributing to the development and utilization of the marine environment. Full article
(This article belongs to the Special Issue Modern Trends in Nonlinear Dynamics in Ocean Engineering)
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<p>Construction method of ocean white noise perceptual system.</p>
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<p>Generation method of ocean white noise and dynamic graphics.</p>
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<p>The DCNN network structure.</p>
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<p>Image feature processing and extraction process.</p>
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<p>The feature point sampling and optimization. (<b>a</b>) Inverse feature map of waves; (<b>b</b>) initial feature point sampling map; (<b>c</b>) optimized feature point sampling map; (<b>d</b>) the line graphic.</p>
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<p>Algorithm flow for generating dynamic graphics.</p>
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<p>Displaying background design for 8 types of white noise.</p>
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<p>Terminal display.</p>
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<p>The human–computer interaction algorithm.</p>
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<p>User viewpoint tracking map under different audiovisual environments. (<b>a</b>) Static graphic in white noise; (<b>b</b>) dynamic graphic in white noise; (<b>c</b>) dynamic graphic in silence.</p>
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<p>The hot spot map under different audiovisual environments. (<b>a</b>) Static graphic in white noise; (<b>b</b>) dynamic graphic in white noise; (<b>c</b>) dynamic graphic in silence.</p>
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<p>User viewpoint tracking map at different sound intensity levels: (<b>a</b>) at 30 dB; (<b>b</b>) at 40 dB; (<b>c</b>) at 50 dB; (<b>d</b>) at 60 dB; (<b>e</b>) at 70 dB.</p>
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<p>User hot spot map at different sound intensity levels (superposition of 10 subjects): (<b>a</b>) at 30 dB; (<b>b</b>) at 40 dB; (<b>c</b>) at 50 dB; (<b>d</b>) at 60 dB; (<b>e</b>) at 70 dB.</p>
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<p>Fixation duration influence.</p>
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<p>Saccade influence.</p>
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<p>Pupil diameter influence.</p>
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17 pages, 11750 KiB  
Article
Innovative Application of Salophen Derivatives in Organic Electronics as a Composite Film with a Poly(3,4-Ethylenedioxythiophene)-poly(styrenesulfonate) Matrix
by María Elena Sánchez Vergara, Omar Jimenez Correa, Ricardo Ballinas-Indilí, Ismael Cosme, José Ramón Álvarez Bada and Cecilio Álvarez-Toledano
Polymers 2024, 16(18), 2622; https://doi.org/10.3390/polym16182622 (registering DOI) - 17 Sep 2024
Viewed by 148
Abstract
In this work, we present the innovative synthesis of salophen (acetaminosalol) derivatives in a solvent-free environment by high-speed ball milling, using a non-conventional activation method, which allowed obtaining compounds in a shorter time and with a better yield. Furthermore, for the first time, [...] Read more.
In this work, we present the innovative synthesis of salophen (acetaminosalol) derivatives in a solvent-free environment by high-speed ball milling, using a non-conventional activation method, which allowed obtaining compounds in a shorter time and with a better yield. Furthermore, for the first time, the salophen derivatives were deposited as composite films, using a matrix of poly 3,4-ethylene dioxythiophene:polystyrene sulfonate (PEDOT:PSS) polymer. Significant findings include the transformation from the benzoid to the quinoid form of PEDOT post-IPA treatment, as evidenced by Raman spectroscopy. SEM analysis revealed the formation of homogeneous films, and AFM provided insights into the changes in surface roughness and morphology post-IPA treatment, which may be crucial for understanding potential applications in electronics. The optical bandgap ranges between 2.86 and 3.2 eV for PEDOT:PSS-salophen films, placing them as organic semiconductors. The electrical behavior of the PEDOT:PSS-salophen films undergoes a transformation with the increase in voltage, from ohmic to space charge-limited conduction, and subsequently to constant current, with a maximum of 20 mA. These results suggest the possible use of composite films in organic electronics. Full article
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<p>Chemical structure of PEDOT:PSS and the benzoid and quinoid forms of PEDOT.</p>
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<p>Molecular structure of salophen derivatives.</p>
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<p>(<b>a</b>) FT-IR spectrum of salophen compounds and (<b>b</b>) UV-Vis spectrum for SA, SB, and SC in chloroform.</p>
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<p>Raman spectroscopy of the (<b>a</b>) PEDOT:PSS-SA, (<b>b</b>) PEDOT:PSS-SB, and (<b>c</b>) PEDOT:PSS-SC composite films.</p>
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<p>Photomicrographs at 50,000× of the (<b>a</b>,<b>b</b>) PEDOT:PSS-SA, (<b>c</b>,<b>d</b>) PEDOT:PSS-SB, and (<b>e</b>,<b>f</b>) PEDOT:PSS-SC composites films before and after IPA post-treatment.</p>
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<p>EDS of the PEDOT:PSS-SC composites films (<b>a</b>) before and (<b>b</b>) after the IPA post-treatment.</p>
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<p>AFM images of the (<b>a</b>,<b>b</b>) PEDOT:PSS-SA, (<b>c</b>,<b>d</b>) PEDOT:PSS-SB, and (<b>e</b>,<b>f</b>) PEDOT:PSS-SC composites films before and after the IPA post-treatment.</p>
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<p>(<b>a</b>) Transmittance, (<b>b</b>) absorbance, (<b>c</b>) absorption coefficient, and (<b>d</b>) Tauc plot for the PEDOT:PSS-salophen films.</p>
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<p>Current–voltage curves for glass/FTO/PEDOT:PSS-salophen/Ag devices (<b>a</b>) before and (<b>b</b>) after the IPA treatment.</p>
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<p>Salophen general reaction <b>A</b>–<b>C</b>.</p>
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15 pages, 1646 KiB  
Article
Protein Microarrays for High Throughput Hydrogen/Deuterium Exchange Monitored by FTIR Imaging
by Joëlle De Meutter and Erik Goormaghtigh
Int. J. Mol. Sci. 2024, 25(18), 9989; https://doi.org/10.3390/ijms25189989 (registering DOI) - 16 Sep 2024
Viewed by 236
Abstract
Proteins form the fastest-growing therapeutic class. Due to their intrinsic instability, loss of native structure is common. Structure alteration must be carefully evaluated as structural changes may jeopardize the efficiency and safety of the protein-based drugs. Hydrogen deuterium exchange (HDX) has long been [...] Read more.
Proteins form the fastest-growing therapeutic class. Due to their intrinsic instability, loss of native structure is common. Structure alteration must be carefully evaluated as structural changes may jeopardize the efficiency and safety of the protein-based drugs. Hydrogen deuterium exchange (HDX) has long been used to evaluate protein structure and dynamics. The rate of exchange constitutes a sensitive marker of the conformational state of the protein and of its stability. It is often monitored by mass spectrometry. Fourier transform infrared (FTIR) spectroscopy is another method with very promising capabilities. Combining protein microarrays with FTIR imaging resulted in high throughput HDX FTIR measurements. BaF2 slides bearing the protein microarrays were covered by another slide separated by a spacer, allowing us to flush the cell continuously with a flow of N2 gas saturated with 2H2O. Exchange occurred simultaneously for all proteins and single images covering ca. 96 spots of proteins that could be recorded on-line at selected time points. Each protein spot contained ca. 5 ng protein, and the entire array covered 2.5 × 2.5 mm2. Furthermore, HDX could be monitored in real time, and the experiment was therefore not subject to back-exchange problems. Analysis of HDX curves by inverse Laplace transform and by fitting exponential curves indicated that quantitative comparison of the samples is feasible. The paper also demonstrates how the whole process of analysis can be automatized to yield fast analyses. Full article
(This article belongs to the Special Issue Protein Structure Research 2024)
15 pages, 2322 KiB  
Article
Experimental Determination of Influences of Static Eccentricities on the Structural Dynamic Behavior of a Permanent Magnet Synchronous Machine
by Julius Müller, Marius Franck, Kevin Jansen, Gregor Höpfner, Jörg Berroth, Georg Jacobs and Kay Hameyer
Machines 2024, 12(9), 649; https://doi.org/10.3390/machines12090649 - 16 Sep 2024
Viewed by 199
Abstract
In electrified vehicles, the masking noise behavior of internal combustion engines is absent, making the tonal excitation of the electric machine particularly noticeable in vehicle acoustics, which is perceived as disturbing by consumers. Due to manufacturing tolerances, the tonal NVH characteristics of the [...] Read more.
In electrified vehicles, the masking noise behavior of internal combustion engines is absent, making the tonal excitation of the electric machine particularly noticeable in vehicle acoustics, which is perceived as disturbing by consumers. Due to manufacturing tolerances, the tonal NVH characteristics of the electric machine are significantly influenced at wide frequency ranges. This paper presents a systematic exploration of the influence of static eccentricity as one manufacturing tolerance on the NVH behavior of Permanent Magnet Synchronous Machines (PMSMs). The study utilizes a novel test bench setup enabling isolated variations in static eccentricity of up to 0.2 mm in one PMSM. Comparative analysis of acceleration signals reveals significant variations in the dominance of excitation orders with different eccentricity states, impacting critical operating points and dominant frequency rages of the electric machine. Despite experimentation, no linear correlation is observed between increased eccentricity and changes in acceleration behavior. Manufacturing eccentricity and deviations in rotor magnetization are discussed as potential contributors to the observed effects. The findings emphasize static eccentricity as a critical parameter in NVH optimization, particularly in electrified powertrains. However, the results indicate that further investigations are needed to explore the influence of eccentricities and magnetization deviations on NVH behavior comprehensively. Full article
(This article belongs to the Section Machines Testing and Maintenance)
22 pages, 3249 KiB  
Article
LSTM-Autoencoder Based Detection of Time-Series Noise Signals for Water Supply and Sewer Pipe Leakages
by Yungyeong Shin, Kwang Yoon Na, Si Eun Kim, Eun Ji Kyung, Hyun Gyu Choi and Jongpil Jeong
Water 2024, 16(18), 2631; https://doi.org/10.3390/w16182631 - 16 Sep 2024
Viewed by 300
Abstract
The efficient management of urban water distribution networks is crucial for public health and urban development. One of the major challenges is the quick and accurate detection of leaks, which can lead to water loss, infrastructure damage, and environmental hazards. Many existing leak [...] Read more.
The efficient management of urban water distribution networks is crucial for public health and urban development. One of the major challenges is the quick and accurate detection of leaks, which can lead to water loss, infrastructure damage, and environmental hazards. Many existing leak detection methods are ineffective, especially in complex and aging pipeline networks. If these limitations are not overcome, it can result in a chain of infrastructure failures, exacerbating damage, increasing repair costs, and causing water shortages and public health risks. The leak issue is further complicated by increasing urban water demand, climate change, and population growth. Therefore, there is an urgent need for intelligent systems that can overcome the limitations of traditional methodologies and leverage sophisticated data analysis and machine learning technologies. In this study, we propose a reliable and advanced method for detecting leaks in water pipes using a framework based on Long Short-Term Memory (LSTM) networks combined with autoencoders. The framework is designed to manage the temporal dimension of time-series data and is enhanced with ensemble learning techniques, making it sensitive to subtle signals indicating leaks while robustly dealing with noise signals. Through the integration of signal processing and pattern recognition, the machine learning-based model addresses the leak detection problem, providing an intelligent system that enhances environmental protection and resource management. The proposed approach greatly enhances the accuracy and precision of leak detection, making essential contributions in the field and offering promising prospects for the future of sustainable water management strategies. Full article
(This article belongs to the Special Issue Prediction and Assessment of Hydrological Processes)
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<p>Water supply and sewage system.</p>
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<p>LSTM-autoencoder architecture.</p>
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<p>Proposed framework.</p>
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<p>Actual valve installation site.</p>
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<p>Completed sensor installation.</p>
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<p>Sensor installation close to the ground.</p>
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<p>Use case of leak detection.</p>
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<p>Leak data without noise.</p>
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<p>FFT for leak data.</p>
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<p>Actual and predicted values for data without noise.</p>
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<p>Actual and predicted values for data with noise.</p>
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<p>Noise attenuation.</p>
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<p>Accuracy.</p>
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<p>Precision.</p>
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<p>Recall.</p>
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<p>F1 scores.</p>
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<p>AUC scores.</p>
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