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Keywords = IrO2 synthesis

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14 pages, 3593 KiB  
Article
Spontaneous Emergence of Cefiderocol Resistance in Klebsiella pneumoniae KPC-163: Genomic and Transcriptomic Insights
by Irene Luu, Vyanka Mezcord, Jenny Escalante, German M. Traglia, Marisel R. Tuttobene, Cecilia Rodriguez, Chun Fu Cheng, Quentin Valle, Rajnikant Sharma, Marcelo E. Tolmasky, Robert A. Bonomo, Gauri Rao, Fernando Pasteran and Maria Soledad Ramirez
Antibiotics 2025, 14(8), 832; https://doi.org/10.3390/antibiotics14080832 - 15 Aug 2025
Abstract
Background/Objectives: Carbapenem-resistant Klebsiella pneumoniae (CRKP) is an urgent public health threat due to its rapid dissemination and resistance to last-line antibiotics. Cefiderocol (FDC), a novel siderophore cephalosporin, targets resistant Gram-negative pathogens by exploiting bacterial iron uptake mechanisms. However, resistance to FDC is emerging [...] Read more.
Background/Objectives: Carbapenem-resistant Klebsiella pneumoniae (CRKP) is an urgent public health threat due to its rapid dissemination and resistance to last-line antibiotics. Cefiderocol (FDC), a novel siderophore cephalosporin, targets resistant Gram-negative pathogens by exploiting bacterial iron uptake mechanisms. However, resistance to FDC is emerging among Klebsiella pneumoniae carbapenemase (KPC)-producing K. pneumoniae strains. This study characterizes a spontaneous FDC-resistant subpopulation (IHC216) derived from a KPC-producing strain (KPNMA216) using comprehensive genomic, transcriptional, and phenotypic analyses. Methods: Given the whole-genome sequencing results, where mutations were identified in genes involved in transcriptional regulation and membrane permeability (ompC) among others, in the present work we further explore their potential implications and conduct a more detailed analysis of the IHC216 genome. A qRT-PCR analysis highlighted significant downregulation of classical siderophore-mediated iron acquisition systems (fepA, cirA, iroN) and upregulation of alternative iron uptake pathways (iucA, fiU), reflecting a switch in iron acquisition strategies. Results: A notable downregulation of blaKPC-163 correlated with restored susceptibility to carbapenems, indicating collateral susceptibility. Altered expressions of pbp2 and pbp3 implicated adaptive changes in cell wall synthesis, potentially affecting FDC resistance mechanisms. Furthermore, enhanced oxidative stress responses via upregulated sodC expression and increased capsule production were observed. Conclusions: These findings underscore the complex interplay of genetic and transcriptional adaptations underlying FDC resistance, highlighting potential therapeutic vulnerabilities. Full article
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21 pages, 6025 KiB  
Article
Solar-Activated Titanium-Based Cu4O3/ZrO2/TiO2 Ternary Nano-Heterojunction for Rapid Photocatalytic Degradation of the Textile Dye Everzol Yellow 3RS
by Saira, Wesam Abd El-Fattah, Muhammad Shahid, Sufyan Ashraf, Zeshan Ali Sandhu, Ahlem Guesmi, Naoufel Ben Hamadi, Mohd Farhan and Muhammad Asam Raza
Catalysts 2025, 15(8), 751; https://doi.org/10.3390/catal15080751 - 6 Aug 2025
Viewed by 434
Abstract
Persistent reactive azo dyes released from textile finishing are a serious threat to water systems, but effective methods using sunlight to break them down are still limited. Everzol Yellow 3RS (EY-3RS) is particularly recalcitrant: past studies have relied almost exclusively on physical adsorption [...] Read more.
Persistent reactive azo dyes released from textile finishing are a serious threat to water systems, but effective methods using sunlight to break them down are still limited. Everzol Yellow 3RS (EY-3RS) is particularly recalcitrant: past studies have relied almost exclusively on physical adsorption onto natural or modified clays and zeolites, and no photocatalytic pathway employing engineered nanomaterials has been documented to date. This study reports the synthesis, characterization, and performance of a visible-active ternary nanocomposite, Cu4O3/ZrO2/TiO2, prepared hydrothermally alongside its binary (Cu4O3/ZrO2) and rutile TiO2 counterparts. XRD, FT-IR, SEM-EDX, UV-Vis, and PL analyses confirm a heterostructured architecture with a narrowed optical bandgap of 2.91 eV, efficient charge separation, and a mesoporous nanosphere-in-matrix morphology. Photocatalytic tests conducted under midsummer sunlight reveal that the ternary catalyst removes 91.41% of 40 ppm EY-3RS within 100 min, markedly surpassing the binary catalyst (86.65%) and TiO2 (81.48%). Activity trends persist across a wide range of operational variables, including dye concentrations (20–100 ppm), catalyst dosages (10–40 mg), pH levels (3–11), and irradiation times (up to 100 min). The material retains ≈ 93% of its initial efficiency after four consecutive cycles, evidencing good reusability. This work introduces the first nanophotocatalytic strategy for EY-3RS degradation and underscores the promise of multi-oxide heterojunctions for solar-driven remediation of colored effluents. Full article
(This article belongs to the Special Issue Recent Advances in Photocatalysis for Environmental Applications)
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7 pages, 421 KiB  
Short Note
1,3,4,5-Tetra-O-benzoyl-α-d-tagatopyranose
by Yiming Hu, Akihiro Iyoshi, Yui Makura, Masakazu Tanaka and Atsushi Ueda
Molbank 2025, 2025(3), M2041; https://doi.org/10.3390/M2041 - 22 Jul 2025
Cited by 1 | Viewed by 272
Abstract
d-Tagatose, a rare sugar, is recognized as a low-calorie sweetener, used in daily life. Although d-tagatose exhibits intriguing biological activities, the synthesis of its derivatives has rarely been reported. In this study, we developed a method for synthesizing 1,3,4,5-tetra-O-benzoyl-α- [...] Read more.
d-Tagatose, a rare sugar, is recognized as a low-calorie sweetener, used in daily life. Although d-tagatose exhibits intriguing biological activities, the synthesis of its derivatives has rarely been reported. In this study, we developed a method for synthesizing 1,3,4,5-tetra-O-benzoyl-α-d-tagatopyranose through the regioselective benzoylation of d-tagatose in a single step, achieving an 88% yield on a gram scale. Additionally, 1,2,3,4,5-penta-O-benzoyl-α-d-tagatopyranose and 1,2,3,4,6-penta-O-benzoyl-α-d-tagatofuranose were synthesized in 50% yield as a 7:1 mixture. The structures of the three new benzoylated d-tagatose derivatives were confirmed by 1H, 13C NMR, 2D NMR, FT-IR, and HRMS analyses. Full article
(This article belongs to the Section Organic Synthesis and Biosynthesis)
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15 pages, 3095 KiB  
Article
Effect of Silver/Reduced Graphene Oxide@Titanium Dioxide (Ag/rGO@TiO2) Nanocomposites on the Mechanical Characteristics and Biocompatibility of Poly(Styrene-co-Methyl Methacrylate)-Based Bone Cement
by Mohan Raj Krishnan, Reem M. Alshabib and Edreese H. Alsharaeh
Polymers 2025, 17(14), 1970; https://doi.org/10.3390/polym17141970 - 18 Jul 2025
Viewed by 356
Abstract
This study reports the impact of a silver nanoparticles/reduced graphene oxide@titanium dioxide nanocomposite (Ag/rGO@TiO2) on the mechanical and biocompatibility properties of poly(styrene-co-methylmethacrylate)/poly methyl methacrylate (PS-PMMA/PMMA)-based bone cement. The chemical, structural, mechanical, and thermal characteristics of Ag/rGO@TiO2 nanocomposite-reinforced PS-PMMA bone cement [...] Read more.
This study reports the impact of a silver nanoparticles/reduced graphene oxide@titanium dioxide nanocomposite (Ag/rGO@TiO2) on the mechanical and biocompatibility properties of poly(styrene-co-methylmethacrylate)/poly methyl methacrylate (PS-PMMA/PMMA)-based bone cement. The chemical, structural, mechanical, and thermal characteristics of Ag/rGO@TiO2 nanocomposite-reinforced PS-PMMA bone cement ((Ag/rGO@TiO2)/(PS-PMMA)/PMMA) were evaluated using Fourier Transform Infrared spectroscopy (FT-IR), X-ray diffraction (XRD), nano-indentation, and electron microscopy. FT-IR, XRD, and transmission electron microscopy results confirmed the successful synthesis of the nanocomposite and the nanocomposite-incorporated bone cement. The elastic modulus (E) and hardness (H) of the ((Ag/rGO@TiO2)/(PS-PMMA)/PMMA) bone cement were measured to be 5.09 GPa and 0.202 GPa, respectively, compared to the commercial counterparts, which exhibited E and H values of 1.7 GPa to 3.7 GPa and 0.174 GPa, respectively. Incorporating Ag/rGO@TiO2 nanocomposites significantly enhanced the thermal properties of the bone cement. Additionally, in vitro studies demonstrated that the bone cement was non-toxic to the MG63 cell line. Full article
(This article belongs to the Special Issue Recent Advances and Applications of Polymer Nanocomposites)
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16 pages, 2441 KiB  
Article
Phosphonium Salt-Functionalized β-Cyclodextrin Film for Ultrasensitive and Selective Electrochemical Impedance Spectroscopy Detection of Perchlorate in Drinking Water
by Zeineb Baatout, Achref Jebnouni, Nawfel Sakly, Safa Teka, Nuzaiha Mohamed, Sayda Osman, Raoudha Soury, Mabrouka El Oudi, Salman Hamdan Alsaqri, Nejmeddine Smida Jaballah and Mustapha Majdoub
Polymers 2025, 17(14), 1937; https://doi.org/10.3390/polym17141937 - 15 Jul 2025
Viewed by 441
Abstract
This work represents the first use of a phosphonium salt-functionalized β-Cyclodextrin polymer (β-CDP) as a highly selective sensing membrane for monitoring the safety of drinking water against perchlorate ions (ClO4) using electrochemical impedance spectroscopy (EIS). Structural confirmation via 1H [...] Read more.
This work represents the first use of a phosphonium salt-functionalized β-Cyclodextrin polymer (β-CDP) as a highly selective sensing membrane for monitoring the safety of drinking water against perchlorate ions (ClO4) using electrochemical impedance spectroscopy (EIS). Structural confirmation via 1H NMR, 13C NMR, 31P NMR, and FT-IR spectroscopies combined with AFM and contact angle measurements demonstrate how the enhanced solubility of modified cyclodextrin improves thin film quality. The innovation lies in the synergistic combination of two detection mechanisms: the “Host-Guest” inclusion in the cyclodextrin cavity and anionic exchange between the bromide ions of the phosphonium groups and perchlorate anions. Under optimized functionalization conditions, EIS reveals high sensitivity and selectivity, achieving a record-low detection limit (LOD) of ~10−12 M and a wide linear range of detection (10−11 M–10−4 M). Sensing mechanisms at the functionalized transducer interfaces are examined through numerical fitting of Cole-Cole impedance spectra via a single relaxation equivalent circuit. Real water sample analysis confirms the sensor’s practical applicability, with recoveries between 96.9% and 109.8% and RSDs of 2.4–4.8%. Finally, a comparative study with reported membrane sensors shows that β-CDP offers superior performance, wider range, higher sensitivity, lower LOD, and simpler synthesis. Full article
(This article belongs to the Special Issue Development of Polymer Materials as Functional Coatings)
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19 pages, 1855 KiB  
Article
Enhanced Antimicrobial Activity of Green-Synthesized Artemisia-ZnO Nanoparticles: A Comparative Study with Pure ZnO Nanoparticles and Plant Extract
by Noor Akhras, Abuzer Çelekli and Hüseyin Bozkurt
Foods 2025, 14(14), 2449; https://doi.org/10.3390/foods14142449 - 11 Jul 2025
Viewed by 744
Abstract
The green synthesis of zinc oxide nanoparticles (ZnO NPs) using Artemisia absinthium L. extract has gained considerable attention due to its eco-friendly approach and potential applications in food science. This study investigates the synthesis and characterization of Artemisia-mediated ZnO NPs, focusing on [...] Read more.
The green synthesis of zinc oxide nanoparticles (ZnO NPs) using Artemisia absinthium L. extract has gained considerable attention due to its eco-friendly approach and potential applications in food science. This study investigates the synthesis and characterization of Artemisia-mediated ZnO NPs, focusing on their physicochemical properties. The nanoparticles were characterized using ultraviolet–visible spectroscopy (UV–Vis), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM), and energy dispersive X-ray spectroscopy (EDX). Successful synthesis was achieved through a co-precipitation method, resulting in an average particle size of 36.6 nm. The presence of polyphenols and flavonoids in A. absinthium L. extract acted as both a reducing agent and stabilizer for the nanoparticles. The physicochemical characterization revealed strong absorption peaks indicative of ZnO, confirming successful nanoparticle formation. In addition to the structural findings, this study presents novel insights by demonstrating that Artemisia-mediated ZnO NPs possess significantly enhanced antimicrobial activity compared to both pure ZnO NPs and the plant extract alone. The biosynthesized nanoparticles exhibited notably lower minimum inhibitory concentration (MIC) and minimum bactericidal/fungicidal concentration (MBC/MFC) values against Staphylococcus aureus, Escherichia coli, and Candida albicans, suggesting a strong synergistic effect between ZnO and the phytochemicals of A. absinthium L. Thus, the study confirms and quantifies the superior antibacterial potential of Artemisia-derived ZnO NPs, offering promising implications for food, biomedical and pharmaceutical applications. Full article
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20 pages, 3918 KiB  
Article
Engineered Cu0.5Ni0.5Al2O4/GCN Spinel Nanostructures for Dual-Functional Energy Storage and Electrocatalytic Water Splitting
by Abdus Sami, Sohail Ahmad, Ai-Dang Shan, Sijie Zhang, Liming Fu, Saima Farooq, Salam K. Al-Dawery, Hamed N. Harharah, Ramzi H. Harharah and Gasim Hayder
Processes 2025, 13(7), 2200; https://doi.org/10.3390/pr13072200 - 9 Jul 2025
Viewed by 379
Abstract
The rapid growth in population and industrialization have significantly increased global energy demand, placing immense pressure on finite and environmentally harmful conventional fossil fuel-based energy sources. In this context, the development of hybrid electrocatalysts presents a crucial solution for energy conversion and storage, [...] Read more.
The rapid growth in population and industrialization have significantly increased global energy demand, placing immense pressure on finite and environmentally harmful conventional fossil fuel-based energy sources. In this context, the development of hybrid electrocatalysts presents a crucial solution for energy conversion and storage, addressing environmental challenges while meeting rising energy needs. In this study, the fabrication of a novel bifunctional catalyst, copper nickel aluminum spinel (Cu0.5Ni0.5Al2O4) supported on graphitic carbon nitride (GCN), using a solid-state synthesis process is reported. Because of its effective interface design and spinel cubic structure, the Cu0.5Ni0.5Al2O4/GCN nanocomposite, as synthesized, performs exceptionally well in electrochemical energy conversion, such as the oxygen evolution reaction (OER), the hydrogen evolution reaction (HER), and energy storage. In particular, compared to noble metals, Pt/C- and IrO2-based water-splitting cells require higher voltages (1.70 V), while for the Cu0.5Ni0.5Al2O4/GCN nanocomposite, a voltage of 1.49 V is sufficient to generate a current density of 10 mA cm−2 in an alkaline solution. When used as supercapacitor electrode materials, Cu0.5Ni0.5Al2O4/GCN nanocomposites show a specific capacitance of 1290 F g−1 at a current density of 1 A g−1 and maintain a specific capacitance of 609 F g−1 even at a higher current density of 5 A g−1, suggesting exceptional rate performance and charge storage capacity. The electrode’s exceptional capacitive properties were further confirmed through the determination of the roughness factor (Rf), which represents surface heterogeneity and active area enhancement, with a value of 345.5. These distinctive characteristics render the Cu0.5Ni0.5Al2O4/GCN composite a compelling alternative to fossil fuels in the ongoing quest for a viable replacement. Undoubtedly, the creation of the Cu0.5Ni0.5Al2O4/GCN composite represents a significant breakthrough in addressing the energy crisis and environmental concerns. Owing to its unique composition and electrocatalytic characteristics, it is considered a feasible choice in the pursuit of ecologically sustainable alternatives to fossil fuels. Full article
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27 pages, 7247 KiB  
Article
Layered Perovskite La2Ti2O7 Obtained by Sol–Gel Method with Photocatalytic Activity
by Alexandra Ilie, Luminița Predoană, Crina Anastasescu, Silviu Preda, Ioana Silvia Hosu, Ruxandra M. Costescu, Daniela C. Culiță, Veronica Brătan, Ioan Balint and Maria Zaharescu
Appl. Sci. 2025, 15(14), 7665; https://doi.org/10.3390/app15147665 - 8 Jul 2025
Viewed by 368
Abstract
This paper presents the synthesis of La2Ti2O7 nanoparticles by the sol–gel method starting from lanthanum nitrate and titanium alkoxide (noted as LTA). Subsequently, the lanthanum titanium oxide nanoparticles are modified with noble metals (platinum) using the chemical impregnation [...] Read more.
This paper presents the synthesis of La2Ti2O7 nanoparticles by the sol–gel method starting from lanthanum nitrate and titanium alkoxide (noted as LTA). Subsequently, the lanthanum titanium oxide nanoparticles are modified with noble metals (platinum) using the chemical impregnation method, followed by a reduction process with NaBH4. The comparative analysis of the structure and surface characteristics of the nanopowders subjected to thermal treatment at 900 °C is conducted using Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) with energy-dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray fluorescence (XRF), ultraviolet-visible (UV–Vis) spectroscopy, as well as specific surface area and porosity measurements. The photocatalytic activity is evaluated in the oxidative photodegradation of ethanol (CH3CH2OH) under simulated solar irradiation. The modified sample shows higher specific surfaces areas and improved photocatalytic properties, proving the better conversion of CH3CH2OH than the pure sample. The highest conversion of ethanol (29.75%) is obtained in the case of LTA-Pt after 3 h of simulated solar light irradiation. Full article
(This article belongs to the Special Issue Application of Nanomaterials in the Field of Photocatalysis)
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14 pages, 1106 KiB  
Article
Ni2+ and Cd2+ Biosorption Capacity and Redox-Mediated Toxicity Reduction in Bacterial Strains from Highly Contaminated Soils of Uzbekistan
by Aziza Usmonkulova, Eligio Malusa, Gulchekhra Kadirova, Ilkhom Khalilov, Loredana Canfora and Liliya Abdulmyanova
Microorganisms 2025, 13(7), 1485; https://doi.org/10.3390/microorganisms13071485 - 26 Jun 2025
Viewed by 559
Abstract
In this study, Ni2+ and Cd2+ resistant Pseudomonas aeruginosa 18, Enterobacter ludwigii 11Uz, and Enterobacter cloacae Uz_5 strains were isolated from soils contaminated with heavy metals in the Samarkand and Kashkadarya regions (Uzbekistan), and tested to remove Ni2+ and Cd [...] Read more.
In this study, Ni2+ and Cd2+ resistant Pseudomonas aeruginosa 18, Enterobacter ludwigii 11Uz, and Enterobacter cloacae Uz_5 strains were isolated from soils contaminated with heavy metals in the Samarkand and Kashkadarya regions (Uzbekistan), and tested to remove Ni2+ and Cd2+ ions from the environment via biosorption. The biosorption capacity of these strains was observed under in vitro conditions. The biosorption process was highly dependent on the growing conditions, with the highest biosorption rate observed after 300 min of incubation at pH 7.0, and 40 °C. The presence of functional groups such as S=O, NH2, and COOH in the biosorbing microorganisms was confirmed by IR spectroscopy. The adsorption capacity decreased when the initial metal concentration was increased and was enhanced with higher microbial biomass. Enterobacter ludwigii 11Uz strain was found to alter the toxic oxidation state of Ni2+ and Cd2+ cations, while Pseudomonas aeruginosa 18 and Enterobacter cloacae Uz_5 strains reduced the toxicity of Ni2+ cations only by changing their oxidation state. It was confirmed in our studies that the three selected bacterial strains actively participated in the detoxification of Cd2+ through the synthesis of cysteine amino acid. Full article
(This article belongs to the Special Issue Role of Microbes in the Remediation of Pollutants in the Environment)
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18 pages, 3622 KiB  
Article
Insights into the Crystal Structure and Magnetodielectric Properties of High-Energy Ball Milled Sr Substituted LaFeO3
by Julio C. Aguirre-Espinosa, Félix Sánchez-De Jesús, Claudia A. Cortés-Escobedo and Ana M. Bolarín-Miró
Materials 2025, 18(13), 3014; https://doi.org/10.3390/ma18133014 - 25 Jun 2025
Viewed by 372
Abstract
The effect of strontium substitution on the crystal tructure, as well as the magnetic, and electrical properties of lanthanum ferrite (LaFeO3) synthesized by high-energy ball milling, is studied, with an emphasis on magnetodielectric coupling. X-ray diffraction (XRD) confirmed the successful synthesis [...] Read more.
The effect of strontium substitution on the crystal tructure, as well as the magnetic, and electrical properties of lanthanum ferrite (LaFeO3) synthesized by high-energy ball milling, is studied, with an emphasis on magnetodielectric coupling. X-ray diffraction (XRD) confirmed the successful synthesis of orthorhombic La1−xSrxFeO3 for doping levels up to 0.2 mol. At 0.3 mol Sr2+, two phases appear: La0.6Sr0.4FeO2.976 and La0.8Sr1.2FeO3.714, the latter being metastable. This phase vanishes at 0.5 mol. The Fourier Transform Infrared Spectroscopy (FT-IR) and Scanning Electron Microscopy coupled with Energy Dispersive X-ray Spectroscopy (SEM-EDS) analysis confirmed these results using a vibrating sample magnetometer (VSM), whose measurements show ferromagnetism at 0.1 and 0.3 mol Sr2+, attributed to crystal distortion, magnetic spin rearrangement, and as consequence, modifications in the double-exchange interactions. Dielectric tests reveal that higher Sr2+ concentrations lead to increased relative permittivity, dielectric losses, and conductivity, linked to oxygen vacancy formation. This study demonstrates a room-temperature magnetodielectric coupling of 32% in Sr-doped lanthanum ferrite, highlighting its potential for technological applications. Full article
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13 pages, 2792 KiB  
Article
Engineering C–S–H Sorbents via Hydrothermal Synthesis of PV Glass and Carbide Sludge for Chromium(III) Removal
by Tran Ngo Quan, Le Phan Hoang Chieu and Pham Trung Kien
Coatings 2025, 15(6), 733; https://doi.org/10.3390/coatings15060733 - 19 Jun 2025
Viewed by 637
Abstract
This study investigates the hydrothermal synthesis of calcium silicate hydrate (C-S-H) from photovoltaic (PV) waste glass and carbide sludge as a strategy for resource recovery and sustainable chromium removal from wastewater. Waste-derived precursors were co-ground, blended at controlled Ca/Si molar ratios (0.8, 1.0, [...] Read more.
This study investigates the hydrothermal synthesis of calcium silicate hydrate (C-S-H) from photovoltaic (PV) waste glass and carbide sludge as a strategy for resource recovery and sustainable chromium removal from wastewater. Waste-derived precursors were co-ground, blended at controlled Ca/Si molar ratios (0.8, 1.0, 1.2), and hydrothermally treated at 180 °C for 96 h to yield C-S-H with tunable morphology and crystallinity. Comprehensive characterization using XRD, FT-IR, SEM-EDX, and UV-Vis spectroscopy revealed that a Ca/Si ratio of 1.0 produced a well-ordered tobermorite/xonotlite structure with a high surface area and fibrous network, which is optimal for adsorption. Batch adsorption experiments showed that this material achieved rapid and efficient Cr(III) removal, exceeding 90% uptake within 9 h through a combination of surface complexation, ion exchange (Ca2+/Na+ ↔ Cr3+), and precipitation of CaCrO4 phases. Morphological and structural evolution during adsorption was confirmed by SEM, FT-IR, and XRD, while EDX mapping established the progressive incorporation of Cr into the C-S-H matrix. These findings highlight the viability of upcycling industrial waste into advanced C-S-H sorbents for heavy metal remediation. Further work is recommended to address sorbent regeneration, long-term stability, and application to other contaminants, providing a foundation for circular approaches in advanced wastewater treatment. Full article
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25 pages, 1483 KiB  
Article
Cobalt(II) Complexes of 4′–Nitro–Fenamic Acid: Characterization and Biological Evaluation
by Georgios Malis, Antigoni Roussa, Efstathia Aikaterini Papantopoulou, Stavros Kalogiannis, Antonios G. Hatzidimitriou, Konstantina C. Fylaktakidou and George Psomas
Molecules 2025, 30(12), 2621; https://doi.org/10.3390/molecules30122621 - 17 Jun 2025
Viewed by 410
Abstract
A nitro-derivative of fenamic acid (4′–nitro–fenamic acid) was synthesized and used as ligand for the synthesis of four Co(II) complexes in the absence or presence of the N,N′-donors 2,2′–bipyridylamine, 1,10–phenanthroline and 2,9–dimethyl–1,10–phenanthroline. The characterization of the resultant complexes was performed [...] Read more.
A nitro-derivative of fenamic acid (4′–nitro–fenamic acid) was synthesized and used as ligand for the synthesis of four Co(II) complexes in the absence or presence of the N,N′-donors 2,2′–bipyridylamine, 1,10–phenanthroline and 2,9–dimethyl–1,10–phenanthroline. The characterization of the resultant complexes was performed with diverse techniques (elemental analysis, molar conductivity measurements, IR and UV-vis spectroscopy, single-crystal X-ray crystallography). The biological evaluation of the compounds encompassed (i) antioxidant activity via hydrogen peroxide (H2O2) reduction and free radical scavenging; (ii) antimicrobial screening against two Gram-positive and two Gram-negative bacterial strains; (iii) interactions with calf-thymus (CT) DNA; (iv) cleavage of supercoiled pBR322 plasmid DNA (pDNA), in the dark or under UVA/UVB/visible light irradiation; and (v) binding affinity towards bovine and human serum albumins. The antioxidant activity of the compounds against 2,2′–azinobis–(3–ethylbenzothiazoline–6–sulfonic acid) radicals and H2O2 is significant, especially in the case of H2O2. The complexes exhibit adequate antimicrobial activity against the strains tested. The complexes interact with CT DNA through intercalation with binding constants reaching a magnitude of 106 M−1. The compounds have a significantly enhanced pDNA-cleavage ability under irradiation, showing promising potential as photodynamic therapeutic agents. All compounds can bind tightly and reversibly to both albumins tested. Full article
(This article belongs to the Special Issue Inorganic Chemistry in Europe 2025)
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17 pages, 4080 KiB  
Article
Green Synthesis and Characterization of Iron Oxide Nanoparticles Using Egeria densa Plant Extract
by Maruf Olaide Yekeen, Mubarak Ibrahim, James Wachira and Saroj Pramanik
Appl. Biosci. 2025, 4(2), 27; https://doi.org/10.3390/applbiosci4020027 - 2 Jun 2025
Viewed by 1606
Abstract
An aqueous leaf extract of Egeria densa was used to green-synthesize iron (II) and iron (III) oxide nanoparticles from ferrous sulphate and ferric chloride, respectively. The successful green synthesis of the nanoparticles was confirmed through UV–visible spectroscopy, and the colour of the mixtures [...] Read more.
An aqueous leaf extract of Egeria densa was used to green-synthesize iron (II) and iron (III) oxide nanoparticles from ferrous sulphate and ferric chloride, respectively. The successful green synthesis of the nanoparticles was confirmed through UV–visible spectroscopy, and the colour of the mixtures changed from light-yellow to green-black and reddish-brown for FeO–NPs and Fe2O3–NPs, respectively. The morphological characteristics of the nanoparticles were determined using an X-ray diffractometer (XRD), a Fourier transform infrared spectrophotometer (FTIR), a transmission electron microscope (TEM), and energy-dispersive X-ray spectroscopy (EDX). The UV–Vis spectrum of the FeO–NPs showed a sharp peak at 290 nm due to the surface plasmon resonance, while that of the Fe2O3–NPs showed a sharp peak at 300 nm. TEM analysis revealed that the FeO–NPs were oval to hexagonal in shape and were clustered together with an average size of 18.49 nm, while the Fe2O3-NPs were also oval to hexagonal in shape, but some were irregularly shaped, and they clustered together with an average size of 27.96 nm. EDX analysis showed the presence of elemental iron and oxygen in both types of nanoparticles, indicating that these nanoparticles were essentially present in oxide form. The XRD patterns of both the FeO–NPs and Fe2O3–NPs depicted that the nanoparticles produced were crystalline in nature and exhibited the rhombohedral crystal structure of hematite. The FT-IR spectra revealed that phenolic compounds were present on the surface of the nanoparticles and were responsible for reducing the iron salts into FeO–NPs and Fe2O3–NPs. Conclusively, this work demonstrated for the first time the ability of Elodea aqueous extract to synthesize iron-based nanoparticles from both iron (II) and iron (III) salts, highlighting its versatility as a green reducing and stabilizing agent. The dual-path synthesis approach provides new insights into the influence of the precursor oxidation state on nanoparticle formation, thereby expanding our understanding of plant-mediated nanoparticle production and offering a sustainable route for the fabrication of diverse iron oxide nanostructures. Furthermore, it provides a simple, cost-effective, and environmentally friendly method for the synthesis of the FeO–NPs and Fe2O3–NPs using Egeria densa. Full article
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24 pages, 3339 KiB  
Article
Mesostructured Silica–Zirconia–Tungstophosphoric Acid Composites as Catalyst in Calcium Channel Blocker Nifedipine Synthesis
by Edna X. Aguilera, Ángel G. Sathicq, Alexis Sosa, Marcelo C. Murguía, José J. Martínez, Luis R. Pizzio and Gustavo P. Romanelli
Catalysts 2025, 15(6), 537; https://doi.org/10.3390/catal15060537 - 28 May 2025
Viewed by 641
Abstract
This work studies the effect of mesostructured silica–zirconia–tungstophosphoric acid (SiO2-ZrO2-TPA) composites used as catalysts in the synthesis of nifedipine by the Hantzsch methodology. The selectivity for nifedipine is determined, along with that of secondary products that may form depending [...] Read more.
This work studies the effect of mesostructured silica–zirconia–tungstophosphoric acid (SiO2-ZrO2-TPA) composites used as catalysts in the synthesis of nifedipine by the Hantzsch methodology. The selectivity for nifedipine is determined, along with that of secondary products that may form depending on the reaction conditions. The materials were synthesized via the sol–gel method and characterized by N2 adsorption–desorption isotherms, infrared spectroscopy (FT-IR), 31P solid-state nuclear magnetic resonance (NMR-MAS), X-ray diffraction (XRD), thermogravimetric analysis (TGA), X-ray photoelectron spectra (XPS), and potentiometric titration. The characterization results from the XPS spectra showed that as the Si/Zr ratio drops, the Si-O-Si signal size decreases, while the Zr-O signal size increases. Characterization by titration indicated that an increase in the total acidity of the material, resulting from support modification with tungstophosphoric acid (H3PW12O40, TPA), enhances the reaction yield. The catalytic activity in the solvent-free Hantzsch reaction was evaluated under thermal heating and microwave irradiation. The experiments conducted at 80 °C achieved a maximum yield of 57% after 4 h of reaction using the Si20Zr80TPA30 catalyst (50 mg), while by microwave heating, the yield significantly improved, reaching 77% in only 1 h of reaction. This catalyst exhibited stability and reusability without significant loss of activity up to the third cycle. Depending on the type of material and the reaction conditions, it is possible to modify the selectivity of the reaction, obtaining a 1,2-dihydropyridine isomeric to nifedipine. Reaction intermediates and other minor secondary products that may be formed in the process were also evaluated. Full article
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Article
Synthesis, Characterization, and Biological Activities of Rare Earth Metal Complexes with Gallic Acid
by Nguyen Thi Hien Lan, Hoang Phu Hiep, Dinh Cong Trinh and Pham Van Khang
Inorganics 2025, 13(6), 180; https://doi.org/10.3390/inorganics13060180 - 28 May 2025
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Abstract
This study reports the synthesis and characterization of four novel rare earth-gallic acid complexes, Sm(Gal)3·4H2O, Eu(Gal)3·4H2O, Tb(Gal)3·4H2O, and Dy(Gal)3·4H2O. These complexes were synthesized under optimized conditions (60 [...] Read more.
This study reports the synthesis and characterization of four novel rare earth-gallic acid complexes, Sm(Gal)3·4H2O, Eu(Gal)3·4H2O, Tb(Gal)3·4H2O, and Dy(Gal)3·4H2O. These complexes were synthesized under optimized conditions (60 °C, pH 4–5) and characterized using the Ln3+ elemental content method, infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), mass spectrometry (MS), and fluorescence spectroscopy. IR spectra confirmed the coordination of rare earth ions (Ln3+) with gallic acid through carboxylate oxygen atoms. TGA revealed the thermal decomposition pathways, while MS identified the molecular ion peaks and fragmentation patterns. All complexes exhibited strong luminescence under UV excitation, with emission peaks corresponding to characteristic transitions of Sm3+, Eu3+, Tb3+, and Dy3+. Biological assays demonstrated significant antimicrobial activity against Escherichia coli, Staphylococcus aureus, and Pseudomonas aeruginosa, with Dy(Gal)3·4H2O showing the highest efficacy. Additionally, the complexes displayed inhibitory effects on MCF7 breast cancer cells, with Tb(Gal)3·4H2O exhibiting the lowest IC50 value (11.3 µM). These findings suggest that rare earth metal complexes with gallic acid have potential applications in biomedical fields, particularly as antimicrobial and anticancer agents. Full article
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