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Search Results (352)

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Keywords = nanoparticles and microparticles

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32 pages, 7358 KiB  
Article
Retention of Engineered Nanoparticles in Drinking Water Treatment Processes: Laboratory and Pilot-Scale Experiments
by Norbert Konradt, Laura Schneider, Stefan Bianga, Detlef Schroden, Peter Janknecht and Georg Krekel
Appl. Nano 2024, 5(4), 279-310; https://doi.org/10.3390/applnano5040018 - 5 Dec 2024
Viewed by 533
Abstract
While microparticles can be removed by a filtration step at a drinking water treatment plant (DWTP), engineered nanoparticles (ENPs), which are widely used in industry, commerce and households, pose a major problem due to their special properties, e.g., size, reactivity and polarity. In [...] Read more.
While microparticles can be removed by a filtration step at a drinking water treatment plant (DWTP), engineered nanoparticles (ENPs), which are widely used in industry, commerce and households, pose a major problem due to their special properties, e.g., size, reactivity and polarity. In addition, many ENPs exhibit toxic potential, which makes their presence in drinking water undesirable. Therefore, this study investigated the removal of ENPs in the laboratory and at a pilot-scale DWTP. Eight ENPs were synthesized and tested for stability in different types of water. Only three of them were stable in natural water: cetyltrimethylammonium bromide-coated gold (CTAB/AuNPs), polyvinylpyrrolidone-stabilized gold and silver nanoparticles (PVP/AuNPs, PVP/AgNPs). Their retention on quartz sand, silica gel and fresh anthracite was low, but CTAB/AuNPs could be retained on fresh river sand and thus should not overcome riverbank filtration, while PVP/AuNPs and PVP/AgNPs showed no retention and may be present in raw water. During ozonation, PVP/AuNPs remained stable while PVP/AgNPs were partially degraded. The advanced oxidation process (AOP) was less effective than ozone. PVP/AgNPs were almost completely retained on the pilot plant anthracite sand filter coated with manganese(IV) oxide and ferrihydrite from raw water treatment. PVP/AuNPs passed the filter with no retention. In contrast to PVP/AuNPs, PVP/AgNPs and CTAB/AuNPs were also retained on activated carbon. The integration of a flocculation step with iron(III) salts can improve ENP removal, with PVP/AuNPs requiring higher flocculant doses than PVP/AgNPs. PVP/AuNPs, in particular, are well-suited for testing the effectiveness of water treatment. Further data on the occurrence of stable ENPs in raw water and their behavior during water treatment are needed to perform a risk assessment and derive the measures. Full article
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Figure 1
<p>Classification of matter in water (green) and common separations methods (blue).</p>
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<p>(<b>a</b>) Trisodium citrate; (<b>b</b>) cetyltrimethylammonium bromide (CTAB); (<b>c</b>) polyvinylpyrrolidone (PVP).</p>
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<p>Schematic of the pilot plant with aeration, ozonation and anthracite sand filter with sampling points. A detailed description of the sampling points is provided in the <a href="#app1-applnano-05-00018" class="html-app">Supplementary Data, Section S4</a>.</p>
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<p>Breakthrough curve and determination of the 50% breakthrough time.</p>
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<p>UV-VIS spectra of CA/AuNPs (<b>a</b>) diluted in DI (green), DW (red) and RH (black); (<b>b</b>) CA/AuNPs dispersions diluted with DI, DW and RH (from left to right) with c(Au) = 17.9 mg L<sup>−1</sup>.</p>
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<p>UV-VIS absorption spectra of the diluted CTAB/AuNPs in DI (black), DW (red) and RH (green) with c(Au) = 10 mg L<sup>−1</sup>.</p>
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<p>UV-Vis absorption spectra of the diluted PVP/AuNPs in DI (black), DW (red) and RH (green) with c(Au) = 5.88 mg L<sup>−1</sup>.</p>
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<p>UV-Vis absorption spectra of the diluted PVP/AgNPs in DI (black), DW (red) and RH (green) with c(Ag) = 20.2 mg L<sup>−1</sup>.</p>
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<p>Adsorption isotherm data for PVP/AgNPs as Ag on sand (dots) with (<b>a</b>) Langmuir and (<b>b</b>) Freundlich regression lines.</p>
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<p>Adsorption isotherm data for PVP/AgNPs as Ag on silica gel (dots) with (<b>a</b>) Langmuir and (<b>b</b>) Freundlich regression lines.</p>
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<p>Breakthrough curves of stable ENPs in DW (flow rate 0.8 mL/min) for a 10 g quartz sand bed.</p>
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<p>Breakthrough curves of DW-stable ENPs in RH (flow rate 0.8 mL/min) for a 10 g non-treated Rhine sand bed.</p>
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<p>Breakthrough curves of stable NPs in RH (flow rate 2 mL/min) for a 0.5 g silica gel bed.</p>
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<p>Breakthrough curves of stable NPs in DW (flow rate 2.0 mL/min) for a 0.5 g activated carbon bed.</p>
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<p>Breakthrough curves of PVP-coated NPs in RH (flow rate 2 mL/min) for a fresh anthracite bed (3.15 g).</p>
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<p>Breakthrough curves of PVP-coated NPs in RH (flow rate 2 mL/min) for a used anthracite (3.40 g) from the pilot plant.</p>
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<p>Flocculation of ENPs. Error bars correspond to the relative combined uncertainty of ~7% (<a href="#app1-applnano-05-00018" class="html-app">Supplementary Data, Table S18</a>).</p>
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<p>Retention of PVP/AuNPs on a pilot scale with ozonation and anthracite sand filtration. The location of the sampling points is shown in <a href="#applnano-05-00018-f003" class="html-fig">Figure 3</a>. The data points of the same sampling points are connected to improve clarity.</p>
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<p>Retention of PVP/AgNPs at the pilot plant with ozonation and anthracite sand filtration. The data points of the same sampling points are connected to improve clarity.</p>
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16 pages, 7589 KiB  
Article
Effect of Hybrid Addition of Boron Nitride and Vanadium Carbide on Microstructure, Tribological, and Mechanical Properties of the AA6061 Al-Based Composites Fabricated by FSP
by Ahmad H. Milyani, Ahmed O. Mosleh and Essam B. Moustafa
J. Compos. Sci. 2024, 8(12), 500; https://doi.org/10.3390/jcs8120500 - 1 Dec 2024
Viewed by 678
Abstract
This work investigates the impact of friction stir processing (FSP) on the microstructure and mechanical characteristics of AA 6061 alloy and its composites, which are strengthened with boron nitride nanoparticles and vanadium carbide microparticles. Composite samples were created using different proportions of reinforcing [...] Read more.
This work investigates the impact of friction stir processing (FSP) on the microstructure and mechanical characteristics of AA 6061 alloy and its composites, which are strengthened with boron nitride nanoparticles and vanadium carbide microparticles. Composite samples were created using different proportions of reinforcing particles, including mono and hybrid composites. The efficacy of FSP as a technological method for enhancing the grain size of AA 6061 alloy and its composites has been proven. Adding reinforcing particles led to enhanced grain refinement, especially when using VC particles, which demonstrated greater efficacy than BN particles; thus, mono composite AA6061/VC shows the highest percentage reduction (94.29%) in grain size. Hybrid composites with a higher concentration of VC particles exhibited a more symmetrical microhardness profile. The microhardness of hybrid composites with a larger concentration of VC particles (40 vol.%BN + 60 vol.%VC) shows the most significant enhancement, with an increase of 51.61%. The Young’s and shear modulus of all composite samples processed by (FSP) had greater values than the wrought AA 6061 alloy. The investigated composite samples, especially 60% BN and 40% VC, enhanced the tribological properties of AA6061 and reduced the wear rate by about 52%. The observed characteristics may be due to BN and VC particles in the hybrid compost. This is because these particles effectively prevent grain elongation and inconsistent movement. This is because reinforcing particles can be tailored to have specific properties for specific applications. Full article
(This article belongs to the Section Metal Composites)
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<p>TEM images of the investigated reinforcement particles (<b>a</b>) BN, (<b>b</b>) VC.</p>
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<p>Friction stir process schematic drawing and design.</p>
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<p>Manufacturing the composite sheet using FSP: (<b>a</b>) typical FSP process using a milling machine, (<b>b</b>) a thermal image during the manufacturing process.</p>
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<p>Optical micrographs showing the grain structure of (<b>a</b>) AA 6061 base alloy and (<b>b</b>) the refined grain structure in the stirred zone after friction stir processing (FSP), (<b>b</b>) Al/BN, (<b>c</b>) Al/VC, and (<b>d</b>) hybrid Al/50%BN + 50%VC.</p>
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<p>Grain size distribution of the manufactured composites in the stirred zone: (<b>a</b>) Al/BN, (<b>b</b>) Al/VC, and (<b>c</b>) hybrid Al/50%BN + 50%VC.</p>
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<p>Percentage of grain refinement due to friction stir processing (FSP) in AA 6061 alloy and its composites.</p>
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<p>(SEM) images of hybrid composite samples containing (<b>a</b>) AA6061/BN mono composite, (<b>b</b>) AA6061/VC mono composite, and (<b>c</b>) hybrid composite AA6061/40%BN + 60%VC.</p>
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<p>(SEM) images of hybrid composite samples containing (<b>a</b>) 60% BN + 40%VC, (<b>b</b>) hybrid composite AA6061/50%BN + 50%VC.</p>
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<p>Bulk density values of the investigated samples.</p>
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<p>Microhardness behavior (<b>a</b>) AVG microhardness value in the stirred zone; mechanical properties: (<b>b</b>) profile of the base metal, mono composite, and hybrid composite samples fabricated through friction stir processing (FSP).</p>
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<p>Mechanical properties: (<b>a</b>) Young’s modulus of AA 6061 alloy and its composites with different reinforcement percentages, (<b>b</b>) influence of shear modulus on AA 6061 alloy and its composites.</p>
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<p>The wear rate behavior of the investigated sample using the weight loss method.</p>
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<p>The radar plot shows the comparative performance of AA6061 and its composites.</p>
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15 pages, 4496 KiB  
Article
ZnOnp/CaCO3 Core–Shell Nanoparticle Coatings on Kraft Paper: A Comparative Study of Antimicrobial Efficacy, Tensile Strength, and Hydrophobicity
by Theerarat Sengsuk, Nicha Yotthanon, Ponusa Songtipya, Yeampon Nakaramontri, Waranyou Sridach and Ladawan Songtipya
Coatings 2024, 14(12), 1501; https://doi.org/10.3390/coatings14121501 - 28 Nov 2024
Viewed by 419
Abstract
This study introduces a novel paper coating approach using modified zinc oxide (ZnO), providing a comparison with conventional materials used in the paper industry. The research focused on determining the concentration for effective microbial growth inhibition and evaluates the impact of different ZnO [...] Read more.
This study introduces a novel paper coating approach using modified zinc oxide (ZnO), providing a comparison with conventional materials used in the paper industry. The research focused on determining the concentration for effective microbial growth inhibition and evaluates the impact of different ZnO types on coated-paper properties, including antimicrobial activity, surface morphology, tensile strength, and water absorption. Specifically, ZnO microparticles (ZnOws), ZnO nanoparticles (ZnOnp), and modified ZnOnp (ZnOnp-CaCO3, with a core–shell structure composed of calcium carbonate [CaCO3] and nano-zinc oxide) were incorporated into coating formulations at varying concentrations (0 × MIC, 1 × MIC, 2 × MIC, and 3 × MIC, based on minimum inhibitory concentrations [MICs]). The results demonstrated that among all tested microorganisms, ZnOnp-CaCO3 showed the lowest MIC values. ZnOnp-CaCO3-coated paper exhibited superior antimicrobial activity against both Gram-positive and Gram-negative bacteria, as well as fungi, outperforming ZnOws and ZnOnp. At 1 × MIC, %inhibition for E. coli, S. aureus, and A. niger were 98.3%, 99.1%, and 90.8%, respectively. Additionally, ZnOnp-CaCO3 coatings caused minimal color change in the paper compared to the other ZnO variants. The coating did not negatively impact the mechanical properties of the paper across all ZnO types and concentrations. Water absorption tests showed increased hydrophobicity with higher ZnO content, with ZnOnp and ZnOnp-CaCO3 exhibiting greater reductions in water absorption than ZnOws. Overall, ZnOnp-CaCO3 showed strong potential as an antimicrobial agent for paper surfaces, making it ideal for packaging and hygiene products. By partially replacing ZnOnp with inexpensive CaCO3 core particles, ZnOnp-CaCO3 delivers enhanced performance, reduced costs, and greater sustainability for large-scale applications. Full article
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<p>MIC testing of the effect of ZnO<sub>np</sub>-CaCO<sub>3</sub> on the growth of <span class="html-italic">E. coli</span>, <span class="html-italic">S. aureus</span>, and <span class="html-italic">A. niger.</span></p>
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<p>Visual appearance of the uncoated papers and the papers coated with different types and concentrations of ZnO.</p>
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<p>Surface images of (<b>A</b>) uncoated paper; (<b>B</b>) paper coated with a starch solution, without ZnO; and papers coated with (<b>C</b>) ZnO<sub>ws</sub>, (<b>D</b>) ZnO<sub>np</sub>, and (<b>E</b>) ZnO<sub>np</sub>-CaCO<sub>3</sub> at 1 × MIC.</p>
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<p>Growth inhibition of (<b>A</b>) <span class="html-italic">E. coli</span>, (<b>B</b>) <span class="html-italic">S. aureus</span>, and (<b>C</b>) <span class="html-italic">A. niger</span> by uncoated papers and papers coated with different types and concentrations of ZnO. Note: Significant differences (<span class="html-italic">p</span> &lt; 0.05) were indicated by different letters above the bars.</p>
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<p>SEM images of fixed bacterial and fungal cells before and after treatment with 1 × MIC ZnO<sub>np</sub>-CaCO<sub>3</sub>.</p>
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<p>Schematic diagram of the bacterial fixation procedure (<span class="html-italic">E. coli</span> and <span class="html-italic">S. aureus</span>) for morphological analysis via SEM.</p>
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<p>Schematic diagram of the fungal fixation procedure (<span class="html-italic">A. niger</span>) for morphological analysis via SEM.</p>
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17 pages, 4840 KiB  
Article
Dulcitol/Starch Systems as Shape-Stabilized Phase Change Materials for Long-Term Thermal Energy Storage
by Martyna Szatkowska and Kinga Pielichowska
Polymers 2024, 16(22), 3229; https://doi.org/10.3390/polym16223229 - 20 Nov 2024
Viewed by 654
Abstract
In recent years, there has been an increasing interest in phase change materials (PCM) based on dulcitol and other sugar alcohols. These materials have almost twice as large latent heat of fusion as other organic materials. Sugar alcohols are relatively cheap, and they [...] Read more.
In recent years, there has been an increasing interest in phase change materials (PCM) based on dulcitol and other sugar alcohols. These materials have almost twice as large latent heat of fusion as other organic materials. Sugar alcohols are relatively cheap, and they can undergo cold crystallization, which is crucial for long-term thermal energy storage. The disadvantage of dulcitol and other sugar alcohols is the solid–liquid phase transition. As a result, the state of matter of the material and its volume change, and in the case of materials modified with microparticles or nanoparticles, sedimentation of additives in liquid PCM can occur. In this study, we obtained shape-stable phase change materials (SSPCM) by co-gelation of starch and dulcitol. To characterize the samples obtained, differential scanning calorimetry (DSC), step-mode DSC, thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM) were used, and they were also used to test for shape stabilization. The results show that the obtained systems have great potential as shape-stabilized phase change materials. The sample dulcitol/starch with a 50:50 ratio exhibited the highest heat of cold crystallization, up to 52.90 J/g, while the heat of melting was 126.16 J/g under typical DSC measuring conditions. However, depending on the applied heating program, the heat of cold crystallization can even reach 125 J/g. The thermal stability of all compositions was higher than the phase change temperature, with only 1% mass loss occurring at temperatures above 200 °C, while the phase change occurred at a maximum of 190 °C. Full article
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<p>Scheme of preparation of the samples.</p>
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<p>DSC curves for dulcitol/starch heating (<b>a</b>,<b>b</b>) and cooling (<b>c</b>,<b>d</b>).</p>
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<p>DSC curves for dulcitol/starch heating according to temperature programs 1–6, diagrams (<b>a</b>–<b>f</b>) respectively. Diagrams (<b>g</b>–<b>i</b>) are isothermal segment for program 4–6 respectively.</p>
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<p>The storage capacity of dulcitol/starch PCMs.</p>
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<p>TG (<b>a</b>) and DTG (<b>b</b>) curves for dulcitol/starch systems.</p>
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<p>Samples subjected to shape stability analysis: (<b>a</b>) samples before analysis, (<b>b</b>) after 15 min in the dryer at 190 °C, and (<b>c</b>) after 15 min in the dryer at 210 °C.</p>
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<p>Basic chemical structural formulas of amylopectin (<b>a</b>), amylase (<b>b</b>), dulcitol (<b>c</b>) and hydrogen bond formation between amylopectin and dulcitol (<b>d</b>), amylase and dulcitol (<b>e</b>).</p>
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<p>FTIR spectra of dulcitol/starch systems.</p>
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<p>SEM microphotographs (350×) of the obtained dulcitol/starch PCMs with different mass ratios: (<b>a</b>) 50:50, (<b>b</b>) 60:40, (<b>c</b>) 70:30, (<b>d</b>) 80:20, (<b>e</b>) 85:15, (<b>f</b>) 90:10, (<b>g</b>) 100:0.</p>
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<p>SEM (1000×) microstructural observations and EDX analysis on sample dulcitol/starch with mass ratio 85:15 <span class="html-italic">w</span>/<span class="html-italic">w</span>.</p>
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<p>Optical microscopy (50×) microstructural observations of the obtained dulcitol/starch PCMs with different mass ratios: (<b>a</b>) 50:50, (<b>b</b>) 60:40, (<b>c</b>) 70:30, (<b>d</b>) 80:20, (<b>e</b>) 85:15, (<b>f</b>) 90:10, (<b>g</b>) 100:0.</p>
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20 pages, 10850 KiB  
Article
Lipid–Polymer Hybrid Nanoparticles in Microparticle-Based Powder: Evaluating the Potential of Methylprednisolone Delivery for Future Lung Disease Treatment via Inhalation
by Cinzia Scialabba, Emanuela Fabiola Craparo, Sofia Bonsignore, Marta Cabibbo and Gennara Cavallaro
Pharmaceutics 2024, 16(11), 1454; https://doi.org/10.3390/pharmaceutics16111454 - 14 Nov 2024
Viewed by 657
Abstract
Background. Lipid–polymer hybrid nanoparticles (LPHNPs) offer a promising method for delivering methylprednisolone (MePD) to treat lung inflammation, addressing aggregation issues seen with polymer-only formulations. Objectives. This study aimed to develop LPHNPs for MePD delivery, assessing their physicochemical properties, drug loading, cytocompatibility, and release [...] Read more.
Background. Lipid–polymer hybrid nanoparticles (LPHNPs) offer a promising method for delivering methylprednisolone (MePD) to treat lung inflammation, addressing aggregation issues seen with polymer-only formulations. Objectives. This study aimed to develop LPHNPs for MePD delivery, assessing their physicochemical properties, drug loading, cytocompatibility, and release profiles, ultimately enabling inhalable microparticle-based powder. Methods. The nanoparticles were formulated using α,β-poly(N-2-hydroxyethyl)-DL-aspartamide-g-Rhodamine B-g-poly(lactic acid) (PHEA-g-RhB-g-PLA) and phospholipids DPPC, DOTAP, and DSPE-PEG2000 in a 45:30:25 weight ratio. Their size, redispersion after freeze-drying, drug loading (DL%), and controlled release were evaluated. Cytocompatibility was assessed on 16-HBE cell lines, measuring anti-inflammatory effects via IL-6 and IL-8 levels. Spray drying was optimized to produce microparticles using mannitol (MAN), leucine (LEU), and N-acetylcysteine (NAC). Results. The nanoparticles had a size of 186 nm and a DL% of 2.9% for MePD. They showed good cytocompatibility, significantly reducing IL-6 and IL-8 levels. Spray drying yielded microparticles with a fine particle fraction (FPF) of 62.3% and a mass median aerodynamic diameter (MMAD) of 3.9 µm. Inclusion of LPHNPs@MePD (0.25% w/v) resulted in FPF and MMAD values of 56.7% and 4.4 µm. In conclusion, this study described the production of novel inhalable powders as carriers for MePD-loaded nanostructures with favorable physicochemical properties, cytocompatibility, and promising aerosol performance, indicating their potential as an effective inhalable therapy for lung inflammation with corticosteroids, especially for treating chronic diseases. Full article
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<p>Z Average, PDI, and ζ potential values of empty and drug-loaded NPs and LPHNPs, before and after lyophilization. The number above the histogram represents the PDI of the Z average.</p>
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<p>MePD release profile from LPHNPs (dashed line) and NPs@MePD (solid line), in SLF4 (black), DPBS (red), and ALF (blue).</p>
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<p>Cell viability % (MTS assay) on 16-HBE cells after 24 and 48 h of incubation with MePD, LPHNPs@MePD, and LPHNPs. The results are reported as the mean ± SD (n = 3).</p>
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<p>Evaluation of MePD, free or loaded into LPHNPs, and empty LPHNPs effects on 16-HBE cells as cytokine IL-6 e IL-8 production via ELISA test.</p>
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<p>SEM images depicting samples MPs_A, MPs_B, MPs_C, and MPs_D with magnifications of 500× (upper) and 3000× (down).</p>
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<p>Characteristics of the samples obtained via SD in terms of geometric diameter (d<sub>geo</sub>), bulk density (ρ<sub>bulk</sub>), tapped density (ρ<sub>tapped</sub>), aerodynamic diameter (d<sub>aer</sub>), and Hausner Index (H).</p>
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<p>SEM images depicting samples MPs_C1, MPs_C2, and NiM@MePD (containing LPHNPs at 0.25% <span class="html-italic">w</span>/<span class="html-italic">v</span>), with magnifications of 500× (upper) and 3000× (down).</p>
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<p>Geometric diameter (d<sub>geo</sub>), bulk density (ρb), tapped density (ρ<sub>tapped</sub>), aerodynamic diameter (d<sub>aer</sub>), and Hausner Index (H) of MPs_C1, MPs_C2 and NiM@MePD samples. MPs_C sample is reported for comparison.</p>
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<p>Deposition of MPs_C, MPs_C1, MPs_C2 and NiM@MePD samples on the stages of the ACI, after testing via Breezhaler<sup>®</sup> at a flow rate of 90 L/min.</p>
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<p>Transmittance at 650 nm of dispersions containing mucin alone, MPs_C1, NiM@MePD and LPHNPs@MePD samples (1 mg/mL), in water or in mucin dispersion at final concentration of 0.08% <span class="html-italic">w</span>/<span class="html-italic">v</span>.</p>
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<p>Schematic representation of the Nano into Microparticle (NiM) production starting from hybrid nanoparticles (LPHNPs@MePD) and excipients (Mann, LEU, NAC), and characterization.</p>
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22 pages, 7689 KiB  
Article
Influence of SS316L Nanoparticles on the Sintered Properties of Two-Component Micro-Powder Injection Moulded Bimodal SS316L/Zirconia Bi-Materials
by Al Basir, Abu Bakar Sulong, Norhamidi Muhamad, Afifah Z. Juri, Nashrah Hani Jamadon, Farhana Mohd Foudzi, Nabilah Afiqah Mohd Radzuan and Kambiz Rashidi
Materials 2024, 17(22), 5536; https://doi.org/10.3390/ma17225536 - 13 Nov 2024
Viewed by 564
Abstract
Two-component micro-powder injection moulding (2C-μPIM) is a prospective approach for fabricating bi-material micro-components of stainless steel 316L (SS316L) and 3 mol% yttria-stabilised zirconia (3YSZ) at an appealing cost. However, the fundamental challenge lies in preventing the formation of large-scale cracks at the interface [...] Read more.
Two-component micro-powder injection moulding (2C-μPIM) is a prospective approach for fabricating bi-material micro-components of stainless steel 316L (SS316L) and 3 mol% yttria-stabilised zirconia (3YSZ) at an appealing cost. However, the fundamental challenge lies in preventing the formation of large-scale cracks at the interface of two different materials during sintering. This study investigated how SS316L nanoparticles in bimodally configured SS316L powder that incorporated both nanoparticles and microparticles influenced the sintering of 2C-μPIM-processed miniature bi-materials made of bimodal SS316L and 3YSZ. In this study, feedstocks were developed by integrating monomodal (micro-sized) SS316L powder, three types of nano/micro-bimodal SS316L powders, and 3YSZ powder individually with palm stearin and low-density polyethylene binders. The results indicated that increasing the SS316L nanoparticle content to 45 vol.% caused a 19.5% increase in the critical powder loading in the bimodal SS316L powder as compared to that in the monomodal SS316L powder. The addition of SS316L nanoparticles increased the relative density and hardness of the sintered bi-materials, with the maximum values obtained being 96.8% and 1156.8 HV, respectively. Field emission scanning electron microscopy investigations revealed that adding 15 vol.% and 30 vol.% SS316L nanoparticle contents reduced interface cracks in bi-materials significantly, while 45 vol.% resulted in a crack-free interface. Full article
(This article belongs to the Special Issue Advances in Materials Processing (3rd Edition))
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<p>Morphology of the powders: (<b>a</b>) FESEM image of SS316L nanopowder, (<b>b</b>) FESEM image of SS316L micropowder, (<b>c</b>) FESEM image of bimodal SS316L powder with nanopowder content of 15 vol.%, (<b>d</b>) FESEM image of bimodal SS316L powder with nanopowder content of 30 vol.%, (<b>e</b>) FESEM image of bimodal SS316L powder with nanopowder content of 45 vol.%, and (<b>f</b>–<b>h</b>) TEM images of 3YSZ powder at different magnifications.</p>
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<p>Diagram depicting the steps involved in thermal debinding and sintering.</p>
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<p>Critical powder contents of (<b>a</b>) monomodal and bimodal SS316L powders and (<b>b</b>) 3YSZ powder.</p>
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<p>Mixing curves of the feedstocks: (<b>a</b>) monomodal and bimodal SS316L and (<b>b</b>) 3YSZ.</p>
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<p>FESEM micrographs of the feedstocks: (<b>a</b>) monomodal SS316L, (<b>b</b>) 45:55 bimodal SS316L, and (<b>c</b>) 3YSZ.</p>
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<p>Variation in viscosity with shear rate for (<b>a</b>) monomodal SS316L, (<b>b</b>) 15:85 bimodal SS316L, (<b>c</b>) 30:70 bimodal SS316L, (<b>d</b>) 45:55 bimodal SS316L, and (<b>e</b>) 3YSZ feedstocks.</p>
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<p>(<b>a</b>) Green monomodal SS316L/3YSZ and 45:55 bimodal SS316L/3YSZ micro-components, (<b>b</b>) FESEM image of the joining region of green monomodal SS316L/3YSZ micro-component, and (<b>c</b>) FESEM image of the joining region of green 45:55 bimodal SS316L/3YSZ micro-component.</p>
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<p>(<b>a</b>) Mass loss of palm stearin binder during solvent extraction process from (<b>a</b>) monomodal SS316L/3YSZ, (<b>b</b>) 15:85 bimodal SS316L/3YSZ, (<b>c</b>) 30:70 bimodal SS316L/3YSZ, and (<b>d</b>) 45:55 bimodal SS316L/3YSZ micro-components.</p>
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<p>TGA graph of 45:55 bimodal SS316L/3YSZ micro-component (a) before and (b) after thermal debinding at 550 °C.</p>
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<p>Variation in relative densities in sintered bi-materials with increasing SS316L nanoparticle contents.</p>
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<p>Photograph of micro-injection moulded and sintered bi-material.</p>
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<p>Variation in linear shrinkages in sintered bi-materials with increasing SS316L nanoparticle contents.</p>
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<p>FESEM images exhibiting three different regions of the interfaces of the bi-materials: (<b>a</b>–<b>c</b>) monomodal SS316L/3YSZ micro-component, (<b>d</b>–<b>f</b>) 15:85 bimodal SS316L/3YSZ micro-component, (<b>g</b>–<b>i</b>) 30:70 bimodal SS316L/3YSZ micro-component, and (<b>j</b>–<b>l</b>) 45:55 bimodal SS316L/3YSZ micro-component.</p>
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<p>EDX mapping of the sintered 45:55 bimodal SS316L/3YSZ micro-component: (<b>a</b>) layered image, (<b>b</b>) Zr map, (<b>c</b>) Fe map, (<b>d</b>) O map, (<b>e</b>) Cr map, and (<b>f</b>) Ni map.</p>
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<p>Effect of addition of nanoparticles on the hardness values of the joining region of sintered bi-materials.</p>
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18 pages, 5513 KiB  
Article
Novel Hybrid Catalysts of Cysteine Proteases Enhanced by Chitosan and Carboxymethyl Chitosan Micro- and Nanoparticles
by Marina Holyavka, Yulia Redko, Svetlana Goncharova, Maria Lavlinskaya, Andrey Sorokin, Maxim Kondratyev and Valery Artyukhov
Polymers 2024, 16(22), 3111; https://doi.org/10.3390/polym16223111 - 6 Nov 2024
Viewed by 884
Abstract
Micro- and nanoparticles of chitosan and carboxymethyl chitosan were synthesized, both with and without ascorbic acid. Methods were developed to form complexes between these micro- and nanoparticles and plant proteases—ficin, papain, and bromelain. It was demonstrated that the activity of cysteine protease complexes [...] Read more.
Micro- and nanoparticles of chitosan and carboxymethyl chitosan were synthesized, both with and without ascorbic acid. Methods were developed to form complexes between these micro- and nanoparticles and plant proteases—ficin, papain, and bromelain. It was demonstrated that the activity of cysteine protease complexes with carboxymethyl chitosan micro- and nanoparticles was higher compared to those with chitosan micro- and nanoparticles. Additionally, the complexes of ficin, papain, and bromelain with chitosan and carboxymethyl chitosan micro- and nanoparticles synthesized in the presence of ascorbic acid exhibited greater proteolytic activity than those formed with particles prepared without ascorbic acid. Molecular docking studies revealed that the amino acid residues of ficin, papain, and bromelain primarily interact with chitosan and carboxymethyl chitosan through hydrogen bonding and hydrophobic interactions. The amino acid residues in the active sites of these enzymes participate in a complex formation, which likely contributes to the increased activity and stability of cysteine proteases in complexes with chitosan and carboxymethyl chitosan micro- and nanoparticles. Full article
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<p>Distribution of microparticles (<b>A</b>) and nanoparticles (<b>B</b>) of chitosan and microparticles (<b>C</b>) and nanoparticles (<b>D</b>) of carboxymethyl chitosan by size: 1–200 kDa; 2–200 kDa with ascorbic acid; and 3–350 kDa; 4–350 kDa with ascorbic acid.</p>
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<p>Catalytic (proteolytic) activity (<b>left</b>) and residual catalytic activity (<b>center</b>, <b>right</b>) of ficin, papain, and bromelain: free (1); in a complex with Ch200Mp/CMCh200Mp (2); Ch200MpAsc/CMCh200MpAsc (3); Ch350Mp/CMCh350Mp (4); Ch350MpAsc/CMCh350MpAsc (5); Ch200Np/CMCh200Np (6); Ch200NpAsc/CMCh200NpAsc (7); Ch350Np/CMCh350Np (8); and Ch350NpAsc/CMCh350NpAsc (9). The activity of free enzymes under optimum hydrolysis conditions (<b>left</b>) and the activity of the samples without their pre-incubation and under optimal hydrolysis conditions (<b>center</b>, <b>right</b>) were taken as 100%. * indicates statistical differences.</p>
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<p>Bonds and interactions in complexes of ficin with chitosan and carboxymethyl chitosan with and without ascorbic acid: dashed lines indicate hydrogen bonds, and their lengths are given in Å. Red arcs indicate the presence of weak physical interactions (electrostatic, hydrophobic, and van der Waals) between the amino acid residues of the enzyme and the carrier/ligand. C-atoms are black, O-atoms are red, N-atoms are blue.</p>
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<p>Bonds and interactions in complexes of papain with chitosan and carboxymethyl chitosan with and without ascorbic acid: dashed lines indicate hydrogen bonds, and their lengths are given in Å. Red arcs indicate the presence of weak physical interactions (electrostatic, hydrophobic, and van der Waals) between the amino acid residues of the enzyme and the carrier/ligand. C-atoms are black, O-atoms are red, N-atoms are blue.</p>
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<p>Bonds and interactions in bromelain complexes with chitosan and carboxymethyl chitosan with and without ascorbic acid: dashed lines indicate hydrogen bonds, and their lengths are given in Å. Red arcs indicate the presence of weak physical interactions (electrostatic, hydrophobic, and van der Waals) between the amino acid residues of the enzyme and the carrier/ligand. C-atoms are black, O-atoms are red, N-atoms are blue.</p>
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22 pages, 7402 KiB  
Article
Development of Nanocomposite Microspheres for Nasal Administration of Deferiprone in Neurodegenerative Disorders
by Radka Boyuklieva, Plamen Katsarov, Plamen Zagorchev, Silviya Abarova, Asya Hristozova and Bissera Pilicheva
J. Funct. Biomater. 2024, 15(11), 329; https://doi.org/10.3390/jfb15110329 - 5 Nov 2024
Viewed by 884
Abstract
Elevated brain iron levels are characteristic of many neurodegenerative diseases. As an iron chelator with short biological half-life, deferiprone leads to agranulocytosis and neutropenia with a prolonged therapeutic course. Its inclusion in sustained-release dosage forms may reduce the frequency of administration. On the [...] Read more.
Elevated brain iron levels are characteristic of many neurodegenerative diseases. As an iron chelator with short biological half-life, deferiprone leads to agranulocytosis and neutropenia with a prolonged therapeutic course. Its inclusion in sustained-release dosage forms may reduce the frequency of administration. On the other hand, when administered by an alternative route of administration, such as the nasal route, systemic exposure to deferiprone will be reduced, thereby reducing the occurrence of adverse effects. Direct nose-to-brain delivery has been raised as a non-invasive strategy to deliver drugs to the brain, bypassing the blood–brain barrier. The aim of the study was to develop and characterize nanocomposite microspheres suitable for intranasal administration by combining nano- and microparticle-based approaches. Nanoparticles with an average particle size of 213 ± 56 nm based on the biodegradable polymer poly-ε-caprolactone were developed using the solvent evaporation method. To ensure the deposition of the particles in the nasal cavity and avoid exhalation or deposition into the small airways, the nanoparticles were incorporated into composite structures of sodium alginate obtained by spray drying. Deferiprone demonstrated sustained release from the nanocomposite microspheres and high iron-chelating activity. Full article
(This article belongs to the Special Issue Medical Application of Functional Biomaterials (2nd Edition))
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<p>Chemical structure of DFP (<b>A</b>) and iron ion binding sites (<b>B</b>).</p>
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<p>Schematic illustration of nanoparticle preparation by double emulsion technique (figure created with <a href="http://BioRender.com" target="_blank">BioRender.com</a>).</p>
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<p>Schematic illustration of the experimental set-up for the study of mucoadhesive ability.</p>
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<p>DLS histograms of nanoparticles from batches NP1-DFP (<b>A</b>) and NP2-DFP (<b>B</b>).</p>
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<p>SEM micrograph of DFP-loaded nanoparticles from model NP1-DFP (20,000×).</p>
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<p>TEM micrographs of nanoparticles loaded with DFP from model NP1-DFP (28,000×).</p>
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<p>DFP release profiles from batches NP1-DFP and NP2-DFP.</p>
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<p>SEM micrograph of nanocomposite microspheres from batch M-NP1-DFP (3500×).</p>
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<p>Particle size distribution of batch M-NP1-DFP.</p>
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<p>Release profiles of DFP from nanoparticles (NP1-DFP) and composite microspheres (M-NP1-DFP).</p>
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<p>FTIR spectra of DFP, PCL, sodium alginate, and nanocomposite microparticles of model M-NP1-DFP.</p>
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<p>DSC thermograms of sodium alginate (<b>A</b>), PCL (<b>B</b>), DFP (<b>C</b>), and particles from batches M-NP1-DFP (<b>D</b>) and M-NP-Placebo (<b>E</b>).</p>
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<p>Chronological change of the maximal adhesion force in batch M-NP1-DFP. The symbols *, #, indicate the presence of a statistically significant difference compared to the initial moment (*) and after the established steady state of the process 15 min (#).</p>
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<p>Comparison of Fe-chelating activity of DFP solution, nanocomposite microspheres without the drug (M-NP-Placebo), and DFP-loaded nanocomposite microspheres (M-NP1-DFP). Data is presented as mean values ± SD, <span class="html-italic">n</span> = 3. * Indicates a statistically significant result (<span class="html-italic">p</span> &lt; 0.05).</p>
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<p>Fluorescence spectra of HSA (2.7 mg/mL) upon addition of different volumes of samples containing dispersed particles from batch M-NP1-DFP and placebo particles at 37 °C.</p>
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10 pages, 6033 KiB  
Article
Three-Dimensional (3D) Surface-Enhanced Raman Spectroscopy (SERS) Substrates for Sensing Low-Concentration Molecules in Solution
by Ashutosh Mukherjee, Frank Wackenhut, Alfred J. Meixner, Hermann A. Mayer and Marc Brecht
Nanomaterials 2024, 14(21), 1728; https://doi.org/10.3390/nano14211728 - 29 Oct 2024
Viewed by 678
Abstract
The use of surface-enhanced Raman spectroscopy (SERS) in liquid solutions has always been challenging due to signal fluctuations, inconsistent data, and difficulties in obtaining reliable results, especially at very low analyte concentrations. In our study, we introduce a new method using a three-dimensional [...] Read more.
The use of surface-enhanced Raman spectroscopy (SERS) in liquid solutions has always been challenging due to signal fluctuations, inconsistent data, and difficulties in obtaining reliable results, especially at very low analyte concentrations. In our study, we introduce a new method using a three-dimensional (3D) SERS substrate made of silica microparticles (SMPs) with attached plasmonic nanoparticles (NPs). These SMPs were placed in low-concentration analyte solutions for SERS analysis. In the first approach to perform SERS in a 3D environment, glycerin was used to immobilize the particles, which enabled high-resolution SERS imaging. Additionally, we conducted time-dependent SERS measurements in an aqueous solution, where freely suspended SMPs passed through the laser focus. In both scenarios, EFs larger than 200 were achieved, which enabled the detection of low-abundance analytes. Our study demonstrates a reliable and reproducible method for performing SERS in liquid environments, offering significant advantages for the real-time analysis of dynamic processes, sensitive detection of low-concentration molecules, and potential applications in biomolecular interaction studies, environmental monitoring, and biomedical diagnostics. Full article
(This article belongs to the Special Issue Nanostructures for SERS and Their Applications (2nd Edition))
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<p>(<b>a</b>) Schematics (not to scale) of bottom illumination/collection configuration for SMPs@Ags immersed in a solution of glycerin and MB, and (<b>b</b>) microscopic (bright-field) image of SMP@Ags mixed in glycerin–MB. The image shows that the SMP@Ags are localized in different planes in the solution. Inset: SEM image of an SMP@Ag.</p>
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<p>(<b>a</b>) SERS spectra of glycerin and MB at different spatial positions on SMP@Ags, position 1 (bright region), position 2 (low-intensity region), background (BG), and BG accumulated (BG acc), acquired separately from the same solution with 500 accumulations. Inset: SERS spectra and non-SERS spectra of MB in water (measured separately only for reference). (<b>b</b>) SERS image of an SMP@Ag immersed in glycerin–MB solution at 1626 cm<sup>−1</sup>. The marks show the positions where the spectra in (<b>a</b>) are acquired. (<b>c</b>) Spatial distribution of EF for the MB peak at 1626 cm<sup>−1</sup> and (<b>d</b>) spatial distribution of EF for the glycerin peak at 1464 cm<sup>−1</sup>.</p>
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<p>(<b>a</b>) Video snapshots of SMP@Ags immersed in a water–MB solution passing through a laser spot at different time frames. (<b>b</b>) SERS intensity of MB (at 1626 cm<sup>−1</sup>) measured as a function of time (for a preset duration of 500 s) for SMP@Ags passing through the laser focus spot in a water–MB solution. (<b>c</b>) SERS spectra of MB for the corresponding time frames shown in (<b>b</b>). (<b>d</b>) SERS intensity of MB (at 1626 cm<sup>−1</sup>) acquired after a resting time, also measured as a function of time (for a preset duration of 750 s) for SMP@Ags passing through the laser focus spot in a water–MB solution. (<b>e</b>) SERS spectra of MB for the corresponding time frames shown in (<b>d</b>).</p>
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<p>(<b>a</b>) Surface plot of MB spectra spanning 750 s ranging from 1200 cm<sup>−1</sup> to 1700 cm<sup>−1</sup> and (<b>b</b>) maximum and average EFs for the SMPs in water–MB solution.</p>
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20 pages, 6824 KiB  
Article
Comparative Validation of Scintillator Materials for X-Ray-Mediated Neuronal Control in the Deep Brain
by Mercedes Hildebrandt, Masanori Koshimizu, Yasuki Asada, Kansai Fukumitsu, Mahito Ohkuma, Na Sang, Takashi Nakano, Toshiaki Kunikata, Kai Okazaki, Noriaki Kawaguchi, Takayuki Yanagida, Linyuan Lian, Jianbing Zhang and Takayuki Yamashita
Int. J. Mol. Sci. 2024, 25(21), 11365; https://doi.org/10.3390/ijms252111365 - 22 Oct 2024
Viewed by 887
Abstract
When exposed to X-rays, scintillators emit visible luminescence. X-ray-mediated optogenetics employs scintillators for remotely activating light-sensitive proteins in biological tissue through X-ray irradiation. This approach offers advantages over traditional optogenetics, allowing for deeper tissue penetration and wireless control. Here, we assessed the short-term [...] Read more.
When exposed to X-rays, scintillators emit visible luminescence. X-ray-mediated optogenetics employs scintillators for remotely activating light-sensitive proteins in biological tissue through X-ray irradiation. This approach offers advantages over traditional optogenetics, allowing for deeper tissue penetration and wireless control. Here, we assessed the short-term safety and efficacy of candidate scintillator materials for neuronal control. Our analyses revealed that lead-free halide scintillators, such as Cs3Cu2I5, exhibited significant cytotoxicity within 24 h and induced neuroinflammatory effects when injected into the mouse brain. In contrast, cerium-doped gadolinium aluminum gallium garnet (Ce:GAGG) nanoparticles showed no detectable cytotoxicity within the same period, and injection into the mouse brain did not lead to observable neuroinflammation over four weeks. Electrophysiological recordings in the cerebral cortex of awake mice showed that X-ray-induced radioluminescence from Ce:GAGG nanoparticles reliably activated 45% of the neuronal population surrounding the implanted particles, a significantly higher activation rate than europium-doped GAGG (Eu:GAGG) microparticles, which activated only 10% of neurons. Furthermore, we established the cell-type specificity of this technique by using Ce:GAGG nanoparticles to selectively stimulate midbrain dopamine neurons. This technique was applied to freely behaving mice, allowing for wireless modulation of place preference behavior mediated by midbrain dopamine neurons. These findings highlight the unique suitability of Ce:GAGG nanoparticles for X-ray-mediated optogenetics. The deep tissue penetration, short-term safety, wireless neuronal control, and cell-type specificity of this system offer exciting possibilities for diverse neuroscience applications and therapeutic interventions. Full article
(This article belongs to the Special Issue Advances in Molecular Physics and Optical Materials)
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<p>Short-term safety assessment of scintillators for potential use in X-ray-mediated optogenetics. (<b>a</b>) Representative images of cultured HEK293 cells incubated for 24 h with various scintillator particles at a concentration of 50 μg/mL. Control cells were not exposed to any scintillator particles. Insets show magnified views of the area indicated by dotted squares. Scale bar = 200 (main image) and 50 μm (insets). (<b>b</b>) Cell viability measured 24 h post-incubation with scintillator particles at 5 μg/mL (left) and 50 μg/mL (right). Values are normalized to the mean of the control group (<span class="html-italic">n</span> = 6 for each). **** <span class="html-italic">p</span> &lt; 0.0001; ns, not significant; Dunnett’s multiple comparison test versus control. (<b>c</b>) Epi-fluorescence images of coronal brain slices showing immunostaining for microglia (Iba1, red) and astrocytes (GFAP, green) at the injection sites of either vehicle (left) or SNPs (right, outlined with a dashed line). We injected both vehicle and SNPs into different hemispheres of the same mouse, with slices collected 4 days (4 d), 1 week (1 w), or 4 weeks (4 w) post-injection. Blue: DAPI. (<b>d</b>) Semi-quantification of Iba1 (left) and GFAP (right) immunoreactivity expressed as the percentage of stained pixels in a 100 μm × 100 μm square near the injection traces (<span class="html-italic">n</span> = 3 for each). ns, not significant; paired <span class="html-italic">t</span>-tests with Bonferroni’s correction for multiple comparisons. Open circles represent individual data points, and yellow lines denote individual mice. Black horizontal lines and error bars indicate mean ± SD. Statistical details are shown in <a href="#app1-ijms-25-11365" class="html-app">Table S1</a>.</p>
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<p>SNPs and their use for X-ray-mediated optogenetics. (<b>a</b>) Left, a scanning electron micrograph of SNPs. Right, size distribution of SNPs measured by dynamic light scattering. Mean = 498 ± 8 nm (<span class="html-italic">n</span> = 3). The black line and shadow indicate mean ± SD. (<b>b</b>) Pulse-height spectra of SNPs synthesized with different Ce concentrations (in mol%). (<b>c</b>) Schematic drawing of electrophysiological recordings underneath an X-ray machine designed for human radiography. Note that the electrodes of the silicon probe face injected SNPs. Insets: Epi-fluorescence images of SNPs in S1 region (left, circled) and silicon probe recording trace posterior to SNPs (right, dashed line). Green: ChRmine-eYFP; Red: DiI; Blue: DAPI. (<b>d</b>) Average AP waveforms during X-irradiation (red) superimposed with average AP waveforms at other timings (black) and their cross-correlation coefficients (blue). Scale bar: 1 ms, 0.5 mV.</p>
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<p>X-ray-mediated optogenetics using SNPs caused excitation of the local neuronal circuit. (<b>a</b>) Raster plots and peri-stimulus time histograms (PSTHs) of two representative neurons excited by X-irradiation (red shadow). Inset: average AP waveforms of these neurons during X-irradiation (red) and other timings (black, superimposed). The cross-correlation coefficient between these waveforms was 0.963 for neuron 1 and 0.950 for neuron 2. Scale bar: 1 ms, 0.5 mV. (<b>b</b>) Top: grand average of Z-scored PSTHs of different conditions (SNPs+ ChRmine+ [orange]: <span class="html-italic">n</span> = 82 neurons from 5 mice; SNPs– ChRmine+ [cyan]: <span class="html-italic">n</span> = 76 neurons from 6 mice; SNPs+ ChRmine– [green]: <span class="html-italic">n</span> = 80 neurons from 2 mice; SNPs– ChRmine– [gray]: <span class="html-italic">n</span> = 129 neurons from 3 mice). Bottom: Z-scored mean AP rate changes induced by X-irradiation. SNPs– ChRmine+, * <span class="html-italic">p</span> = 0.0458; SNPs+ ChRmine–, * <span class="html-italic">p</span> = 0.0169; SNPs– ChRmine–, *** <span class="html-italic">p</span> = 0.0007; Dunn’s post hoc tests vs. SNPs+ ChRmine+ group. (<b>c</b>) Top: proportions of the neurons that were excited (blue), inhibited (magenta), and non-modulated (gray) by X-irradiation. **** <span class="html-italic">p</span> &lt; 0.0001, Chi-square tests vs. SNPs+ ChRmine+ group with Bonferroni’s correction for multiple comparisons. Bottom: grand average Z-scored PSTHs of these neurons in the SNPs+ ChRmine+ group. (<b>d</b>) Pooled data of the proportion of the neurons excited by X-irradiation with varying dose rates (0 mGy/s, <span class="html-italic">n</span> = 5 recordings from 4 mice; 5 mGy/s, <span class="html-italic">n</span> = 3 recordings from 2 mice; 10 mGy/s, <span class="html-italic">n</span> = 5 recordings from 4 mice; 27 mGy/s, <span class="html-italic">n</span> = 7 recordings from 5 mice). ** <span class="html-italic">p</span> = 0.0012, Kruskal–Wallis test. Colored lines and shadows in the PSTHs denote mean ± SEM. Open circles represent individual data points. Black horizontal bars and error bars indicate mean ± SD. Statistical details are shown in <a href="#app1-ijms-25-11365" class="html-app">Table S1</a>.</p>
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<p>X-ray-mediated optogenetics using Eu:GAGG particles did not induce discernible neuronal dynamics. (<b>a</b>) Left, grand average of Z-scored AP rate of all neurons of test group (Eu:GAGG+ ChRmine+, magenta) and two control groups (Eu:GAGG– ChRmine+, green; Eu:GAGG–ChRmine–, gray). Right, Z-scored AP rate changes induced by X-irradiation. ns, not significant, Dunn’s post hoc tests. (<b>b</b>) Proportions of the neurons that were excited (blue), inhibited (magenta), and non-modulated (gray) by X-irradiation. ns, not significant, Chi-square tests with Bonferroni’s correction for multiple comparisons. Colored lines and shadows in the PSTHs denote mean ± SEM. Open circles represent individual data points. Black horizontal bars and error bars indicate mean ± SD. Statistical details are shown in <a href="#app1-ijms-25-11365" class="html-app">Table S1</a>.</p>
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<p>Deep brain stimulation of VTA-DA neurons via X-ray-mediated optogenetics. (<b>a</b>) Schematic of the experiment. Insets: epi-fluorescence images of SNPs in the VTA (left, dashed white circle) and silicon probe trace posterior to SNPs (right, dashed white line). The electrodes on the silicon probe faced the SNP-injection site. Green: ChRmine-eYFP; Red: DiI; Blue: DAPI. Scale bars: 500 µm. (<b>b</b>) Raster plots and PSTHs of two representative neurons excited by X-irradiation (red shadow). Inset: average AP waveform of these neurons during X-irradiation (red) and other timings (black, superimposed). The cross-correlation coefficient between these waveforms was 0.998 for neuron 1 and 0.966 for neuron 2. Scale bar: 1 ms, 0.5 mV. (<b>c</b>) Grand average of Z-scored AP rate of all neurons of test group (SNPs+ ChRmine+, orange) and two control groups (SNPs + ChRmine – [hrGFP+], green; SNPs – ChRmine-, gray). (<b>d</b>) Z-scored AP rate changes induced by X-irradiation. ** <span class="html-italic">p</span> = 0.0070, **** <span class="html-italic">p</span> &lt; 0.0001, Dunn’s post hoc tests vs. SNPs+ ChRmine+ group. (<b>e</b>) Proportions of the neurons that were excited (blue), inhibited (magenta), and non-modulated (gray) by X-irradiation. *** <span class="html-italic">p</span> = 0.000225, **** <span class="html-italic">p</span> &lt; 0.0001, Chi-square tests with Bonferroni’s correction for multiple comparisons. (<b>f</b>) Grand average Z-scored PSTHs of these neurons in the SNPs+ ChRmine+ group. Colored lines and shadows in the PSTHs denote mean ± SEM. Open circles represent individual data points. Black horizontal bars and error bars indicate mean ± SD. Statistical details are shown in <a href="#app1-ijms-25-11365" class="html-app">Table S1</a>.</p>
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<p>X-ray-mediated optogenetics using SNPs applied to behavioral tests with freely moving mice. (<b>a</b>) Schematic of the experiment. Inset: epi-fluorescence image of a coronal section containing the left VTA with SNPs (dashed outline) injected into two locations. Green: ChRmine-eYFP; blue: DAPI. (<b>b</b>) Schematic of CPP tests. (<b>c</b>) Representative tracking data (left) and corresponding heat maps (right) for ChRmine− (top) and hrGFP− (bottom) expressing mice. Dotted rectangles show the area used for analysis. (<b>d</b>) Relative time spent in the X-irradiated compartment of ChRmine (top, 7 mice) and hrGFP (bottom, 7 mice) mice in the pre-test (day 0) compared to that in the post-test (day 5). * <span class="html-italic">p</span> = 0.0353; ns, not significant; paired <span class="html-italic">t</span>-test. (<b>e</b>) Quantification of initial preference for the X-irradiated compartment. ns, not significant; unpaired <span class="html-italic">t</span>-test. (<b>f</b>) Quantification of CPP scores. ** <span class="html-italic">p</span> = 0.0041; Mann–Whitney <span class="html-italic">U</span> test. Open circles represent individual data points, and the lines connecting the open circles denote individual mice. Black horizontal bars and error bars indicate mean ± SD. Statistical details are shown in <a href="#app1-ijms-25-11365" class="html-app">Table S1</a>.</p>
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14 pages, 3923 KiB  
Article
Antimicrobial Activity of Amino-Modified Cellulose Nanofibrils Decorated with Silver Nanoparticles
by Vesna Lazić, Jovan M. Nedeljković and Vanja Kokol
J. Funct. Biomater. 2024, 15(10), 304; https://doi.org/10.3390/jfb15100304 - 13 Oct 2024
Viewed by 1087
Abstract
Silver nanoparticles (Ag NPs) conjugated with amino-functionalized cellulose nanofibrils (NH2−CNFs) were in situ-prepared by reducing silver ions with free amino groups from NH2−CNFs. The spectroscopy and transmission electron microscopy measurements confirmed the presence of non-agglomerated nanometer-in-size Ag NPs within [...] Read more.
Silver nanoparticles (Ag NPs) conjugated with amino-functionalized cellulose nanofibrils (NH2−CNFs) were in situ-prepared by reducing silver ions with free amino groups from NH2−CNFs. The spectroscopy and transmission electron microscopy measurements confirmed the presence of non-agglomerated nanometer-in-size Ag NPs within micrometer-large NH2−CNFs of high (20 wt.-%) content. Although the consumption of amino groups during the formation of Ag NPs lowers the ζ-potential and surface charge of prepared inorganic–organic hybrids (from +31.3 to +19.9 mV and from 2.4 to 1.0 mmol/g at pH 7, respectively), their values are sufficiently positive to ensure electrostatic interaction with negatively charged cell walls of pathogens in acidic and slightly (up to pH ~8.5) alkaline solutions. The antimicrobial activity of hybrid microparticles against various pathogens (Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus, and Candida albicans) is comparable with pristine NH2−CNFs. However, a long-timescale use of hybrids ensures the slow and controlled release of Ag+ ions to surrounding media (less than 1.0 wt.-% for one month). Full article
(This article belongs to the Special Issue Nanostructured Materials/Biomaterials for Healthcare Applications)
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<p>(<b>A</b>) Kubelka-Munk transformations of reflection data of NH<sub>2</sub>−CNFs and Ag/NH<sub>2</sub>−CNFs. (<b>B</b>) TG curves, measured in the air at a heating rate of 10 °C/min, of CNFs, NH<sub>2</sub>−CNFs, and Ag/NH<sub>2</sub>−CNFs.</p>
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<p>The XRD pattern of the Ag/NH<sub>2</sub>−CNFs hybrid; inset: the XRD patterns of CNFs and NH<sub>2</sub>−CNFs.</p>
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<p>Low-magnification TEM images of Ag/NH<sub>2</sub>−CNFs composite (<b>A</b>,<b>B</b>) and corresponding SAED pattern (<b>C</b>) as well as EDX spectrum (<b>D</b>). High-magnification TEM image of typical Ag NP attached to NH<sub>2</sub>−CNFs support (<b>E</b>).</p>
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<p>Potentiometric titration curves of native CNFs, NH<sub>2</sub>-CNF, and Ag/NH<sub>2</sub>-CNF with corresponding charges suspended in water; concentration: 0.001 wt.%. Inset: the titration curves (forth and back) of pure HMDA.</p>
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<p>(<b>A</b>) ζ-potentials and (<b>B</b>) average hydrodynamic size distribution of native CNFs, NH<sub>2</sub>-CNF, and Ag/NH<sub>2</sub>-CNF in water and water containing different volume percent of ethanol or acetone at pH 7, analyzed by DLS; concentration: 0.001 wt.%.</p>
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<p>Synthetic pathway for preparation of inorganic–organic hybrid consisting of Ag NPs and amino-functionalized CNFs.</p>
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19 pages, 5961 KiB  
Article
NiO Nano- and Microparticles Prepared by Solvothermal Method—Amazing Catalysts for CO2 Methanation
by Arkadii Bikbashev, Tomáš Stryšovský, Martina Kajabová, Zuzana Kovářová, Robert Prucek, Aleš Panáček, Josef Kašlík, Tamás Fodor, Csaba Cserháti, Zoltán Erdélyi and Libor Kvítek
Molecules 2024, 29(20), 4838; https://doi.org/10.3390/molecules29204838 - 12 Oct 2024
Viewed by 1164
Abstract
Nickel oxide (NiO) is one of the most popular hydrogenation catalysts. In heterogeneous catalysis, nickel oxide is used, for example, as a suitable methanation catalyst in the Fischer–Tropsch reaction not only for CO hydrogenation but also in the modified Fischer–Tropsch reaction with CO [...] Read more.
Nickel oxide (NiO) is one of the most popular hydrogenation catalysts. In heterogeneous catalysis, nickel oxide is used, for example, as a suitable methanation catalyst in the Fischer–Tropsch reaction not only for CO hydrogenation but also in the modified Fischer–Tropsch reaction with CO2. However, CH4 selectivity and CO2 conversion strongly depend on NiO micro- (MPs) and nanoparticles’ (NPs) shape, size, and surface area. In this study, the synthesis of NiO micro- and nanoparticles was conducted using the simple solvothermal method. Different morphologies (microspheres, sheet clusters, hexagonal microparticles, and nanodiscs) were prepared using this method with different solvents and stabilizers. The prepared catalysts were tested in the hydrogenation of CO2 in a gas phase with excellent conversion values and high selectivity to produce CH4. The best results were obtained with the NiO with disc or sphere morphology, which produced methane with selectivity at a level near 100% and conversion close to 90%. Full article
(This article belongs to the Special Issue Research on Heterogeneous Catalysis—2nd Edition)
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<p>Test experiment: conversion CO<sub>2</sub> (<b>a</b>) and selectivity CH<sub>4</sub> (<b>b</b>) for NiOhx1 sample at temperature ramp from 250 up to 500 °C.</p>
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<p>TG/DSC graphs of nickel hydroxide (pre-NiOnd, before calcination).</p>
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<p>SEM images of NiO: NiOms1 (<b>a</b>), NiOms2 (<b>b</b>), NiOms3 (<b>c</b>), NiOshc (<b>d</b>), NiOhx1 (<b>e</b>), NiOhx2 (<b>f</b>), NiOhx+m (<b>g</b>), and NiO nd (<b>h</b>).</p>
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<p>SEM images of NiO: NiOms1 (<b>a</b>), NiOms2 (<b>b</b>), NiOms3 (<b>c</b>), NiOshc (<b>d</b>), NiOhx1 (<b>e</b>), NiOhx2 (<b>f</b>), NiOhx+m (<b>g</b>), and NiO nd (<b>h</b>).</p>
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<p>SEM images of NiO samples after catalysis: NiOms2* (<b>a</b>), NiOms3* (<b>b</b>), NiOshc* (<b>c</b>), NiOhx2* (<b>d</b>), and NiOnd* (<b>e</b>). * Marking of the spent catalyst</p>
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<p>XPS (nickel 2p spectra) diagram of pre-catalysis samples: NiOhx1 (red), NiOms1 (green), and NiOhx+m (blue).</p>
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<p>XPS (survey spectra) diagram of pre-catalysis samples, NiOms1 (black), NiOhx1 (blue), and NiOhx+m (light blue), and post-catalysis samples, NiOms1* (red), NiOhx1* (green), and NiOhx+m* (light green).</p>
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<p>Temperature-programmed reduction (TPR-H<sub>2</sub>) spectrum measured with NiOhx2 sample (T = 25–600 °C).</p>
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<p>Temperature-programmed desorption (TPD-CO<sub>2</sub>) spectrum measured with NiOhx2 sample (T = 25–600 °C).</p>
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<p>Graphs of conversion CO<sub>2</sub> (<math display="inline"><semantics> <mrow> <msub> <mrow> <mi mathvariant="normal">x</mi> </mrow> <mrow> <msub> <mrow> <mi mathvariant="normal">C</mi> <mi mathvariant="normal">O</mi> </mrow> <mrow> <mn>2</mn> </mrow> </msub> </mrow> </msub> </mrow> </semantics></math>), selectivity CH<sub>4</sub> (<math display="inline"><semantics> <mrow> <msub> <mrow> <mi mathvariant="normal">s</mi> </mrow> <mrow> <msub> <mrow> <mi mathvariant="normal">C</mi> <mi mathvariant="normal">H</mi> </mrow> <mrow> <mn>4</mn> </mrow> </msub> </mrow> </msub> </mrow> </semantics></math>), reaction yield CH<sub>4</sub> (<math display="inline"><semantics> <mrow> <msub> <mrow> <mi mathvariant="sans-serif">η</mi> </mrow> <mrow> <msub> <mrow> <mi mathvariant="normal">C</mi> <mi mathvariant="normal">H</mi> </mrow> <mrow> <mn>4</mn> </mrow> </msub> </mrow> </msub> </mrow> </semantics></math>), space–time yield (<math display="inline"><semantics> <mrow> <msub> <mrow> <mi mathvariant="normal">S</mi> <mi mathvariant="normal">T</mi> <mi mathvariant="normal">Y</mi> </mrow> <mrow> <msub> <mrow> <mi mathvariant="normal">C</mi> <mi mathvariant="normal">H</mi> </mrow> <mrow> <mn>4</mn> </mrow> </msub> </mrow> </msub> </mrow> </semantics></math>), and selectivity CO (s<sub>co</sub>) of NiOhx1 (green), NiOhx2 (yellow), NiOhx+m (red), and NiOnd (grey).</p>
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<p>Graphs of conversion CO<sub>2</sub> (<math display="inline"><semantics> <mrow> <msub> <mrow> <mi mathvariant="normal">x</mi> </mrow> <mrow> <msub> <mrow> <mi mathvariant="normal">C</mi> <mi mathvariant="normal">O</mi> </mrow> <mrow> <mn>2</mn> </mrow> </msub> </mrow> </msub> </mrow> </semantics></math>), selectivity CH<sub>4</sub> (<math display="inline"><semantics> <mrow> <msub> <mrow> <mi mathvariant="normal">s</mi> </mrow> <mrow> <msub> <mrow> <mi mathvariant="normal">C</mi> <mi mathvariant="normal">H</mi> </mrow> <mrow> <mn>4</mn> </mrow> </msub> </mrow> </msub> </mrow> </semantics></math>), reaction yield CH<sub>4</sub> (<math display="inline"><semantics> <mrow> <msub> <mrow> <mi mathvariant="sans-serif">η</mi> </mrow> <mrow> <msub> <mrow> <mi mathvariant="normal">C</mi> <mi mathvariant="normal">H</mi> </mrow> <mrow> <mn>4</mn> </mrow> </msub> </mrow> </msub> </mrow> </semantics></math>), space–time yield (<math display="inline"><semantics> <mrow> <msub> <mrow> <mi mathvariant="normal">S</mi> <mi mathvariant="normal">T</mi> <mi mathvariant="normal">Y</mi> </mrow> <mrow> <msub> <mrow> <mi mathvariant="normal">C</mi> <mi mathvariant="normal">H</mi> </mrow> <mrow> <mn>4</mn> </mrow> </msub> </mrow> </msub> </mrow> </semantics></math>), and selectivity CO (s<sub>CO</sub>) of NiOms1 (purple), NiOms2 (light green), NiOms3 (red), and NiOshc (blue).</p>
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44 pages, 3893 KiB  
Review
Advancements in Ocular Therapy: A Review of Emerging Drug Delivery Approaches and Pharmaceutical Technologies
by Bhupendra Raj Giri, Deeksha Jakka, Michael A. Sandoval, Vineet R. Kulkarni and Quanying Bao
Pharmaceutics 2024, 16(10), 1325; https://doi.org/10.3390/pharmaceutics16101325 - 12 Oct 2024
Viewed by 2822
Abstract
Eye disorders affect a substantial portion of the global population, yet the availability of efficacious ophthalmic drug products remains limited. This can be partly ascribed to a number of factors: (1) inadequate understanding of physiological barriers, treatment strategies, drug and polymer properties, and [...] Read more.
Eye disorders affect a substantial portion of the global population, yet the availability of efficacious ophthalmic drug products remains limited. This can be partly ascribed to a number of factors: (1) inadequate understanding of physiological barriers, treatment strategies, drug and polymer properties, and delivery systems; (2) challenges in effectively delivering drugs to the anterior and posterior segments of the eye due to anatomical and physiological constraints; and (3) manufacturing and regulatory hurdles in ocular drug product development. The present review discusses innovative ocular delivery and treatments, encompassing implants, liposomes, nanoparticles, nanomicelles, microparticles, iontophoresis, in situ gels, contact lenses, microneedles, hydrogels, bispecific antibodies, and gene delivery strategies. Furthermore, this review also introduces advanced manufacturing technologies such as 3D printing and hot-melt extrusion (HME), aimed at improving bioavailability, reducing therapeutic dosages and side effects, facilitating the design of personalized ophthalmic dosage forms, as well as enhancing patient compliance. This comprehensive review lastly offers insights into digital healthcare, market trends, and industry and regulatory perspectives pertaining to ocular product development. Full article
(This article belongs to the Special Issue Controlled-Release Systems for Ophthalmic Applications)
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<p>A summary of the key barriers and their properties impeding ocular drug delivery.</p>
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<p>An illustration depicting the interaction of cationic liposomes on the cornea with the negatively charged mucin layer. Created with <a href="http://BioRender.com" target="_blank">BioRender.com</a> (accessed on 3 August 2024).</p>
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<p>Ophthalmic drug delivery using in situ gelling polymer systems. Created with <a href="http://BioRender.com" target="_blank">BioRender.com</a> (accessed on 3 August 2024).</p>
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<p>Different types of microneedles for ocular drug delivery. Created with <a href="http://BioRender.com" target="_blank">BioRender.com</a> (accessed on 3 August 2024).</p>
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<p>A schematic representation of subretinal gene therapy. Created with <a href="http://BioRender.com" target="_blank">BioRender.com</a> (accessed on 3 August 2024).</p>
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<p>Schematic diagram of different types of 3D printing (3DP) technologies: (<b>A</b>) fused deposition modeling (FDM), (<b>B</b>) semi-solid extrusion (SSE), (<b>C</b>) stereolithography (SLA), and (<b>D</b>) digital light processing (DLP). Created with <a href="http://BioRender.com" target="_blank">BioRender.com</a> (accessed on 27 August 2024).</p>
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<p>Various ocular dosage forms fabricated using different 3D printing technologies.</p>
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<p>A schematic representation of critical hot-melt extrusion steps and ocular dosage forms manufactured with HME technology.</p>
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26 pages, 3897 KiB  
Review
A Comprehensive Review of Xanthan Gum-Based Oral Drug Delivery Systems
by Buddhadev Layek
Int. J. Mol. Sci. 2024, 25(18), 10143; https://doi.org/10.3390/ijms251810143 - 21 Sep 2024
Cited by 1 | Viewed by 1974
Abstract
Xanthan gum (XG) is an exopolysaccharide synthesized by the aerobic fermentation of simple sugars using Xanthomonas bacteria. It comprises a cellulosic backbone with a trisaccharide side chain connected to alternative glucose residues in the main backbone through α (1→3) linkage. XG dissolves readily [...] Read more.
Xanthan gum (XG) is an exopolysaccharide synthesized by the aerobic fermentation of simple sugars using Xanthomonas bacteria. It comprises a cellulosic backbone with a trisaccharide side chain connected to alternative glucose residues in the main backbone through α (1→3) linkage. XG dissolves readily in cold and hot water to produce a viscous solution that behaves like a pseudoplastic fluid. It shows excellent resistance to enzymatic degradation and great stability throughout a broad temperature, pH, or salt concentration range. Additionally, XG is nontoxic, biocompatible, and biodegradable, making it a suitable carrier for drug delivery. Furthermore, the carboxylic functions of pyruvate and glucuronic acid offer a considerable opportunity for chemical modification to meet the desired criteria for a specific application. Therefore, XG or its derivatives in conjunction with other polymers have frequently been studied as matrices for tablets, nanoparticles, microparticles, and hydrogels. This review primarily focuses on the applications of XG in various oral delivery systems over the past decade, including sustained-release formulations, gastroretentive dosage forms, and colon-targeted drug delivery. Source, production methods, and physicochemical properties relevant to drug delivery applications of XG have also been discussed. Full article
(This article belongs to the Collection Feature Papers in Molecular Pharmacology)
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<p>Chemical structure of xanthan gum.</p>
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<p>Ordered structures proposed from computer-modelling of X-ray fiber diffraction data for xanthan: (<b>a</b>) single helix (<b>b</b>) antiparallel double helix. Both structures have 5-fold symmetry and a pitch of 4.7 nm, derived directly from the experimental diffraction patterns. Reprinted with permission from Ref. [<a href="#B3-ijms-25-10143" class="html-bibr">3</a>]. Copyright 2019, Elsevier.</p>
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<p>Preclinical efficacy of XGD6 formulation (acetylated hydrogel particles of CEXG: CMXG at 1:2 ratio). Key: diabetic control (♦, received only distilled water), negative control (■, received formulation without drug), pure repaglinide suspension (▲, 4 mg/kg body weight), and XGD6 formulation (●, repaglinide-loaded XGD6 hydrogel particles containing an equivalent amount of repaglinide). Reprinted with permission from Ref. [<a href="#B44-ijms-25-10143" class="html-bibr">44</a>]. Copyright 2022, Elsevier.</p>
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<p>Photographs taken of G10% (galactomannan 10%), GX7:3 (physical mixtures of galactomannan and xanthan gum at 7:3 ratio), and X10% (xanthan gum 10%) systems after swelling for 2, 6, 12 and 24 h in the dissolution test. Reprinted with permission from Ref. [<a href="#B50-ijms-25-10143" class="html-bibr">50</a>]. Copyright 2012, Elsevier.</p>
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<p>Plasma concentration vs. time curves of pure curcumin and curcumin-loaded PAAm-g-XG nanoparticles (CN20 NPs). Reprinted with permission from Ref. [<a href="#B91-ijms-25-10143" class="html-bibr">91</a>]. Copyright 2016, Elsevier.</p>
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<p>(<b>a</b>) The percentage of cell viability of different concentrations of XG/PVI hydrogel sample after 24 h incubation with VERO cell lines and (<b>b</b>) microscope examination of VERO cells that were incubated 24 h with different concentrations of hydrogel samples and compared with control cells (untreated cells). Reprinted with permission from Ref. [<a href="#B112-ijms-25-10143" class="html-bibr">112</a>]. Copyright 2019, Elsevier.</p>
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25 pages, 7423 KiB  
Review
Lubricant Strategies in Osteoarthritis Treatment: Transitioning from Natural Lubricants to Drug Delivery Particles with Lubricant Properties
by Agnese Fragassi, Antonietta Greco and Roberto Palomba
J. Xenobiot. 2024, 14(3), 1268-1292; https://doi.org/10.3390/jox14030072 - 19 Sep 2024
Cited by 1 | Viewed by 1428
Abstract
Osteoarthritis (OA) is a debilitating joint disease characterized by cartilage degradation, leading to pain and functional impairment. A key contributor to OA progression is the decline in cartilage lubrication. In physiological conditions, synovial fluid (SF) macromolecules like hyaluronic acid (HA), phospholipids, and lubricin [...] Read more.
Osteoarthritis (OA) is a debilitating joint disease characterized by cartilage degradation, leading to pain and functional impairment. A key contributor to OA progression is the decline in cartilage lubrication. In physiological conditions, synovial fluid (SF) macromolecules like hyaluronic acid (HA), phospholipids, and lubricin play a crucial role in the boundary lubrication of articular cartilage. In early OA, cartilage damage triggers inflammation, altering SF composition and compromising the lubrication layer. This increases friction between mating interfaces, worsening cartilage degradation and local inflammation. Therefore, early-stage restoration of lubrication (by injecting in the joint different classes of compounds and formulations) could alleviate, and potentially reverse, OA progression. In the light of this, a broad variety of lubricants have been investigated for their ability to reduce friction in OA joints and promote cartilage repair in clinical and preclinical studies. This review examines recent advancements in lubricant-based therapy for OA, focusing on natural, bioinspired, and alternative products. Starting from the currently applied therapy, mainly based on natural lubricants as HA, we will present their modified versions, either in hydrogel form or with specific biomimetic moieties with the aim of reducing their clearance from the joint and of enhancing their lubricating properties. Finally, the most advanced and recent formulation, represented by alternative strategies, will be proposed. Particular emphasis will be placed on those ones involving new types of hydrogels, microparticles, nanoparticles, and liposomes, which are currently under investigation in preclinical studies. The potential application of particles and liposomes could foster the transition from natural lubricants to Drug Delivery Systems (DDSs) with lubricant features; transition which could provide more complete OA treatments, by simultaneously providing lubrication replacement and sustained release of different payloads and active agents directly at the joint level. Within each category, we will examine relevant preclinical studies, highlighting challenges and future prospects. Full article
(This article belongs to the Section Nanotoxicology and Nanopharmacology)
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<p>Schematic representation of boundary lubrication in articular cartilage. On the left, a coronal section of knee joint: under load application the pressure increases and the outer surfaces of opposing articular cartilage make molecular contact. On the right, the proposed structure of the lubrication layer on the cartilage surface, showing phosphocholine groups of lipids at the interface to reduce friction through the hydration mechanism.</p>
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<p>Schematic of a coronal section of knee joint indicating on the left the main anatomical components, and on the right the main pathological effects of OA.</p>
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