Search Results (95)

p-nitrophenol (p-NP) is a pollutant with environmental persistence, bioaccumulation potential, and significant health risks, and is widely dispersed in wastewater, so efficient removal of p-NP is imperative. Among the various methods, the catalytic reduction of p-NP to p-aminophenol (p-AP) using sodium borohydride (NaBH₄) is a particularly promising one and, herein, catalysts play a crucial role. Among the various metals, Au shows unique catalytic activity for p-NP reduction. However, nanosized Au often exhibit limited activity and stability due to their high surface free energy. To address this challenge, we designed and synthesized Au-SnO_x hybrid nanoparticles confined within hollow mesoporous silica nanoreactors (Au-SnO_x@hm-SiO₂) via a soft-template-assisted co-adsorption strategy. The resulting bimetallic Au-SnO_x@hm-SiO₂ nanoreactor showed significantly enhanced catalytic activity toward the NaBH₄-mediated reduction of p-nitrophenol (p-NP) compared with its monometallic Au@hm-SiO₂ counterpart, owing to the synergistic effect between Au and SnO_x. Among various Au/Sn ratios, the catalyst with an Au/Sn molar ratio of 1:0.1 demonstrated the highest activity, achieving complete conversion of p-NP within 5 min at a p-NP/Au molar ratio of 529:1—a tenfold improvement over Au@hm-SiO₂. Moreover, the catalyst maintained high efficiency over six consecutive cycles, with only slight deactivation, benefiting from the protective silica shell. Full article

The catalytic reduction of toxic 4-Nitrophenol (4-NP) to valuable 4-aminophenol is highly important for environmental remediation. However, developing catalysts with high activity, good recyclability, and facile preparation remains challenging. Herein, Ag@Fe₃O₄ nanocomposites were controllably synthesized with a facile one-pot polyol method. By varying the Ag:Fe precursor ratio, the structure could be tuned from dense and porous core-shell to Janus architectures. The porous Ag@Fe₃O₄ nanoreactors (Ag:Fe-0.4) exhibited exceptional catalytic performance, achieving complete 4-NP reduction within 75 s, with an apparent rate constant (k) of 6.29 × 10⁻² s⁻¹, a normalized rate constant (k_n) of 3742 s⁻¹ mmol⁻¹, and a TOF value of 1042 h⁻¹. XPS results verified that the excellent activity originated from the porous structure and interfacial charge transfer from Ag to Fe₃O₄. The catalysts showed super-paramagnetism and could be reused for at least eight cycles with >95% conversion retained. It also displayed high efficiency in reducing diverse nitroaromatics and in natural water. This work highlights the significance of structural and electronic modulation, providing a scalable strategy for magnetically recyclable catalysts toward environmental remediation and heterogeneous catalysis. Full article

Proanthocyanidins (PACs) are a key group of bioactive phytochemicals known to provide health benefits. Most PACs are non-bioavailable polymeric molecules that need to be biotransformed by colonic microbes into simple metabolites to exert their pharmacological effects. In this study, six previously unexamined PAC metabolites from Saccharomyces cerevisiae, 3-aminophenol (3-AMP), 3-aminosalicylic acid, 2,4-dihydroxy-6-methylbenzaldehyde, 4-hydroxyphenylacetamide (4-HPA), 3-phenyllactic acid, and 2,4,6-trihydroxyacetophenone, were tested for their antiadipogenic activity using an insulin-dependent 3T3-L1 preadipocyte differentiation model. Lipid accumulation in differentiating preadipocytes was visualized and measured with the Oil Red O assay. Only 3-AMP and 4-HPA significantly reduced lipid accumulation at a concentration of 25 µM. To understand the cellular mechanisms, protein levels of key regulators of adipogenesis and lipid metabolism were analyzed using Western blotting. 3-AMP and 4-HPA may attenuate lipid accumulation by suppressing de novo lipogenesis, with 3-AMP downregulating the peroxisome proliferator-activated receptor (PPAR)-γ/acetyl-CoA carboxylase (ACC)/fatty acid synthase (FAS) axis and 4-HPA primarily inhibiting ACC/FAS signaling. Molecular docking studies indicated that 3-AMP may downregulate PPAR-γ expression through competitive inhibition of insulin receptors. These preliminary findings suggest that 3-AMP and 4-HPA exhibit potential antiadipogenic effects, highlighting PAC-derived postbiotics as promising nutraceuticals for mitigating obesity risk. Full article

Benzoxazoles are recognized as significant building blocks in organic synthesis and materials science. This work observed the formation of benzoxazole from o-aminophenol and o-hydroxybenzaldehyde using online ¹H NMR (continuous flow cell, 80 MHz). The identification of changes in the functional group was complemented by ATR-FTIR analysis. Additionally, the kinetic roles of phenylboronic acid and cyanide in the one-pot condensation-cyclization reaction are examined. Real-time monitoring has revealed three observable events: the rapid condensation of the aldehyde and o-aminophenol to produce the imine; the formation of the boron complex in the presence of phenylboronic acid; and the cyanide-assisted cyclization that converts the intermediate into benzoxazole. The findings clarify the transformations that control throughput and provide valuable insights for optimizing reagent loadings under environmentally friendly conditions. Full article

Paracetamol (PAR) is a common antipyretic and analgesic extensively used to treat cold and flu symptoms. It has been proven to be effective in headaches and relieving fever and pain. It is usually found as an over-the-counter drug, which has been associated with an increase in cases of poisoning due to overdose. Therefore, the development of new analytical tools for the detection of PAR at low concentrations in different samples is necessary. In this work, a Molecularly Imprinted Polymer (MIP)-based electrochemical sensor was designed for the selective and sensitive determination of PAR using a glassy carbon electrode (GCE) modified with a polymeric film obtained through the electropolymerization of o-aminophenol. A complete characterization based on electrochemical techniques, such as electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV), and scanning electron microscopy (SEM) was used to examine all steps involved in the construction of the MIP-based electrochemical sensor. In addition, all parameters affecting the MIP were optimized. As a result, the MIP-based electrochemical sensor showed a very low limit of detection (LOD) of 10 nM, with an analytical sensitivity of (3.4 ± 0.1) A M⁻¹. In addition, construction of the MIP-based electrochemical sensor showed highly reproducibility, expressed in terms of a variation coefficient lower than 4%. The MIP-based electrochemical sensor was successfully used in an assay for the determination of PAR in pharmaceutical products. The performance of the MIP-based electrochemical sensor was compared to High Performance Liquid Chromatography (HPLC) for the determination of PAR in pharmaceutical samples, showing excellent agreement between the two methodologies. A very important aspect of the developed sensor was its reusability for at least twenty times. The MIP-based electrochemical sensor is a reliable analytical tool for the determination of PAR. Full article

An anion exchange-assisted technique was used for the synthesis of platinum-decorated SnO₂ supports, providing nanocatalysts with enhanced activity for the reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP). In this study, a series of SnO₂ supports, namely SnA (synthesized almost at room temperature), SnB (hydrothermally treated at 180 °C), and SnC (annealed at 600 °C), are systematically investigated, all loaded with 1 mol% Pt from H₂PtCl₆ under identical mild conditions. The chloride ions from the SnCl₄ precursors were efficiently removed via a strong-base anion exchange reaction, resulting in highly dispersed, crystalline ~5 nm cassiterite SnO₂ particles. All Pt/SnO₂ composites displayed mesoporous structures with type IVa isotherms and H₂-type hysteresis, with SP1a (Pt on SnA) exhibiting the largest surface area (122.6 m²/g) and the smallest pores (~3.5 nm). STEM-HAADF imaging revealed well-dispersed PtOx domains (~0.85 nm), while XPS confirmed the dominant Pt⁴⁺ and Pt²⁺ species, with ~25% Pt⁰ likely resulting from photoreduction and/or interactions with Sn–OH surface groups. Raman spectroscopy revealed three new bands (260–360 cm⁻¹) that were clearly visible in the sample with 10 mol% Pt and were due to the vibrational modes of the PtOx species and Pt-Cl bonds introduced due the addition and hydrolysis of H₂PtCl₆ precursor. TGA/DSC analysis revealed the highest mass loss for SP1a (~7.3%), confirming the strong hydration of the PtOx domains. Despite the predominance of oxidized PtOx species, SP1a exhibited the highest catalytic activity (k_app = 1.27 × 10⁻² s⁻¹) and retained 84.5% activity for the reduction of 4-NP to 4-AP after 10 cycles. This chloride-free low-temperature synthesis route offers a promising and generalizable strategy for the preparation of noble metal-based nanocatalysts on oxide supports with high catalytic activity and reusability. Full article

Vitamins are crucial micro-nutrients for overall well-being, making continuous monitoring essential. There are demands to provide an alternative detection, especially using a portable detection or a point-of-care-testing (POCT) device. One promising approach is employing an in situ electro-polymerised MIP (eMIP), which offers a straightforward polymerisation technique on screen-printed electrodes (SPEs). Here, we report a review based on three databases (PubMed, Scopus, and Web of Science) from 2014 to 2024 using medical subject heading (MeSH) terms “electrochemical polymerisation” OR “electropolymerisation” crossed with the terms “molecularly imprinted polymer” AND “vitamin A” OR “vitamin D” OR “vitamin E” OR “vitamin K” OR “fat soluble vitamin” OR “vitamin B” OR “vitamin C” OR “water soluble vitamin”. The resulting 12 articles covered the detection of vitamins in ascorbic acid, riboflavin, cholecalciferol, calcifediol, and menadione using monomers of catechol (CAT), 3,4-ethylenedioxythiophene (EDOT), o-aminophenol (oAP), o-phenylenediamine (oPD), pyrrole, p-aminophenol (pAP), p-phenylenediamine (pPD), or resorcinol (RES), using common bare electrodes including graphite rod electrode (GRE), glassy carbon electrode (GCE), gold electrode (GE), and screen-printed carbon electrode (SPCE). The most common electrochemical detections were differential pulse voltammetry (DPV) and linear sweep voltammetry (LSV). The imprinting factor (IF) of the eMIP-modified electrodes were from 1.6 to 21.0, whereas the cross-reactivity was from 0.0% to 29.9%. Several types of food and biological samples were tested, such as supplement tablets, poultry and pharmaceutical drugs, soft drinks, beverages, milk, infant formula, human and calf serum, and human plasma. However, more discoveries and development of detection methods needs to be performed, especially for the vitamins that have not been studied yet. This will allow the improvement in the application of eMIPs on portable-based detection and POCT devices. Full article

Designing conducting polymers with novel structures is essential for electrochemical energy storage devices. Here, copolymers of s-triazine and o-aminophenol are electropolymerized from an aqueous solution onto a carbon cloth substrate using the galvanostatic method. The poly(s-triazine-co-o-aminophenol) (PT-co-oAP) is characterized, and its charge storage properties are investigated in 1 M H₂SO₄ and in 1 M ZnSO₄. At 1 A g⁻¹, the specific capacities of PT-co-oAP reach 101.3 mAh g⁻¹ and 84.4 mAh g⁻¹ in 1 M H₂SO₄ and in 1 M ZnSO₄, respectively. The specific capacity of PT-co-oAP maintains 90.3% of its initial value after cycling at 10 A g⁻¹ for 2000 cycles in 1 M H₂SO₄. The high specific capacity achieved originates from abundant surface active sites, facile ion diffusion, with optimized active site structure achieved by forming copolymer. The charge storage mechanism involves the redox processes of amino/imino groups and hydroxyl/carbonyl groups in the copolymer, together with the insertion of cations. Two electrode devices using two PT-co-oAP and aqueous 1 M H₂SO₄ are assembled, and the maximum energy density reaches 63 Wh kg⁻¹ at 0.5 A g⁻¹ with a power density of 540 W kg⁻¹. The capacity retention of the device after 3000 cycles at 10 A g⁻¹ reaches 81.2%. Full article

We report a method for the synthesis of 2-substituted benzoxazoles from tertiary amides and 2-aminophenols in the presence of triflic anhydride (Tf₂O) and 2-Fluoropyridine (2-F-Pyr). The cascade reaction involves the activation of the amide carbonyl group by Tf₂O, nucleophilic addition, intramolecular cyclization, and elimination. Furthermore, we explore the scope of this method by varying both the amide and 2-aminophenol substrates, highlighting its versatility in the synthesis of a wide range of functionalized benzoxazole derivatives. Full article

The availability of water-soluble nanoparticles allows catalytic reactions to occur in highly desirable green environments. The catalytic activity and selectivity of water-soluble palladium nanoparticles capped with 6-(carboxylate)hexanethiolate (C6-PdNP) and 5-(trimethylammonio)pentanethiolate (C5-PdNP) were investigated for the reduction of 4-nitrophenol, the oxidation of α,β-conjugated aldehydes, and the C-C coupling of phenylboronic acid. The study showed that between the two PdNPs, C6-PdNP exhibits better catalytic activity for the reduction of 4-nitrophenol to 4-aminophenol in the presence of sodium borohydride and the selective oxidation of conjugated aldehydes to conjugated carboxylic acids. For the latter reaction, molecular hydrogen (H₂) and H₂O act as oxidants for the surface palladium atoms on PdNPs and conjugated aldehyde substrates, respectively. The results indicated that the competing addition activities of Pd-H and H₂O toward the π-bond of different unsaturated substrates promote either reduction or oxidation reactions under mild conditions in organic solvent-free environments. In comparison, C5-PdNP exhibited higher catalytic activity for the C-C coupling of phenylboronic acid. Gas chromatography–mass spectrometry (GC-MS) was mainly used as an analytical technique to examine the products of catalytic reactions. Full article

The reduction of unfriendly 4-nitrophenol to make it unimpactful with the environment (4-aminophenol) was carried out using the metastable form of copper ferrite (CuFe₅O₈) synthesized by the co-precipitation of metal nitrate salts, an efficient method with inexpensive and abundant starting materials. The samples were obtained by calcination at various temperatures ranging from 600 °C to 900 °C. The material characterizations, including X-ray diffraction, N₂ adsorption/desorption, scanning electron microscope, X-ray absorption spectroscopy, and ultraviolet–visible spectrometry, were employed to identify the detailed structures and describe their correlations with catalytic activities. The X-ray diffraction and X-ray absorption spectroscopy analyses revealed the presence of mixed CuFe₅O₈ and copper oxide phases, where the formers are rich in Cu²⁺, Fe²⁺, and Fe³⁺ ions. The electron transfer between Cu²⁺, Fe²⁺, and Fe³⁺ led to the high efficiency of the catalytic reaction of the synthesized copper ferrites. Especially for the sample calcined at 600 °C, the apparent kinetic constant (k) for a reduction of 4-nitrophenol was equal to 0.25 min⁻¹, illustrating nearly 100% conversion of 4-nitrophenol to 4-aminophenol within less than 9 min. Regarding the N₂ adsorption/desorption isotherms, the samples calcined at 600 °C have the highest specific Brunauer–Emmett–Teller (BET) surface area (15.93 m² g⁻¹) among the others in the series, which may imply the most effective catalytic performance investigated herein. The post-catalytic X-ray diffraction investigation indicated the stability of the prepared catalysts. Furthermore, the chemical stability of the prepared catalysts was confirmed by its reusability in five consecutive cycles. Full article

Emerging pollutants, such as N-acetyl-para-aminophenol, pose significant challenges to environmental sustainability, and Bi₂Fe₂O₂ (BFO) nanomaterials are an emerging class of piezoelectric materials. This study presents a novel piezoelectric-driven Fenton system based on Bi₂Fe₄O₉ nanosheets for the efficient degradation of organic pollutants. BFO nanosheets with varying thicknesses were synthesized, and their piezoelectric properties were confirmed through piezoresponse force microscopy and heavy metal ion reduction experiments. The piezoelectric electrons generated within the BFO nanosheets facilitate the in situ production of hydrogen peroxide, which in turn drives the Fenton-like reaction. Furthermore, the piezoelectric electrons enhance the redox cycling of iron in the Fenton process, boosting the overall catalytic efficiency. The energy band structure of BFO nanosheets is well-suited for this process, enabling efficient hydrogen peroxide generation and promoting Fe³⁺ reduction. The findings demonstrate that thinner BFO nanosheets exhibit superior piezoelectric activity, leading to enhanced catalytic performance. Additionally, the incorporation of gold nanodots onto BFO nanosheets further boosts their piezocatalytic efficiency, particularly in the reduction of Cr (VI). The system exhibited robust oxidative capacity, stability, and recyclability, with reactive oxygen species (ROS) verified via electron paramagnetic resonance spectroscopy. Overall, BFO nanosheets, with their optimal energy band structure, self-supplied hydrogen peroxide, and enhanced Fe³⁺ reduction, represent a promising, sustainable solution for advanced oxidation processes in wastewater treatment and other applications. Full article

A series of new quinazolin-2,4-dione derivatives incorporating amide/eight-membered nitrogen-heterocycles 2a–c, in addition, acylthiourea/amide/dithiolan-4-one and/or phenylthiazolidin-4-one 3a–d and 4a–d. The starting compound 1 was prepared by reaction of 4-(2,4-dioxo-1,4-dihydro-2H-quinazolin-3-yl)-benzoyl chloride with ammonium thiocyanate and cyanoacetic acid hydrazide. The reaction of 1 with strong electrophiles, namely, o-aminophenol, o-amino thiophenol, and/or o-phenylene diamine, resulted in corresponding quinazolin-2,4-dione derivatives incorporating eight-membered nitrogen-heterocycles 2a–d. Compounds 3a–d and 4a–d were synthesized in good-to-excellent yield through a one-pot multi-component reaction (MCR) of 1 with carbon disulfide and/or phenyl isocyanate under mild alkaline conditions, followed by ethyl chloroacetate, ethyl iodide, methyl iodide, and/or concentrated HCl, respectively. The obtained products were physicochemically characterized by melting points, elemental analysis, and spectroscopic techniques, such as FT-IR, ¹H-NMR, ¹³C-NMR, and MS. The antibacterial efficacy of the obtained eleven molecules was examined in vitro against two Gram-positive bacterial strains (Staphylococcus aureus and Staphylococcus haemolyticus). Furthermore, Computer-Aided Drug Design (CADD) was performed on the synthesized derivatives, standard drug (Methotrexate), and reported antibacterial drug with the target enzymes of bacterial strains (S. aureus and S. haemolyticus) to explain their binding mode of actions. Notably, our findings highlight compounds 2b and 2c as showing both the best antibacterial activity and docking scores against the targets. Finally, according to ADMET predictions, compounds 2b and 2c possessed acceptable pharmacokinetics properties and drug-likeness properties. Full article

Yearly, thousands of tons of wasted coffee grounds are produced according to high coffee consumption. Still, after the coffee brewing, wasted coffee grounds contain some amounts of caffeine (CAF). CAF, in turn, contains multiple O and N chelating atoms in its structure. These have a potential to be reductors for complexes of metals. In this context, within the present study, a set of CAF extracts derived from coffee beans and coffee grounds were obtained and then used for the one-step reduction of ReO₄⁻ ions with no additional toxic chemicals. Within this approach, CAF was applied as a secondary, green resource for the synthesis of unique rhenium nanoparticles (ReNPs) containing Re species at 0 and +6 oxidation states. The obtained ReNPs were identified and characterized with the use of X-ray powder diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM). Further, the capping and stabilization of ReNPs by CAF were verified with the aid of Fourier transformation infrared spectroscopy (FT-IR). The so-obtained “green” ReNPs were then used as a homogenous catalyst in the catalytic hydrogenation of 4-nitrophenol (4-NP). This new nanomaterial revealed a superior catalytic activity, leading to the complete reduction of 4-NP to 4-aminophenol within 40–60 min with a first-order rate constant of 0.255 min⁻¹. Full article

This study investigates the significant impact of metal–support interactions on catalytic reaction mechanisms at the interface of oxide-supported metal nanoparticles. The distinct and contrasting effects of SiO₂ and TiO₂ supports on reaction dynamics using NaBD₄ were studied and focused on the relative yields of [HD]/[H₂] and [D₂]/[H₂]. The findings show a consistent increase in HD yields with rising [BD₄⁻] concentrations. Notably, the sequence of HD yield enhancement follows the order of TiO₂-Au⁰-NPs < Au⁰-NPs < SiO₂-Au⁰-NPs. Conversely, the rate of H₂ evolution during BH₄^- hydrolysis exhibits an inverse trend, with TiO₂-Au⁰-NPs outperforming the others, followed by Au⁰-NPs and SiO₂-Au⁰-NPs, demonstrating the opposing effects exerted by the TiO₂ and SiO₂ supports on the catalytic processes. Further, the catalytic reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP) confirms the catalytic mechanism, with TiO₂-Au⁰-NPs demonstrating superior activity. The catalytic activity observed aligns with the order of TiO₂-Au⁰-NPs > Au⁰-NPs > SiO₂-Au⁰-NPs, suggesting that SiO₂ donates electrons to Au⁰-NPs, while TiO₂ withdraws them. It is of interest to note that two very different processes, that clearly proceed via different mechanisms, are affected similarly by the supports. This study reveals that the choice of support material influences catalytic activity, impacting overall yield and efficiency. These findings underscore the importance of selecting appropriate support materials for tailored catalytic outcomes. Full article