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Search Results (296)

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Keywords = rapid infrared scans

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13 pages, 3260 KiB  
Article
Influence of Rapid Heat Treatment on the Photocatalytic Activity and Stability of Barium Titanates Against a Broad Range of Pollutants
by Mahsa Abedi, Haythem S. Basheer, Laura Lakatos, Ákos Kukovecz, Zoltán Kónya, Tamás Gyulavári and Zsolt Pap
Molecules 2024, 29(22), 5350; https://doi.org/10.3390/molecules29225350 - 14 Nov 2024
Viewed by 208
Abstract
Barium titanate photocatalysts were synthesized via a sol–gel method involving a unique, cost-effective calcination technique that includes rapid heating and short exposure. The samples were characterized by X-ray diffractometry, scanning electron microscopy, diffuse reflectance spectroscopy, photoluminescence spectroscopy, infrared spectroscopy, and nitrogen adsorption–desorption measurements. [...] Read more.
Barium titanate photocatalysts were synthesized via a sol–gel method involving a unique, cost-effective calcination technique that includes rapid heating and short exposure. The samples were characterized by X-ray diffractometry, scanning electron microscopy, diffuse reflectance spectroscopy, photoluminescence spectroscopy, infrared spectroscopy, and nitrogen adsorption–desorption measurements. The photooxidation activity and stability of the samples were evaluated by the degradation of phenol, oxalic acid, and chlorophenol. Their photoreduction activity was also investigated by the photocatalytic conversion of CO2 to CO. In both cases, UV irradiation was applied to activate the catalysts. As references, commercially available cubic and tetragonal barium titanates were used, with the addition of benchmark P25 TiO2 in some cases. Increasing the calcination temperature resulted in increased primary crystallite sizes, decreased specific surface areas, and slightly redshifted band gaps. On the one hand, the overall photooxidation activity of the samples for pollutant degradation was rather low, possibly due to their unfavorable valence band maximum position. On the other hand, our samples displayed significantly superior photoreduction activity, surpassing that of all the references, including P25 TiO2. The high photoactivity was mainly attributed to the specific surface areas that changed per the efficiency of the samples. Last, the cost comparison calculations showed that applying our calcination technique is 29.5% more cost-efficient than conventional calcination, and the same amount of energy is sufficient for preparing even a 1.4 times higher amount of barium titanite. Full article
(This article belongs to the Section Photochemistry)
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Graphical abstract

Graphical abstract
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<p>XRD patterns of BTO_Ref and BTO_RHSE samples calcined at different temperatures (<b>a</b>) and zoomed-in section between 44.5 and 46 2θ° demonstrating cubic and tetragonal structures (<b>b</b>).</p>
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<p>SEM micrographs of commercial BTO and BTO_RHSE photocatalysts calcined at various temperatures.</p>
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<p>DR absorbance (<b>a</b>) and first-order derivative spectra (<b>b</b>) of the BTO_Ref and BTO_RHSE samples.</p>
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<p>Photoluminescence spectrum for the BTO_Ref and BTO_RHSE samples.</p>
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<p>IR spectra of the BTO_Ref and BTO_RHSE samples.</p>
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<p>Degradation curves for (<b>a</b>) phenol, (<b>b</b>) chlorophenol, and (<b>c</b>) oxalic acid.</p>
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<p>Photocatalytic conversion of CO<sub>2</sub> using BTO_Ref, BTO_RHSE, and P25 TiO<sub>2</sub> samples.</p>
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19 pages, 7438 KiB  
Article
Engineering pH and Temperature-Triggered Drug Release with Metal-Organic Frameworks and Fatty Acids
by Wanying Wei and Ping Lu
Molecules 2024, 29(22), 5291; https://doi.org/10.3390/molecules29225291 - 8 Nov 2024
Viewed by 370
Abstract
This study reports the successful synthesis of core-shell microparticles utilizing coaxial electrospray techniques, with zeolitic imidazolate framework-8 (ZIF-8) encapsulating rhodamine B (RhB) in the core and a phase change material (PCM) shell composed of a eutectic mixture of lauric acid (LA) and stearic [...] Read more.
This study reports the successful synthesis of core-shell microparticles utilizing coaxial electrospray techniques, with zeolitic imidazolate framework-8 (ZIF-8) encapsulating rhodamine B (RhB) in the core and a phase change material (PCM) shell composed of a eutectic mixture of lauric acid (LA) and stearic acid (SA). ZIF-8 is well-recognized for its pH-responsive degradation and biocompatibility, making it an ideal candidate for targeted drug delivery. The LA-SA PCM mixture, with a melting point near physiological temperature (39 °C), enables temperature-triggered drug release, enhancing therapeutic precision. The structural properties of the microparticles were extensively characterized through scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). Drug release studies revealed a dual-stimuli response, where the release of RhB was significantly influenced by both temperature and pH. Under mildly acidic conditions (pH 4.0) at 40 °C, a rapid and complete release of RhB was observed within 120 h, while at 37 °C, the release rate was notably slower. Specifically, the release at 40 °C was 79% higher than at 37 °C, confirming the temperature sensitivity of the system. Moreover, at physiological pH (7.4), minimal drug release occurred, demonstrating the system’s potential for minimizing premature drug release under neutral conditions. This dual-stimuli approach holds promise for improving therapeutic outcomes in cancer treatment by enabling precise control over drug release in response to both pH and localized hyperthermia, reducing off-target effects and improving patient compliance. Full article
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Figure 1
<p>Schematic representation of the ZIF-8 synthesis process.</p>
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<p>SEM images of ZIF-8 at various magnifications. (<b>A</b>) 10,000×, (<b>B</b>) 20,000×, (<b>C</b>) 30,000×, (<b>D</b>) 50,000×, and (<b>E</b>) 100,000×. These images highlight the rhombic dodecahedral and cubic morphologies of the particles. (<b>F</b>) Diameter distribution of ZIF-8 particles.</p>
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<p>SEM micrographs and particle size distribution of RhB@ZIF-8 microparticles. Images (<b>A</b>) through (<b>E</b>) display the morphology of RhB@ZIF-8 at varying magnifications: (<b>A</b>) 10,000×, (<b>B</b>) 20,000×, (<b>C</b>) 30,000×, (<b>D</b>) 50,000×, and (<b>E</b>) 100,000×. The micrographs reveal uniform rhombic dodecahedron-shaped microparticles with smooth surfaces, typical of ZIF-8 structures. Plot (<b>F</b>) shows the corresponding particle diameter distribution of RhB@ZIF-8, demonstrating a relatively narrow size distribution with an average diameter centered around 200 nm.</p>
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<p>SEM images of PLA microparticles at various concentrations of PLA in dichloromethane (DCM) under 20,000× magnification: (<b>A</b>) 1 wt% PLA in DCM, showing shriveled particles with prominent surface pores; (<b>B</b>) 2 wt% PLA in DCM, displaying fuller particles with fewer wrinkles and visible pores; (<b>C</b>) 3 wt% PLA in DCM, showing nearly spherical particles with minimal wrinkles and fewer pores compared to lower concentrations. The increase in PLA concentration results in more uniform and spherical microparticle morphology.</p>
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<p>SEM images of RhB@PCM microparticles at varying magnifications in DCM: (<b>A</b>) 5000× magnification, showing the overall surface morphology with irregular and wrinkled structures; (<b>B</b>) 10,000× magnification, providing a closer view of the individual microparticles, revealing shrinkage and deformation of the particle surfaces; and (<b>C</b>) 20,000× magnification, displaying detailed surface texture and porosity, highlighting the structural inconsistencies and the non-uniformity of the particle surfaces.</p>
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<p>SEM images of RhB@ZIF-8@PCM microparticles at varying magnifications: (<b>A</b>,<b>B</b>) show the surface morphology of RhB@ZIF-8@PCM microparticles at 5000× magnification, highlighting their clustered structure and partial aggregation; (<b>C</b>–<b>F</b>) show the same particles at 10,000× magnification, revealing more detailed structural features, including the presence of fine fibers and surface irregularities. (<b>F</b>) includes the diameter distribution plot, indicating a relatively narrow size range with a peak centered around 892 nm.</p>
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<p>XRD patterns illustrating the crystallographic structures of the various components. (<b>A</b>) shows the diffraction patterns of RhB, ZIF-8, and RhB@ZIF-8, highlighting the characteristic peaks of each material. (<b>B</b>) presents the XRD patterns of LASA, RhB@ZIF-8, and RhB@ZIF-8@PCM.</p>
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<p>FTIR spectra of LA, SA, ZIF-8, RhB@ZIF-8, and RhB@ZIF-8@PCM.</p>
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<p>Cumulative RhB release profiles under different pH and temperature conditions. (<b>A</b>) RhB release from RhB@ZIF-8 at pH 4.0, 7.4, and 10.0 at 37 °C, showing rapid release at pH 4.0 and slower, sustained release at neutral and basic pH values. (<b>B</b>) RhB release from RhB@ZIF-8@PCM at pH 4.0 under 37 °C and 40 °C, demonstrating a significantly higher release rate at the elevated temperature. (<b>C</b>) RhB release from RhB@ZIF-8@PCM at pH 7.4 under 37 °C and 40 °C, with a noticeable increase in release at 40 °C compared to 37 °C. (<b>D</b>) RhB release from RhB@ZIF-8@PCM at pH 10.0 under 37 °C and 40 °C, showing minimal release at both temperatures, indicating stability under basic conditions.</p>
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<p>Cumulative RhB release profiles under different conditions. (<b>A</b>) Release of RhB from RhB@PCM at pH 7.4 and temperatures of 37 °C and 40 °C, showing a significantly higher release rate at 40 °C compared to 37 °C. (<b>B</b>) Comparison of RhB release from RhB@PCM and RhB@ZIF-8@PCM at 40 °C and pH 7.4, highlighting the faster release from RhB@PCM due to the absence of the ZIF-8 core, while RhB@ZIF-8@PCM shows a more controlled and sustained release due to the ZIF-8 framework.</p>
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<p>Schematic representation of the stepwise synthesis process for RhB@ZIF-8.</p>
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<p>Schematic illustration of the coaxial electrospraying experimental setup for the production of core-shell microparticles (RhB@ZIF-8@PCM).</p>
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18 pages, 3296 KiB  
Article
Improving the Gelation Properties of Pea Protein Isolates Using Psyllium Husk Powder: Insight into the Underlying Mechanism
by Qiongling Chen, Jiewen Guan, Zhengli Wang, Yu Wang, Xiaowen Wang and Zhenjia Chen
Foods 2024, 13(21), 3413; https://doi.org/10.3390/foods13213413 - 26 Oct 2024
Viewed by 811
Abstract
The industrial application of pea protein is limited due to its poor gelation properties. This study aimed to evaluate the effects of psyllium husk powder (PHP) on improving the rheological, textural, and structural properties of heat-induced pea protein isolate (PPI) gel. Scanning electron [...] Read more.
The industrial application of pea protein is limited due to its poor gelation properties. This study aimed to evaluate the effects of psyllium husk powder (PHP) on improving the rheological, textural, and structural properties of heat-induced pea protein isolate (PPI) gel. Scanning electron microscopy (SEM), intermolecular forces analysis, the quantification of the surface hydrophobicity and free amino groups, and Fourier transform infrared spectroscopy (FTIR) were conducted to reveal the inner structures of PPI-PHP composite gels, conformational changes, and molecular interactions during gelation, thereby clarifying the underlying mechanism. The results showed that moderate levels of PHP (0.5–2.0%) improved the textural properties, water holding capacity (WHC), whiteness, and viscoelasticity of PPI gel in a dose-dependent manner, with the WHC (92.60 ± 1.01%) and hardness (1.19 ± 0.02 N) peaking at 2.0%. PHP significantly increased surface hydrophobicity and enhanced hydrophobic interactions, hydrogen bonding, and electrostatic interactions in PPI-PHP composite gels. Moreover, the electrostatic repulsion between anionic PHP and negatively charged PPI in a neutral environment prevented the rapid and random aggregation of proteins, thereby promoting the formation of a well-organized gel network with more β-sheet structures. However, the self-aggregation of excessive PHP (3.0%) weakened molecular interactions and disrupted the continuity of protein networks, slightly reducing the gel strength. Overall, PHP emerged as an effective natural gel enhancer for the production of pea protein gel products. This study provides technical support for the development of innovative plant protein-based foods with strong gel properties and enriched dietary fiber content. Full article
(This article belongs to the Section Food Physics and (Bio)Chemistry)
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<p>Schematic diagram of molecular interactions between protein and polysaccharide.</p>
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<p>Optical (<b>A</b>) and scanning electron microscopy (<b>B</b>) images of heat-induced PPI-PHP composite gels.</p>
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<p>Changes of the storage modulus (G′), loss modulus (G″), and loss angle (tan δ) in temperature sweep for the dispersions of PPI-PHP mixtures.</p>
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<p>The surface hydrophobicity (<b>A</b>) and the content of free amino groups (<b>B</b>) of heat-induced PPI-PHP composite gels. Different letters at the top of the columns represent significant differences (<span class="html-italic">p</span> &lt; 0.05) in varying amounts of PHP.</p>
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<p>Molecular interaction forces of heat-induced PPI-PHP composite gels. Different letters at the top of the columns represent significant differences (<span class="html-italic">p</span> &lt; 0.05) in varying amounts of PHP.</p>
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<p>Sodium dodecyl sulfate polyacrylamide gel electrophoresis (SDS-PAGE) pattern of heat-induced PPI-PHP composite gels. CV stands for con-vicilin, V for vicilin, L<sub>α</sub> for legumin acidic subunit, and L<sub>β</sub> for legumin basic subunit.</p>
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<p>Fourier-transform infrared spectra of PPI−PHP composite gels in the range of 400−4000 cm<sup>−1</sup> (<b>A</b>) and the relative proportion of secondary structures (<b>B</b>). Different letters in the columns represent significant differences (<span class="html-italic">p</span> &lt; 0.05) in varying amounts of PHP.</p>
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<p>A schematic diagram of the influence mechanism of PHP on the heat-induced PPI gelation.</p>
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19 pages, 3381 KiB  
Article
Isolation and Identification of Four Strains of Bacteria with Potential to Biodegrade Polyethylene and Polypropylene from Mangrove
by Xilin Fang, Zeming Cai, Xiaocui Wang, Ziyu Liu, Yongkang Lin, Minqian Li, Han Gong and Muting Yan
Microorganisms 2024, 12(10), 2005; https://doi.org/10.3390/microorganisms12102005 - 2 Oct 2024
Viewed by 646
Abstract
With the rapid growth of global plastic production, the degradation of microplastics (MPs) has received widespread attention, and the search for efficient biodegradation pathways has become a hot topic. The aim of this study was to screen mangrove sediment and surface water for [...] Read more.
With the rapid growth of global plastic production, the degradation of microplastics (MPs) has received widespread attention, and the search for efficient biodegradation pathways has become a hot topic. The aim of this study was to screen mangrove sediment and surface water for bacteria capable of degrading polyethylene (PE) and polypropylene (PP) MPs. In this study, two strains of PE-degrading bacteria and two strains of PP-degrading candidate bacteria were obtained from mangrove, named Pseudomonas sp. strain GIA7, Bacillus cereus strain GIA17, Acinetobacter sp. strain GIB8, and Bacillus cereus strain GIB10. The results showed that the degradation rate of the bacteria increased gradually with the increase in degradation time for 60 days. Most of the MP-degrading bacteria had higher degradation rates in the presence of weak acid. The appropriate addition of Mg2+ and K+ was favorable to improve the degradation rate of MPs. Interestingly, high salt concentration inhibited the biodegradation of MPs. Results of scanning electron microscopy (SEM), atomic force microscopy (AFM), and Fourier-transform infrared spectroscopy (FTIR) indicated the degradation and surface changes of PP and PE MPs caused by candidate bacteria, which may depend on the biodegradation-related enzymes laccase and lipase. Our results indicated that these four bacterial strains may contribute to the biodegradation of MPs in the mangrove environment. Full article
(This article belongs to the Section Environmental Microbiology)
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Figure 1
<p>Results of physiological and biochemical experiments on potentially efficient microplastic-degrading bacteria.</p>
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<p>Phylogenetic tree indicating the relationship between the 16S rRNA gene sequences of (<b>A</b>) <span class="html-italic">Pseudomonas</span> sp. strain GIA7 and Acinetobacter sp. strain GIB8, (<b>B</b>) Bacillus cereus strain GIA17 and Bacillus cereus strain GIB10. The red triangle signs are the four strains of potentially efficient degrading bacteria.</p>
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<p>Weight loss rate of MPs after degradation by potentially efficient microplastic-degrading bacteria (<b>A</b>) at different times, (<b>C</b>) in different pH environments, (<b>E</b>) under different inorganic salt ions, (<b>G</b>) at different salt concentrations. Plot of ΔOD<sub>600</sub> of potentially efficient microplastic-degrading bacteria (<b>B</b>) at different times, (<b>D</b>) in different pH environments, (<b>F</b>) under different inorganic salt ions, (<b>H</b>) at different salt concentrations.</p>
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<p>Laccase and lipase activities of the strains.</p>
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<p>Surface microscopic characterization of PE and PP microplastics before and after degradation by scanning electron microscopy. Untreated PE microplastics (<b>A</b>) and untreated PP microplastics (<b>B</b>). The surface change of PE MPs after 60 days of degradation by GIA7 (<b>C</b>). The surface change of PE MPs after 60 days of degradation by GIA17 (<b>E</b>). The surface change of PP MPs after 60 days of degradation by GIB8 (<b>D</b>). The surface change of PP MPs after 60 days of degradation by GIB10 (<b>F</b>).</p>
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<p>Bacterial attachment of PE and PP MPs observed using SEM after 60 days of incubation. PE MPs after degradation by GIA7 (<b>A</b>) and GIA17 (<b>B</b>). PP MPs after degradation by GIB8 (<b>C</b>) and GIB10 (<b>D</b>).</p>
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<p>Surface microcharacterization of PE and PP microplastics before and after degradation by atomic force microscopy. PE MPs (<b>A</b>) and PP MPs (<b>D</b>) before degradation. PE MPs after degradation by GIA7 (<b>B</b>) and GIA17 (<b>C</b>). PP MPs after degradation by GIB8 (<b>E</b>) and GIB10 (<b>F</b>).</p>
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<p>Chemical modification of PE (<b>A</b>) and PP (<b>B</b>) treated by microplastic-degrading bacteria was analyzed by Fourier infrared spectroscopy.</p>
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14 pages, 2548 KiB  
Article
Fabrication of a Heptapeptide-Modified Poly(glycidyl Methac-Rylate) Nanosphere for Oriented Antibody Immobilization and Immunoassay
by Xiaoxing Gong, Jie Zhang, Liyan Zhu, Shu Bai, Linling Yu and Yan Sun
Molecules 2024, 29(19), 4635; https://doi.org/10.3390/molecules29194635 - 29 Sep 2024
Viewed by 629
Abstract
Oriented antibody immobilization has been widely employed in immunoassays and immunodiagnoses due to its efficacy in identifying target antigens. Herein, a heptapeptide ligand, HWRGWVC (HC7), was coupled to poly(glycidyl methacrylate) (PGMA) nanospheres (PGMA-HC7). The antibody immobilization behavior and antigen recognition performance were investigated [...] Read more.
Oriented antibody immobilization has been widely employed in immunoassays and immunodiagnoses due to its efficacy in identifying target antigens. Herein, a heptapeptide ligand, HWRGWVC (HC7), was coupled to poly(glycidyl methacrylate) (PGMA) nanospheres (PGMA-HC7). The antibody immobilization behavior and antigen recognition performance were investigated and compared with those on PGMA nanospheres by nonspecific adsorption and covalent coupling via carbodiimide chemistry. The antibodies tested included bovine, rabbit, and human immunoglobulin G (IgG), while the antigens included horseradish peroxidase (HRP) and β-2-Microglobulin (β2-MG). The nanospheres were characterized using zeta potential and particle size analyzers, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, and reversed-phase chromatography, proving each synthesis step was succeeded. Isothermal titration calorimetry assay demonstrated the strong affinity interaction between IgG and PGMA-HC7. Notably, PGMA-HC7 achieved rapid and extremely high IgG adsorption capacity (~3 mg/mg) within 5 min via a specific recognition via HC7 without nonspecific interactions. Moreover, the activities of immobilized anti-HRP and anti-β2-MG antibodies obtained via affinity binding were 1.5-fold and 2-fold higher than those of their covalent coupling counterparts. Further, the oriented-immobilized anti-β2-MG antibody on PGMA-HC7 exhibited excellent performance in antigen recognition with a linear detection range of 0–5.3 μg/mL, proving its great potential in immunoassay applications. Full article
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<p>Schematic diagram of (<b>a</b>) heptapeptide HWRGWVC and IgG, (<b>b</b>) specific identification on the Fc region of IgG by HWRGWVC, and (<b>c</b>) synthesis routes of PGMA nanospheres for IgG immobilization. (I) PGMA-HC7 nanospheres for specific binding via HWRGWVC; (II) PGMA-NH<sub>2</sub> nanospheres for EDC-based covalent immobilization of IgG.</p>
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<p>The SEM and TEM images of PGMA-HC7 nanospheres. (<b>a</b>) SEM at magnifications of 500 nm and (<b>b</b>) TEM at magnifications of 200 nm. Size distributions (<b>c</b>) and Zeta potentials (<b>d</b>) of different nanospheres.</p>
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<p>ITC isotherms of IgG binding to (<b>a</b>) PGMA-HC7 and (<b>b</b>) PGMA-OH nanospheres.</p>
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<p>(<b>a</b>) Uptake kinetic curve of 2 mg/mL bovine IgG on PGMA-HC7 nanospheres in physiological buffer at 19,000 rpm. (<b>b</b>) Adsorption isotherms of bovine IgG on different PGMA-based nanospheres. (<b>c</b>) Adsorption density of bovine IgG on the PGMA-based nanospheres at varying initial concentrations.</p>
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<p>Antibody immobilizations onto different PGMA-modified nanospheres. (<b>a</b>) Capacity and activity of immobilized anti-HRP IgG. (<b>b</b>) Capacity and activity of immobilized anti-β2-MG IgG. (<b>c</b>) Schematic drawing of the covalent coupling and orientated immobilization of IgG. (<b>d</b>) Detection range of PGMA-HC7-anti-β2-MG-IgG system.</p>
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17 pages, 8175 KiB  
Article
Utilization of Banana Juice Biomass Waste to Activate CuO/NiO Composites for Electrocatalytic Oxidation of Urea in Alkaline Media
by Irum Naz, Aneela Tahira, Arfana Begum Mallah, Ihsan Ali Mahar, Asma Hayat, Aqeel Ahmed Shah, Elmuez Dawi, Atef AbdElKader, Lama Saleem, Rafat M. Ibrahim and Zafar Hussain Ibupoto
Catalysts 2024, 14(10), 669; https://doi.org/10.3390/catal14100669 - 27 Sep 2024
Viewed by 1024
Abstract
The hydrothermal synthesis of CuO/NiO composites was conducted using banana fruit biomass waste. In this study, X-ray powder diffraction, scanning electron microscopy, and Fourier transform infrared spectroscopy were used to investigate the crystalline properties, shape structure, and functional group characterization of CuO/NiO composites. [...] Read more.
The hydrothermal synthesis of CuO/NiO composites was conducted using banana fruit biomass waste. In this study, X-ray powder diffraction, scanning electron microscopy, and Fourier transform infrared spectroscopy were used to investigate the crystalline properties, shape structure, and functional group characterization of CuO/NiO composites. The typical morphology of the prepared materials consisted of irregular nanoparticles arranged into clusters of less than 200 nanometers in size. In spite of this, the CuO/NiO composites showed monoclinic CuO and cubic NiO phases and were therefore successfully synthesized. It was observed that rotten banana fruit juice had a significant impact on the particle size and crystal quality of CuO/NiO composites. This was due to the presence of capping, reducing, and stabilizing agents in banana fruit juice. Under alkaline conditions, the CuO/NiO composites were found to be highly electro catalytically active toward the oxidation of urea. Sample 2, which was prepared by adding 1.2 g of CuO decorated with NiO, showed a linear increase in urea detection ranging from 0.1 mM to 17 mM, with a limit of detection of 0.004 mM. Furthermore, sample 2 of the CuO/NiO composite demonstrated exceptional stability, selectivity, and reproducibility. Consequently, sample 2 of CuO/NiO could effectively detect urea in spinach, lotus root, milk, and curd. The improved performance of sample 2 of the CuO/NiO composite can be attributed to its favorable surface properties, which contain enriched active sites and a rapid charge transfer rate. Full article
(This article belongs to the Special Issue Study on Electrocatalytic Activity of Metal Oxides)
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Figure 1
<p>FTIR spectrum of composite materials made with varying concentrations of fruit banana juice, CuO/NiO sample 1, and CuO/NiO sample 2 compared with pure NiO and pure CuO.</p>
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<p>XRD patterns of diffraction for pure NiO and pure CuO nanostructured materials (<b>a</b>,<b>b</b>) without banana juice and (<b>c</b>,<b>d</b>), with 15 mL and 25 mL of banana fruit extract (sample 1 and sample 2), respectively. Blue circles are indicated reflections peaks of pure NiO and red circles are defined the pure CuO in sample 1 and sample 2.</p>
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<p>Images from SEM of pure NiO, pure CuO nano-structured materials made (<b>a</b>–<b>d</b>) without banana fruit juice with different levels of magnification and with (<b>e</b>,<b>f</b>) 15 mL and (<b>g</b>,<b>h</b>) 25 mL of banana fruit extract (sample 1 and sample 2), respectively.</p>
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<p>(<b>a</b>) EDS spectrum of sample 1 of NiO/CuO composite synthesized with 15 mL of banana fruit juice, (<b>b</b>–<b>e</b>) corresponding elemental mapping of O, Ni, and Cu.</p>
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<p>(<b>a</b>) EDS spectrum of sample 2 of NiO/CuO composite synthesized with 25 mL of banana fruit juice, (<b>b</b>–<b>e</b>) corresponding elemental mapping of O, Ni, and Cu, and (<b>f</b>) SEM image of sample 2 after stability test during electrochemical measurements.</p>
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<p>(<b>a</b>) Bare glassy carbon electrode (BGCE) CV curves of pure NiO, pure CuO nanostructured materials, and CuO/NiO composite materials utilizing various volumes of banana fruit juice, including 15 and 25 mL and sample 1 and sample 2 at 50 mV/s in 0.1 M of NaOH with and without urea. (<b>b</b>) CV curves were measured at 50 mV/s in 0.1 mM of urea for pure NiO, pure CuO, sample 1, and sample 2. (<b>c</b>) Pure NiO, pure CuO, and sample 2 are shown in 0.1 mM of urea separately. (<b>d</b>) Sample 2 CV curves measured in 0.1 mM of urea at various scan rates. (<b>e</b>) Anodic and cathodic peak currents are linearly plotted simultaneously versus the scan rate’s square root.</p>
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<p>(<b>a</b>) CV curves of sample 2 at 50 mV/sec for different concentrations of urea made in NaOH (0.1 M). (<b>b</b>) Anodic peak current plotted linearly vs. several urea concentrations. (<b>c</b>) Chronoamperometric behavior of sample 2 to various urea concentrations. (<b>d</b>) Anodic peak current plotted linearly against various concentrations of urea.</p>
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<p>(<b>a</b>) LSV curves of sample 2 at 50 mV/s in 0.1 M NaOH; (<b>b</b>) the oxidation peak current plotted linearly against various concentrations of urea; (<b>c</b>) the reproducibility of various modified electrodes of sample 2 (0.5 mM urea); (<b>d</b>) the reproducibility bar graph of sample 2.</p>
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<p>(<b>a</b>) CV curves at 50 mV/s showing stability of sample 2 (0.5 mM urea); (<b>b</b>) variation in peak current through bar graph of each electrode. (<b>c</b>) Selectivity measured utilizing CV curves at 50 mV/s of sample 2 in alternative environment that interferes. (<b>d</b>) EIS Nyquist plots of pure NiO, pure CuO, sample 1, and sample 2 in 0.5 mM of urea.</p>
Full article ">Figure 9 Cont.
<p>(<b>a</b>) CV curves at 50 mV/s showing stability of sample 2 (0.5 mM urea); (<b>b</b>) variation in peak current through bar graph of each electrode. (<b>c</b>) Selectivity measured utilizing CV curves at 50 mV/s of sample 2 in alternative environment that interferes. (<b>d</b>) EIS Nyquist plots of pure NiO, pure CuO, sample 1, and sample 2 in 0.5 mM of urea.</p>
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<p>(<b>a</b>–<b>d</b>) CV curves of non-faradaic for pure NiO, pure CuO, sample 1, and sample 2 at different scan rates in urea (0.5 mM); (<b>e</b>) linear plot for the quantification of ECSA showing the difference between the current density on the anodic and cathodic sides against the scan rate.</p>
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<p>Generalizing demonstration of non-enzymatic urea sensor using CuO/NiO composites.</p>
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12 pages, 6807 KiB  
Article
Green Synthesis of Iron-Based Nanoparticles Using Pomegranate Leaf Extracts: Characterization, Biomolecules and Indole Removal
by Huifang Sun, Yanjun Liu, Yifan Zhou, Zuliang Chen and Jianfeng Li
Water 2024, 16(18), 2665; https://doi.org/10.3390/w16182665 - 19 Sep 2024
Viewed by 849
Abstract
This study investigates the synthesis of iron-based nanoparticles (Fe NPs) using pomegranate leaf extracts and their application in removing indole, a persistent organic pollutant commonly found in wastewater. The physicochemical properties of the synthesized Fe NPs and the active biomolecules in the pomegranate [...] Read more.
This study investigates the synthesis of iron-based nanoparticles (Fe NPs) using pomegranate leaf extracts and their application in removing indole, a persistent organic pollutant commonly found in wastewater. The physicochemical properties of the synthesized Fe NPs and the active biomolecules in the pomegranate leaf extracts were comprehensively characterized. Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM) analyses revealed that the Fe NPs exhibited quasi-spherical shapes, with sizes ranging from 75 to 105 nm. Energy-Dispersive X-ray Spectroscopy (EDS) confirmed a homogeneous distribution of elements, including C, O, Fe, and S, on the nanoparticle surfaces, with weight percentages of 43.59%, 42.95%, 12.58%, and 0.88%, respectively. Fourier-transform infrared spectroscopy (FTIR) identified key functional groups like −OH, −COOH, and −C=O, which are essential for the capping and stabilization of the nanoparticles. Biomolecules such as ellagic acid (C14H6O8) and gallic acid (C7H6O5) functioned as reducing agents, improving nanoparticle dispersion and preventing aggregation. The synthesized Fe NPs quickly achieved 45.5% removal of indole within just 20 min and maintained a stable removal efficiency of approximately 51.4% after 90 min. This performance was attributed to the synergetic interaction between the biomolecules and the nanoparticles, with the monolayer adsorption of indole molecules on the Fe NP surfaces likely setting an upper limit on the maximum achievable removal efficiency. It appears from this study that pomegranate leaf extracts can be effectively utilized to synthesize Fe NPs as a novel and eco-friendly approach, demonstrating promising potential for the rapid removal of indole from aqueous solutions. Full article
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<p>Morphological and elemental characterization of Fe NPs: (<b>a</b>) SEM image of surface morphology; (<b>b</b>) TEM image; (<b>c</b>) EDS spectra for elemental composition; (<b>d</b>) EDS map for elemental distribution.</p>
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<p>Detailed XPS analysis of Fe NPs: (<b>a</b>) full survey spectrum; (<b>b</b>) high-resolution spectra of Fe 2p; (<b>c</b>) spectra of C 1s; (<b>d</b>) spectra of O 1s.</p>
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<p>FTIR spectra of <span class="html-italic">pomegranate</span> leaf extracts before and after reacting with Fe<sup>2+</sup> solution.</p>
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<p>GC-MS analysis of active biomolecules in Fe NPs.</p>
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<p>LC-MS analysis of active biomolecules of Fe NPs: (<b>a</b>) normal-phase chromatography; (<b>b</b>) reverse-phase chromatography.</p>
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<p>Possible formation mechanisms of Fe NPs.</p>
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<p>(<b>a</b>) Indole efficiency removal by Fe NPs and <span class="html-italic">pomegranate</span> leaf extracts; GC-MS chromatogram of indole removal by Fe NPs (<b>b</b>) and <span class="html-italic">pomegranate</span> leaf extracts (<b>c</b>).</p>
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<p>Adsorption kinetics curve: (<b>a</b>) pseudo first-order kinetics model; (<b>b</b>) pseudo second-order kinetics model.</p>
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<p>(<b>a</b>) Adsorption isotherms at different temperatures, (<b>b</b>) Ce/qe–Ce relationship points and linear fitting.</p>
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22 pages, 5375 KiB  
Article
Formulation and Development of Nanofiber-Based Ophthalmic Insert for the Treatment of Bacterial Conjunctivitis
by Eszter Farkas, Houssam Abboud, Nándor Nagy, Bálint Hofmeister, Eszter Ostorházi, Bence Tóth, Balázs Pinke, László Mészáros, Romána Zelkó and Adrienn Kazsoki
Int. J. Mol. Sci. 2024, 25(17), 9228; https://doi.org/10.3390/ijms25179228 - 25 Aug 2024
Viewed by 855
Abstract
A novel ophthalmic delivery system utilizing levofloxacin-loaded, preservative-free, nanofiber-based inserts was investigated. Polyvinyl alcohol (PVA) and Poloxamer 407 (Polox)were employed as matrix materials, while hydroxypropyl-beta-cyclodextrin (HP-β-CD) was a solubilizer. The formulations were prepared via electrospinning and characterized for fiber morphology, drug dissolution, cytotoxicity, [...] Read more.
A novel ophthalmic delivery system utilizing levofloxacin-loaded, preservative-free, nanofiber-based inserts was investigated. Polyvinyl alcohol (PVA) and Poloxamer 407 (Polox)were employed as matrix materials, while hydroxypropyl-beta-cyclodextrin (HP-β-CD) was a solubilizer. The formulations were prepared via electrospinning and characterized for fiber morphology, drug dissolution, cytotoxicity, and antimicrobial activity. Scanning electron microscopy confirmed uniform fibrous structures. Fourier Transform Infrared spectroscopy and X-ray diffraction analyses demonstrated the amorphous state of levofloxacin within the fibers. In vitro dissolution studies revealed a rapid (within 2 min) and complete drug release, with higher HP-β-CD levels slightly delaying the release. Cytotoxicity tests showed increased HP-β-CD concentrations induced irritation, that was mitigated by sodium hyaluronate. The antimicrobial efficacy of the nanofibers was comparable to conventional eye drops, with lower minimum inhibitory concentrations for most tested strains. The nanofibrous formulation prepared from a PVA–Polox-based viscous solution of the drug:CD 1:1 mol ratio, containing 0.4% (w/w) sodium hyaluronate) was identified as a particularly promising alternative formulation due to its rapid and complete dissolution, good biocompatibility, and effective antimicrobial properties. Its gelling properties indicate that the residence time on the eye surface can be increased, potentially reducing discomfort and enhancing therapeutic outcomes. The nanofibrous formulations enhanced antimicrobial efficacy, providing a preservative-free alternative that minimizes the potential eye irritation that might occur because of the preservative agent and reduces the administrated dose frequency by extending the drug’s retention time on the eye’s surface. Subsequently, it improves patients’ adherence, which would reflect positively on the bioavailability. The levofloxacin-HP-β-CD nanofibers demonstrate promise as an alternative to traditional eye drops, offering advantages in solubility, stability, and patient compliance for ocular infection treatment. Full article
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<p>Schematic representation of the project objectives.</p>
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<p>Scanning electron microscopy (SEM) images of the polyvinyl alcohol (PVA): poloxamer 407 (Polox) (8:2 mass ratio) based, electrospun samples of total polymer concentrations 10% (<span class="html-italic">w</span>/<span class="html-italic">w</span>) (<b>A</b>), 12% (<span class="html-italic">w</span>/<span class="html-italic">w</span>) (<b>B</b>), and 14% (<span class="html-italic">w</span>/<span class="html-italic">w</span>) (<b>C</b>), respectively (Magnification: 5000×).</p>
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<p>Scanning electron microscopic (SEM) images of the electrospun samples that used F4 (<b>A</b>), F5 (<b>B</b>), F6 (<b>C</b>), F7 (<b>D</b>), F8 (<b>E</b>), and F9 (<b>F</b>) precursor solutions for the fiber formation process (Magnification: 5000×).</p>
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<p>FTIR spectra of the components of the nanofibers and the physical mixture (<b>A</b>) and the prepared different compositions of nanofibrous samples and the levofloxacin (LEVO) (<b>B</b>) between 4000–500 cm<sup>−1</sup>.</p>
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<p>Power X-ray patterns of levofloxacin (LEVO), physical mixture, and drug-loaded nanofibers of LEVO–hydroxypropyl-beta-cyclodextrin (LEVO:CD) 1:1 (<b>A</b>) and 1:1.5 (n:n) (<b>B</b>), respectively.</p>
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<p>In vitro dissolution analysis of levofloxacin (LEVO)-loaded fibrous samples was carried out at a phosphate buffer of pH = 7.4, where the curves depict the average and deviation of the three parallel measurements.</p>
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<p>Images of the chorioallantois membrane (CAM) after placing different levofloxacin (LEVO)-loaded nanofibers of levofloxacin–hydroxypropyl-beta-cyclodextrin (LEVO:CD) 1:1 (F6 and F8) and 1:1.5 (n:n) (F7 and F9) and the negative and positive control (phosphate buffer salina (pH = 7.4) and 2M NaOH, respectively). The sodium hyaluronate concentration was 0.2% (<span class="html-italic">w</span>/<span class="html-italic">w</span>) for F6 and F7, and 0.4% (<span class="html-italic">w</span>/<span class="html-italic">w</span>) for F8 and F9 precursor solutions. The blue dashed circle indicates the position of the nanofibrous sample placed on the CAM.</p>
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<p>UV-Vis spectra of the unfiltered (black line) and filtered (red line) precursor solution between 200–800 nm.</p>
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<p>Time–kill plots demonstrating the effects of starting inoculum on the activities of different levofloxacin (LEVO)-containing formulations against <span class="html-italic">Escherichia coli</span> (<span class="html-italic">E. coli</span>), <span class="html-italic">Staphylococcus aureus</span> (<span class="html-italic">S. aureus</span>), and <span class="html-italic">Pseudomonas aeruginosa</span> (<span class="html-italic">P. aeruginosa</span>).</p>
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16 pages, 1756 KiB  
Article
Handheld Near-Infrared Spectroscopy for Undried Forage Quality Estimation
by William Yamada, Jerry Cherney, Debbie Cherney, Troy Runge and Matthew Digman
Sensors 2024, 24(16), 5136; https://doi.org/10.3390/s24165136 - 8 Aug 2024
Viewed by 3812
Abstract
This study investigates the efficacy of handheld Near-Infrared Spectroscopy (NIRS) devices for in-field estimation of forage quality using undried samples. The objective is to assess the precision and accuracy of multiple handheld NIRS instruments—NeoSpectra, TrinamiX, and AgroCares—when evaluating key forage quality metrics such [...] Read more.
This study investigates the efficacy of handheld Near-Infrared Spectroscopy (NIRS) devices for in-field estimation of forage quality using undried samples. The objective is to assess the precision and accuracy of multiple handheld NIRS instruments—NeoSpectra, TrinamiX, and AgroCares—when evaluating key forage quality metrics such as Crude Protein (CP), Neutral Detergent Fiber (aNDF), Acid Detergent Fiber (ADF), Acid Detergent Lignin (ADL), in vitro Total Digestibility (IVTD)and Neutral Detergent Fiber Digestibility (NDFD). Samples were collected from silage bunkers across 111 farms in New York State and scanned using different methods (static, moving, and turntable). The results demonstrate that dynamic scanning patterns (moving and turntable) enhance the predictive accuracy of the models compared to static scans. Fiber constituents (ADF, aNDF) and Crude Protein (CP) show higher robustness and minimal impact from water interference, maintaining similar R2 values as dried samples. Conversely, IVTD, NDFD, and ADL are adversely affected by water content, resulting in lower R2 values. This study underscores the importance of understanding the water effects on undried forage, as water‘s high absorption bands at 1400 and 1900 nm introduce significant spectral interference. Further investigation into the PLSR loading factors is necessary to mitigate these effects. The findings suggest that, while handheld NIRS devices hold promise for rapid, on-site forage quality assessment, careful consideration of scanning methodology is crucial for accurate prediction models. This research contributes valuable insights for optimizing the use of portable NIRS technology in forage analysis, enhancing feed utilization efficiency, and supporting sustainable dairy farming practices. Full article
(This article belongs to the Special Issue Spectral Detection Technology, Sensors and Instruments, 2nd Edition)
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<p>Comparative analysis of forage sample spectra: This graph illustrates the mean spectral signatures of forage samples (<span class="html-italic">n</span> = 600) as measured by three different scanners—TrinamiX (red line—static scan), AgroCares (green line—static scan; blue line—moving scan), and NEOSpectra (yellow—static scan; cyan—moving scan; magenta—turntable scan)—utilizing varying methods. Each line represents the average log(1/R) value across a range of wavelengths from 1400 to 2600 nm. The hue of each line represents the range between the maximum and minimum measured for each instrument.</p>
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<p>RMSE vs. latent variables for each variable. This figure shows the root mean squared error (RMSE) values for different numbers of latent variables across various instruments and target variables. The RMSE values for both calibration and cross-validation (CV) are plotted for each instrument, differentiated by color (purple—AgroCares Static, orange—Agrocares Moving, blue—NEOSpectra Static, green—NEOSpectra Moving, red—NEOSpectra Turntable, brown—Trinamix Static) and line style (continuous—calibration, dashed—CV).</p>
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<p>Comparative evaluation of three handheld spectrometers and methods used to predict nutritional content in feed samples. The different colors and shapes represent readings from moving, static, or turntable methods of using the AgroCares, NEO Spectra, and TrinamiX instruments. Each dot represents the pair of reference data and the prediction using the calibrated PLSR model from the validation set (<span class="html-italic">n</span> = 60). The regression lines for each method showcase the accuracy and precision in predicting the content of Crude Protein (CP), Neutral Detergent Fiber (aNDF), Acid Detergent Fiber (ADF), Acid Detergent Lignin (ADL), Neutral Detergent Fiber Digestibility (NDFD), and in vitro Total Digestibility (IVTD). The dashed black line represents a 1:1 agreement between the reference and predicted values.</p>
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<p>The chart presents the normalized distribution of prediction errors on the validation set for six forage quality variables—CP, NDFD, aNDF, ADL, IVTD, and ADF—obtained using different spectral scanning instruments and methods. Each boxplot shows the median, quartiles, and outliers for the prediction error standard deviation (SD) of each method.</p>
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<p>Undried data <math display="inline"><semantics> <msup> <mi>R</mi> <mn>2</mn> </msup> </semantics></math> comparison with Aurora [<a href="#B3-sensors-24-05136" class="html-bibr">3</a>], calibrated for haylage, corn silage, and Total Mixed Ration, and NEOSpectra [<a href="#B7-sensors-24-05136" class="html-bibr">7</a>] calibrated for grass, alfalfa, and mixed silage forages. Both references were sampled using moving scans. The dots represents the metrics obtained by the references, and the stars represents the metrics obtained by our best model.</p>
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<p>Comparison of <math display="inline"><semantics> <msup> <mi>R</mi> <mn>2</mn> </msup> </semantics></math> values from models calibrated on dried samples (literature) versus our model calibrated on undried samples. Tellspec and ASD QualitySpec [<a href="#B2-sensors-24-05136" class="html-bibr">2</a>] were calibrated for grass. NEOSpectra [<a href="#B4-sensors-24-05136" class="html-bibr">4</a>] was calibrated for grass, alfalfa, and mixed silage forages. Nano and MicroPHAZIR [<a href="#B6-sensors-24-05136" class="html-bibr">6</a>] were calibrated for grass forages. NIR-S-G1, SCiO, and Aurora [<a href="#B8-sensors-24-05136" class="html-bibr">8</a>] were calibrated for alfalfa and grass forages. The dots represent the metrics obtained from the references, and the stars represent the metrics obtained by our best model.</p>
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<p>Loading values of the first latent variable of the spectrum (first derivative). Instruments are divided by color (AgroCares—blue, NEOSpectra—red, and Trinamix—green). The scan modes are divided by the line style (continuous—static, dashed—moving, and dotted—turntable). The vertical lines are the water absorption bands. Very small absorption bands (1778, 2208, and 2384 nm) are in green. The large absorption band (1460 nm) is illustrated in cyan. The very large absorption band (1904 nm) is shown in purple.</p>
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<p>Loading values of the second latent variable of the spectrum (first derivative). Instruments are divided by color (AgroCares—blue, NEOSpectra—red, and Trinamix—green). The scan modes are divided by the line style (continuous—static, dashed—moving, and dotted—turntable). The vertical lines are the water absorption bands. Very small absorption bands (1778, 2208, and 2384 nm) are in green. The large absorption band (1460 nm) is illustrated in cyan. The very large absorption band (1904 nm) is in purple.</p>
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16 pages, 14862 KiB  
Article
Spectrophotometric-Based Sensor for the Detection of Multiple Fertilizer Solutions
by Jianian Li, Zhuoyuan Wu, Jiawen Liang, Yuan Gao and Chenglin Wang
Agriculture 2024, 14(8), 1291; https://doi.org/10.3390/agriculture14081291 - 5 Aug 2024
Viewed by 977
Abstract
The online detection of fertilizer solution information is a crucial link in the implementation of intelligent and precise variable fertilization techniques. However, achieving simultaneous rapid online detection of multiple fertilizer components is still challenging. Therefore, a rapid detection method based on spectrophotometry for [...] Read more.
The online detection of fertilizer solution information is a crucial link in the implementation of intelligent and precise variable fertilization techniques. However, achieving simultaneous rapid online detection of multiple fertilizer components is still challenging. Therefore, a rapid detection method based on spectrophotometry for qualitative and quantitative identification of four fertilizers (typical N, P, and K fertilizers: KNO3, (NH4)2SO4, KH2PO4, and K2SO4) was proposed in this work. Full-scan absorption spectra of fertilizer solutions at varying concentrations were obtained using a UV–visible/near-infrared spectrophotometer. By assessing the linear fit between fertilizer concentration and absorbance at each wavelength within the characteristic band, the characteristic wavelengths for KNO3, (NH4)2SO4, KH2PO4, and K2SO4 were identified as 214 nm, 410 nm, 712 nm, and 1708 nm, respectively. The identification method of fertilizer type and the prediction model of concentration were constructed based on characteristic wavelength and the Lambert–Beer law. Based on the above analysis, a four-channel photoelectric sensor was designed with four LEDs emitting wavelengths closely matched to characteristic wavelengths for fertilizer detection. A detection strategy of “qualitative analysis followed by quantitative detection” was proposed to realize the online detection of four fertilizer types and their concentrations. Evaluation of the sensor’s performance showed its high stability, with an accuracy of 81.5% in recognizing fertilizer types. Furthermore, the relative error of the sensor detection was substantially less than ±15% for the fertilizer concentrations not exceeding 80 mg/L. These results confirm the capability of the sensor to meet the practical requirements for online detection of four fertilizer types and concentrations in the field of agricultural engineering. Full article
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<p>Development strategy for fertilizer detection sensors: (<b>a</b>) The acquisition of UV–vis/NIR absorption spectra of four fertilizer solutions: (<b>i</b>) KNO<sub>3</sub>, (<b>ii</b>) (NH<sub>4</sub>)<sub>2</sub>SO<sub>4</sub>, (<b>iii</b>) KH<sub>2</sub>PO<sub>4</sub>, and (iv) K<sub>2</sub>SO<sub>4</sub>. (<b>b</b>) Determination of characteristic wavelengths and construction of quantitative models. (<b>c</b>) Sensor structure and amplifier circuit design. (<b>d</b>) The detection strategy of qualitative analysis followed by quantitative assessment.</p>
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<p>Fertilizer solution detection sensor. (<b>a</b>) Internal structure of the sensor; (<b>b</b>) external structure of the sensor; (<b>c</b>) physical drawing of the sensor; and (<b>d</b>) fertilizer solution identification and concentration detection strategy.</p>
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<p>Absorption spectra of four fertilizer solutions after Savitzky–Golay smoothing treatment. (<b>a</b>) NO<sub>3</sub><sup>−</sup> solution, (<b>b</b>) NH<sub>4</sub><sup>+</sup> solution, (<b>c</b>) H<sub>2</sub>PO<sub>4</sub><sup>−</sup> solution, and (<b>d</b>) K<sup>+</sup> solution.</p>
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<p>Absorption spectra of four nutrient ions at different concentrations in characteristic bands: (<b>a</b>) NO<sub>3</sub><sup>−</sup>, (<b>b</b>) NH<sub>4</sub><sup>+</sup>, (<b>c</b>) H<sub>2</sub>PO<sub>4</sub><sup>−</sup>, and (<b>d</b>) K<sup>+</sup>. Linear relationships between the ion concentration and the absorbance at characteristic wavelength: (<b>e</b>) NO<sub>3</sub><sup>−</sup>, (<b>f</b>) NH<sub>4</sub><sup>+</sup>, (<b>g</b>) H<sub>2</sub>PO<sub>4</sub><sup>−</sup>, and (<b>h</b>) K<sup>+</sup>.</p>
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<p>Absorbance change trends in four fertilizer solutions at four characteristic wavelengths: (<b>a</b>) NO<sub>3</sub><sup>−</sup>, (<b>b</b>) NH<sub>4</sub><sup>+</sup>, (<b>c</b>) H<sub>2</sub>PO<sub>4</sub><sup>−</sup>, and (<b>d</b>) K<sup>+</sup>.</p>
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<p>Stability test results of the fertilizer solution sensor: (<b>a</b>) the stability of the LED light source characterized by the output voltage of the Photodetector 1; (<b>b</b>) transmission voltage value; and (<b>c</b>) ambient light voltage value.</p>
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<p>The trend in absorbance variation at four detection wavelengths (256, 405, 700, and 1650 nm) of the sensor for 10 concentrations of fertilizer solutions: (<b>a</b>) NO<sub>3</sub><sup>−</sup>, (<b>b</b>) NH<sub>4</sub><sup>+</sup>, (<b>c</b>) H<sub>2</sub>PO<sub>4</sub><sup>−</sup>, and (<b>d</b>) K<sup>+</sup>.</p>
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<p>Confusion matrix charts of the classification results for four fertilizer solutions (KNO<sub>3</sub>, (NH<sub>4</sub>)<sub>2</sub>SO<sub>4</sub>, KH<sub>2</sub>PO<sub>4</sub>, and K<sub>2</sub>SO<sub>4</sub>) obtained by the developed sensor.</p>
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<p>Detection errors of the sensor on the concentration of four fertilizer solutions.</p>
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17 pages, 2205 KiB  
Article
Variation Analysis of Starch Properties in Tartary Buckwheat and Construction of Near-Infrared Models for Rapid Non-Destructive Detection
by Liwei Zhu, Fei Liu, Qianxi Du, Taoxiong Shi, Jiao Deng, Hongyou Li, Fang Cai, Ziye Meng, Qingfu Chen, Jieqiong Zhang and Juan Huang
Plants 2024, 13(15), 2155; https://doi.org/10.3390/plants13152155 - 3 Aug 2024
Viewed by 663
Abstract
Due to the requirements for quality testing and breeding Tartary buckwheat (Fagopyrum tartaricum Gaerth), it is necessary to find a method for the rapid detection of starch content in Tartary buckwheat. To obtain samples with a continuously distributed chemical value, stable Tartary [...] Read more.
Due to the requirements for quality testing and breeding Tartary buckwheat (Fagopyrum tartaricum Gaerth), it is necessary to find a method for the rapid detection of starch content in Tartary buckwheat. To obtain samples with a continuously distributed chemical value, stable Tartary buckwheat recombinant inbred lines were used. After scanning the near-infrared spectra of whole grains, we employed conventional methods to analyze the contents of Tartary buckwheat. The results showed that the contents of total starch, amylose, amylopectin, and resistant starch were 532.1–741.5 mg/g, 176.8–280.2 mg/g, 318.8–497.0 mg/g, and 45.1–105.2 mg/g, respectively. The prediction model for the different starch contents in Tartary buckwheat was established using near-infrared spectroscopy (NIRS) in combination with chemometrics. The Kennard–Stone algorithm was used to split the training set and the test set. Six different methods were used to preprocess the spectra in the wavenumber range of 4000–12,000 cm−1. The Competitive Adaptive Reweighted Sampling algorithm was then used to extract the characteristic spectra, and the prediction model was built using the partial least squares method. Through a comprehensive analysis of each parameter of the model, the best model for the prediction of each nutrient was determined. The correlation coefficient of calibration (Rc) and the correlation coefficient of prediction (Rp) of the best models for total starch and amylose were greater than 0.95, and the Rc and Rp of the best models for amylopectin and resistant starch were also greater than 0.93. The results showed that the NIRS-based prediction model fulfilled the requirement for the rapid determination of Tartary buckwheat starch, thus providing an effective technical approach for the rapid and non-destructive testing of starch content in the food science and agricultural industry. Full article
(This article belongs to the Special Issue Applications of Spectral Techniques in Plant Physiology)
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<p>Frequency distribution of starch-related traits in the grains of the Tartary buckwheat RIL population. (<b>A</b>) Total starch; (<b>B</b>) amylose; (<b>C</b>) amylopectin; (<b>D</b>) resistant starch.</p>
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<p>(<b>A</b>) Regression diagram of true and predicted amylose values and (<b>B</b>) the selected effective wavelengths corresponding to the raw spectrum.</p>
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<p>(<b>A</b>) Regression plot of true and predicted values of amylopectin, and (<b>B</b>) selected effective wavelengths corresponding to the raw spectrum.</p>
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<p>(<b>A</b>) Regression plot of total starch’s true and predicted values and (<b>B</b>) the selected effective wavelengths corresponding to the raw spectrum.</p>
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<p>(<b>A</b>) Regression plot of resistant starch’s true and predicted values and (<b>B</b>) the selected effective wavelengths corresponding to the raw spectrum.</p>
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15 pages, 3036 KiB  
Article
Self-Assembly of Three-Dimensional Hyperbranched Magnetic Composites and Application in High-Turbidity Water Treatment
by Yuan Zhao, Qianlong Fan, Yinhua Liu, Junhui Liu, Mengcheng Zhu, Xuan Wang and Ling Shen
Molecules 2024, 29(15), 3639; https://doi.org/10.3390/molecules29153639 - 1 Aug 2024
Viewed by 752
Abstract
In order to improve dispersibility, polymerization characteristics, chemical stability, and magnetic flocculation performance, magnetic Fe3O4 is often assembled with multifarious polymers to realize a functionalization process. Herein, a typical three-dimensional configuration of hyperbranched amino acid polymer (HAAP) was employed to [...] Read more.
In order to improve dispersibility, polymerization characteristics, chemical stability, and magnetic flocculation performance, magnetic Fe3O4 is often assembled with multifarious polymers to realize a functionalization process. Herein, a typical three-dimensional configuration of hyperbranched amino acid polymer (HAAP) was employed to assemble it with Fe3O4, in which we obtained three-dimensional hyperbranched magnetic amino acid composites (Fe3O4@HAAP). The characterization of the Fe3O4@HAAP composites was analyzed, for instance, their size, morphology, structure, configuration, chemical composition, charged characteristics, and magnetic properties. The magnetic flocculation of kaolin suspensions was conducted under different Fe3O4@HAAP dosages, pHs, and kaolin concentrations. The embedded assembly of HAAP with Fe3O4 was constructed by the N–O bond according to an X-ray photoelectron energy spectrum (XPS) analysis. The characteristic peaks of –OH (3420 cm−1), C=O (1728 cm−1), Fe–O (563 cm−1), and N–H (1622 cm−1) were observed in the Fourier transform infrared spectrometer (FTIR) spectra of Fe3O4@HAAP successfully. In a field emission scanning electron microscope (FE-SEM) observation, Fe3O4@HAAP exhibited a lotus-leaf-like morphological structure. A vibrating sample magnetometer (VSM) showed that Fe3O4@HAAP had a relatively low magnetization (Ms) and magnetic induction (Mr); nevertheless, the ferromagnetic Fe3O4@HAAP could also quickly respond to an external magnetic field. The isoelectric point of Fe3O4@HAAP was at 8.5. Fe3O4@HAAP could not only achieve a 98.5% removal efficiency of kaolin suspensions, but could also overcome the obstacles induced by high-concentration suspensions (4500 NTU), high pHs, and low fields. The results showed that the magnetic flocculation of kaolin with Fe3O4@HAAP was a rapid process with a 91.96% removal efficiency at 0.25 h. In an interaction energy analysis, both the UDLVO and UEDLVO showed electrostatic repulsion between the kaolin particles in the condition of a flocculation distance of <30 nm, and this changed to electrostatic attraction when the separation distance was >30 nm. As Fe3O4@ HAAP was employed, kaolin particles could cross the energy barrier more easily; thus, the fine flocs and particles were destabilized and aggregated further. Rapid magnetic separation was realized under the action of an external magnetic field. Full article
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<p>The FTIR spectra of Fe<sub>3</sub>O<sub>4</sub>, HAAP, Fe<sub>3</sub>O<sub>4</sub>@HAAP.</p>
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<p>The XPS spectra of Fe<sub>3</sub>O<sub>4</sub>@HAAP: (<b>a</b>) Fe 2p spectrum, (<b>b</b>) O 1s spectrum, (<b>c</b>) C 1s spectrum, (<b>d</b>) N 1s spectrum.</p>
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<p>SEM images of Fe<sub>3</sub>O<sub>4</sub>@HAAP: (<b>a</b>) ×50; (<b>b</b>) ×2000; (<b>c</b>) ×10,000; (<b>d</b>) ×50,000.</p>
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<p>The magnetization hysteresis loops of Fe<sub>3</sub>O<sub>4</sub> and Fe<sub>3</sub>O<sub>4</sub>@HAAP.</p>
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<p>Zeta potential of kaolin solution, Fe<sub>3</sub>O<sub>4</sub>, HAAP, and Fe<sub>3</sub>O<sub>4</sub>@HAAP.</p>
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<p>Removing efficiency of Fe<sub>3</sub>O<sub>4</sub>@HAAP on kaolin solution under different conditions: (<b>a</b>) Fe<sub>3</sub>O<sub>4</sub>@HAAP dosage, (<b>b</b>) pH, (<b>c</b>) kaolin concentration, (<b>d</b>) reaction time.</p>
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<p>Removing efficiency of Fe<sub>3</sub>O<sub>4</sub>@HAAP on actual water: (<b>a</b>) Lake 1, (<b>b</b>) Lake 2. The Fe<sub>3</sub>O<sub>4</sub>@HAAP dosage was 50 mg/L, pH = 5.</p>
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<p>The recycling efficiency (<b>a</b>) and removing efficiency (<b>b</b>) of Fe<sub>3</sub>O<sub>4</sub> and Fe<sub>3</sub>O<sub>4</sub>@HAAP on kaolin treatment under 5 recycling times, the colors correspond to different recycling times.</p>
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<p>The interaction energy between Fe<sub>3</sub>O<sub>4</sub>@HAAP and kaolin: (<b>a</b>) kaolin–kaolin; (<b>b</b>) Fe<sub>3</sub>O<sub>4</sub>@HAAP–kaolin. pH = 5.</p>
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15 pages, 3081 KiB  
Article
Synthesis of Keratin Nanoparticles Extracted from Human Hair through Hydrolysis with Concentrated Sulfuric Acid: Characterization and Cytotoxicity
by Otavio A. Silva, Ariane R. S. Rossin, Antônia M. de Oliveira Lima, Andressa D. Valente, Francielle P. Garcia, Celso V. Nakamura, Heveline D. M. Follmann, Rafael Silva and Alessandro F. Martins
Materials 2024, 17(15), 3759; https://doi.org/10.3390/ma17153759 - 30 Jul 2024
Viewed by 1113
Abstract
Human hair, composed primarily of keratin, represents a sustainable waste material suitable for various applications. Synthesizing keratin nanoparticles (KNPs) from human hair for biomedical uses is particularly attractive due to their biocompatibility. In this study, keratin was extracted from human hair using concentrated [...] Read more.
Human hair, composed primarily of keratin, represents a sustainable waste material suitable for various applications. Synthesizing keratin nanoparticles (KNPs) from human hair for biomedical uses is particularly attractive due to their biocompatibility. In this study, keratin was extracted from human hair using concentrated sulfuric acid as the hydrolysis agent for the first time. This process yielded KNPs in both the supernatant (KNPs-S) and precipitate (KNPs-P) phases. Characterization involved scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FTIR), Zeta potential analysis, X-ray diffraction (XRD), and thermogravimetric analysis (TG). KNPs-S and KNPs-P exhibited average diameters of 72 ± 5 nm and 27 ± 5 nm, respectively. The hydrolysis process induced a structural rearrangement favoring β-sheet structures over α-helices in the KNPs. These nanoparticles demonstrated negative Zeta potentials across the pH spectrum. KNPs-S showed higher cytotoxicity (CC50 = 176.67 µg/mL) and hemolytic activity, likely due to their smaller size compared to KNPs-P (CC50 = 246.21 µg/mL), particularly at concentrations of 500 and 1000 µg/mL. In contrast, KNPs-P did not exhibit hemolytic activity within the tested concentration range of 32.5 to 1000 µg/mL. Both KNPs demonstrated cytocompatibility with fibroblast cells in a dose-dependent manner. Compared to other methods reported in the literature and despite requiring careful washing and neutralization steps, sulfuric acid hydrolysis proved effective, rapid, and feasible for producing cytocompatible KNPs (biomaterials) in single-step synthesis. Full article
(This article belongs to the Section Biomaterials)
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<p>Representative scheme of KNP synthesis through hydrolysis with concentrated sulfuric acid.</p>
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<p>FTIR spectra (<b>a</b>) and X-ray diffractograms (<b>b</b>) of human hair (hair) before hydrolysis, keratin nanoparticles (KNPs) obtained from the supernatant resulting from hydrolysis of human hair with concentrated sulfuric acid, and keratin nanoparticles (KNPs-P) obtained from the precipitate resulting from hydrolysis of human hair with concentrated sulfuric acid.</p>
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<p>SEM images ((<b>a</b>) KNPs-P and (<b>b</b>) KNPs-S) and Zeta potentials (<b>c</b>) measured with the KNPs after lyophilization and resuspension in water in the pH range from 2 to 12. KNPs-S = keratin nanoparticles obtained from the supernatant after hydrolysis of human hair with concentrated sulfuric acid; KNPs-P = keratin nanoparticles obtained from the precipitate resulting from hydrolysis of human hair with concentrated sulfuric acid.</p>
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<p>TG/DTG curves: (<b>a</b>) human hair (hair) before hydrolysis, (<b>b</b>) keratin nanoparticles (KNPs) obtained from the supernatant resulting from hydrolysis of human hair with concentrated sulfuric acid, and (<b>c</b>) keratin nanoparticles (KNPs-P) obtained from the precipitate resulting from hydrolysis of human hair with concentrated sulfuric acid.</p>
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14 pages, 681 KiB  
Review
Fundus Autofluorescence in Diabetic Retinopathy
by Otilia-Maria Dumitrescu, Mihail Zemba, Daniel Constantin Brănișteanu, Ruxandra Angela Pîrvulescu, Madalina Radu and Horia Tudor Stanca
J. Pers. Med. 2024, 14(8), 793; https://doi.org/10.3390/jpm14080793 - 26 Jul 2024
Viewed by 868
Abstract
Diabetic retinopathy is a leading cause of visual morbidity worldwide. Fundus autofluorescence is a rapid, non-invasive imaging modality that has gained increased popularity in recent years in the multimodal evaluation of diabetic retinopathy and, in particular, of diabetic macular oedema. Acquired using either [...] Read more.
Diabetic retinopathy is a leading cause of visual morbidity worldwide. Fundus autofluorescence is a rapid, non-invasive imaging modality that has gained increased popularity in recent years in the multimodal evaluation of diabetic retinopathy and, in particular, of diabetic macular oedema. Acquired using either a fundus camera or the confocal scanning laser ophthalmoscope, short-wavelength and near-infrared autofluorescence are the most used techniques in diabetic retinopathy. In diabetic macular oedema, short-wavelength autofluorescence, in its cystoid pattern, is useful for detecting cystoid macular oedema. Increased spot hyperautofluorescence in short-wavelength and granular changes in near-infrared autofluorescence correlate well with other imaging findings, indicating photoreceptor and retinal pigment epithelium damage and being associated with decreased visual acuity. While also being a marker of oxidative stress, increased short-wavelength autofluorescence in the setting of diabetic macular oedema appears to be a prognostic factor for poor visual outcome, even after the resolution of the intraretinal fluid. Autofluorescence also helps in the assessment of diabetic retinal pigment epitheliopathy and choroidopathy. Fundus autofluorescence is an evolving technology that will assist in gaining further insight into the pathophysiology of diabetic retinopathy and allow for a more comprehensive evaluation of these patients. Full article
(This article belongs to the Special Issue Retinal Diseases: Mechanisms, Diagnosis and Treatments)
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<p>Prisma flowchart showing the article selection process.</p>
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25 pages, 7326 KiB  
Article
Physico-Chemical Properties of Copper-Doped Hydroxyapatite Coatings Obtained by Vacuum Deposition Technique
by Yassine Benali, Daniela Predoi, Krzysztof Rokosz, Carmen Steluta Ciobanu, Simona Liliana Iconaru, Steinar Raaen, Catalin Constantin Negrila, Carmen Cimpeanu, Roxana Trusca, Liliana Ghegoiu, Coralia Bleotu, Ioana Cristina Marinas, Miruna Stan and Khaled Boughzala
Materials 2024, 17(15), 3681; https://doi.org/10.3390/ma17153681 - 25 Jul 2024
Viewed by 1125
Abstract
The hydroxyapatite and copper-doped hydroxyapatite coatings (Ca10−xCux(PO4)6(OH)2; xCu = 0, 0.03; HAp and 3CuHAp) were obtained by the vacuum deposition technique. Then, both coatings were analyzed by the X-ray diffraction (XRD), scanning [...] Read more.
The hydroxyapatite and copper-doped hydroxyapatite coatings (Ca10−xCux(PO4)6(OH)2; xCu = 0, 0.03; HAp and 3CuHAp) were obtained by the vacuum deposition technique. Then, both coatings were analyzed by the X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR) and water contact angle techniques. Information regarding the in vitro antibacterial activity and biological evaluation were obtained. The XRD studies confirmed that the obtained thin films consist of a single phase associated with hydroxyapatite (HAp). The obtained 2D and 3D SEM images did not show cracks or other types of surface defects. The FTIR studies’ results proved the presence of vibrational bands characteristic of the hydroxyapatite structure in the studied coating. Moreover, information regarding the HAp and 3CuHAp surface wettability was obtained by water contact angle measurements. The biocompatibility of the HAp and 3CuHAp coatings was evaluated using the HeLa and MG63 cell lines. The cytotoxicity evaluation of the coatings was performed by assessing the cell viability through the MTT assay after incubation with the HAp and 3CuHAp coatings for 24, 48, and 72 h. The results proved that the 3CuHAp coatings exhibited good biocompatible activity for all the tested intervals. The ability of Pseudomonas aeruginosa 27853 ATCC (P. aeruginosa) cells to adhere to and develop on the surface of the HAp and 3CuHAp coatings was investigated using AFM studies. The AFM studies revealed that the 3CuHAp coatings inhibited the formation of P. aeruginosa biofilms. The AFM data indicated that P. aeruginosa’s attachment and development on the 3CuHAp coatings were significantly inhibited within the first 24 h. Both the 2D and 3D topographies showed a rapid decrease in attached bacterial cells over time, with a significant reduction observed after 72 h of exposure. Our studies suggest that 3CuHAp coatings could be suitable candidates for biomedical uses such as the development of new antimicrobial agents. Full article
(This article belongs to the Special Issue Recent Advances and Emerging Challenges in Functional Coatings)
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<p>Schematic representation of the synthesis, characterization techniques and key findings.</p>
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<p>XRD pattern of the HAp (<b>b</b>) and 3CuHAp (<b>a</b>) coatings and JCPDS no. 09-0432.</p>
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<p>(<b>a</b>) SEM image (2D) of the HAp coatings; (<b>b</b>) SEM image (3D) of the HAp coatings; (<b>c</b>) SEM particle size distribution of the HAp coatings; and (<b>d</b>) SEM transversal cross-section image of the HAp coatings.</p>
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<p>(<b>a</b>) SEM image (2D) of the 3CuHAp coatings; (<b>b</b>) SEM image (3D) of the 3CuHAp coatings; (<b>c</b>) SEM particle size distribution of the 3CuHAp coatings; and (<b>d</b>) SEM transversal cross-section image of the 3CuHAp coatings.</p>
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<p>The EDS spectra obtained for the HAp (<b>a</b>) and 3CuHAp (<b>b</b>) coatings.</p>
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<p>(<b>a</b>) The 2D and (<b>b</b>) 3D AFM images obtained for the HAp coatings; and (<b>c</b>) the 2D and (<b>d</b>) 3D AFM images obtained for the 3CuHAp coatings.</p>
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<p>XPS survey scan of the HAp (<b>a</b>) and 3CuHAp (<b>b</b>) coatings obtained by the vacuum deposition process.</p>
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<p>High-resolution XPS spectra of C1s (<b>a</b>), O 1s (<b>b</b>), Ca 2p (<b>c</b>) and P 2p (<b>d</b>) of the HAp coatings obtained by the vacuum deposition process.</p>
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<p>High-resolution XPS spectra of C1s (<b>a</b>), O 1s (<b>b</b>), Ca 2p (<b>c</b>), P 2p (<b>d</b>) and Cu 2p (<b>e</b>) of the 3CuHAp coatings obtained by the vacuum deposition process.</p>
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<p>The FTIR spectra of the HAp and 3CuHAp coatings.</p>
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<p>FTIR second-derivative spectra of the HAp and 3CuHAp coatings.</p>
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<p>Water contact angle of the HAp and 3CuHAp coatings.</p>
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<p>Graphical representation of the cell viability of HeLa and MG63 cells exposed to the HAp and 3CuHAp coatings for 24, 48 and 72 h. The results are depicted as the mean ± standard deviation (SD) and quantified as percentages of the control (100% viability). The ANOVA single-factor test was used for the statistical analysis and <span class="html-italic">p</span> ≤ 0.05 was accepted as statistically significant (* <span class="html-italic">p</span> &lt; 0.03, ** <span class="html-italic">p</span> &lt; 0.001).</p>
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<p>The morphology of HeLa and MG63 cells exposed to the HAp (<b>b</b>,<b>e</b>) and 3CuHAp (<b>c</b>,<b>f</b>) coatings for 72 h. HeLa control cells (<b>a</b>) and MG63 control cells (<b>d</b>).</p>
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<p>The morphology of HeLa and MG63 cells grown on the HAp coatings (<b>a</b>,<b>c</b>) and 3CuHAp coatings (<b>b</b>,<b>d</b>) visualized by fluorescence microscopy evaluation and the morphology of HeLa and MG63 cells grown on the HAp coatings (<b>e</b>,<b>g</b>) and 3CuHAp coatings (<b>f</b>,<b>h</b>) visualized by metallographic microscopy.</p>
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<p>Two-dimensional AFM topography of <span class="html-italic">Pseudomonas aeruginosa</span> 27853 ATCC cells attached to the surface of the 3CuHAp coatings after a 24 (<b>a</b>), 48 (<b>b</b>) and 72 h (<b>c</b>) incubation period and their 3D representation (<b>d</b>–<b>f</b>). Individual bacterial cells chosen and their measured profile in width and in length, where the measurement is pointed out by the yellow arrow.</p>
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<p>Two-dimensional AFM topography of <span class="html-italic">Pseudomonas aeruginosa</span> 27853 ATCC cells attached to the surface of the HAp coatings after a 24 (<b>a</b>), 48 (<b>b</b>) and 72 h (<b>c</b>) incubation period and their 3D representation (<b>d</b>–<b>f</b>). Individual bacterial cells chosen and their measured profile in width and in length, where the measurement is pointed out by the yellow arrow.</p>
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<p>Graphical representation of the log colony forming units (CFUs)/mL of the HAp and 3CuHAp coatings incubated with <span class="html-italic">Pseudomonas aeruginosa</span> cells for 24, 48 and 72 h. The ANOVA single-factor test was used for the statistical analysis and <span class="html-italic">p</span> ≤ 0.05 was accepted as statistically significant (* <span class="html-italic">p</span> &lt; 0.001, ** <span class="html-italic">p</span> &lt; 0.002, and *** <span class="html-italic">p</span> &lt; 0.007).</p>
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