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In this investigation, Pergularia tomentosa leaves were used as a promising source of bioproducts for the reduction of copper sulfate into copper oxide nanoparticles. The prepared nanoparticles were characterized using Fourier-transform infrared spectroscopy (FT-IR), X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Transmission electron microscopy (TEM), and Thermogravimetric analysis (TGA). FI-IR showed the presence of hydroxyl, ester, and aromatic groups, which are characteristics of phenolics and other bioproducts. SEM features exhibited spherical and agglomerated particles. In EDX data, the peak at 1 Kev, is an index of metallic nanoparticles of copper. The signals related to C and O peaks indicated the presence of phytochemicals in the studied extract. The synthesized copper oxide nanoparticles had a face-centered cubic structure. The size of the nanoparticles varied from 1.7 to 15.2 nm. The adsorption capacity of methylene blue using copper oxide nanoparticles reached 93.2 mg/g (pH = 6, T = 22 °C, adsorbent dose = 0.0125 g). Additionally, methylene blue solution was completely decolorized after 2 min of reaction (pH = 6, 0.0057 mg NaBH4, C0 = 10 mg/L, catalyst = 0.005 g). NOVELTY STATEMENTIn this study, Pergularia tomentosa leaves were used, for the first time, as a biomaterial rich in bioproducts for the reduction of copper sulfate into copper oxide nanoparticles. The prepared particles act as promising materials for the decolorization of contaminated water via both adsorption and degradation processes.
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Nanopartículas Metálicas , Nanopartículas , Biodegradação Ambiental , Cobre , Óxidos , Folhas de Planta , Espectroscopia de Infravermelho com Transformada de Fourier , Difração de Raios XRESUMO
The present work describes the preparation and characterization of a new cobalt(III) porphyrin coordination compound named (chlorido)(nicotinoylchloride)[meso-tetra(para-chlorophenyl)porphyrinato]cobalt(III) dichloromethane monosolvate with the formula [CoIII(TClPP)Cl(NTC)]·CH2Cl2 (4). The single-crystal X-ray molecular structure of 4 shows very important ruffling and waving distortions of the porphyrin macrocycle. The Soret and Q absorption bands of 4 are very red-shifted as a consequence of the very distorted porphyrin core. This coordination compound was also studied by fluorescence and cyclic voltammetry. The efficiency of our four porphyrinic compounds-the H2TClPP (1) free-base porphyrin, the [CoII(TClPP)] (2) and [CoIII(TClPP)Cl] (3) starting materials, and the new Co(III) metalloporphyrin [CoIII(TClPP)Cl(NTC)]·CH2Cl2 (4)-as catalysts in the photochemical degradation was tested on malachite green (MG) dye. The current voltage of complexes 3 and 4 was also studied. Electrical parameters, including the saturation current density (Js) and barrier height (Ïb), were measured.
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The growing population and urbanization have adversely affected the environment including water. The waste water from industries has affected not only human but also animals. The availability of clean water is one of the foremost needs for living organism. This makes very urgent to find reliable solutions for cleaning waste water. These days catalysis is one the best solutions to remove and degrade organic pollutants. In this work, porous composite polymer films have been designed through facile method which were employed to stabilize zero-valent metal nanoparticles (NPs). The sustainable, environmentally friendly polymer matrix with attached metal NPs was applied for the effective catalytic degradation of both phenolic compounds and organic dyes. The different composite films consist of ZnO NPs embedded in an Oxidized Alginate-Chitosan (OAlg-CS) biomatrix named as OAlg-CS/ZnO with various percentages of ZnO as a support for metallic Cu NPs. The ZnO NPs have been incorporated into OAlg-CS polymer with 10, 15, and 20 wt% and are designated as OAlg-CS/ZnO-10, OAlg-CS/ZnO-15, OAlg-CS/ZnO-20. Various analytical techniques were utilized to investigate the shape, morphology, elemental composition, functional groups and stability of the composite films. All these polymer nanocomposite films were then evaluated for removal of model organic pollutants comprising p-nitrophenol (4-NP), methylene blue (MB), and methyl orange (MO). The Kapp value for 4-NP was 2.19 × 10-1 min-1, 4.68 × 10-1 min-1 for MO and 8.99× 10-1 min-1 for MB. The experimental results demonstrated that OAlg-CS/ZnO-20 films show the highest catalytic activity as compared to OAlg-CS/ZnO, OAlg-CS/ZnO-10, and OAlg-CS/ZnO-15. The order of rate constants for nitrophenol and dyes using OAlg-CS/ZnO-20 was found to be MB Ë MO Ë 4-NP, showing the selectivity of these composite films. The prepared composite films were also investigated for their antibacterial activity against Gram-positive and Gram-negative bacteria and all the films exhibited good anti-bacterial activity, with OAlg-CS/ZnO-20 showed the highest anti-bacterial activity.
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The cationic methylene blue (MB) dye sequestration was studied by using oxidized carboxymethyl cellulose-chitosan (OCMC-CS) and its composite films with silicon carbide (OCMC-CS-SiC), and silica-coated SiC nanoparticles (OCMC-CS-SiC@SiO2). The resulting composite films were characterized through various analytical techniques, including Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), Thermogravimetric analysis (TGA), Field emission scanning electron microscopy (FESEM), and energy-dispersive X-ray spectroscopy (EDS). The dye adsorption properties of the synthesized composite films were comprehensively investigated in batch experiments and the effect of parameters such as contact time, initial dye concentration, catalyst dosages, temperature, and pH were systematically evaluated. The results indicated that the film's adsorption efficiency was increased by increasing the contact time, catalyst amount, and temperature, and with a decreased initial concentration of dye solution. The adsorption efficiency was highest at neutral pH. The experimental results demonstrated that OCMC-CS films have high dye adsorption capabilities as compared to OCMC-CS-SiC, and OCMC-CS-SiC@SiO2. Additionally, the desorption investigation suggested that the adsorbents are successfully regenerated. Overall, this study contributes to the development of sustainable and effective adsorbent materials for dye removal applications. These films present a promising and environmentally friendly approach to mitigate dye pollution from aqueous systems.
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Celulose Oxidada , Quitosana , Nanopartículas , Poluentes Químicos da Água , Quitosana/química , Azul de Metileno/química , Carboximetilcelulose Sódica/química , Dióxido de Silício , Celulose , Adsorção , Corantes/química , Poluentes Químicos da Água/química , Cinética , Nanopartículas/química , Concentração de Íons de Hidrogênio , Espectroscopia de Infravermelho com Transformada de FourierRESUMO
Functionalization and various applications of biomaterials have progressively gained a major interest due to the cost-effectiveness, renewability, and biodegradability of these substrates. The current work focalized on the functionalization of microcrystalline cellulose with polyethyleneimine solution (3 %, 5 %, and 10 %) and hydrazine sulfate salt (1:1, 1:2, 2:1) using an impregnation method. Untreated and treated samples were characterized using FT-IR, SEM, XRD, TGA, and DTA analyses. The crystallinity index values for control microcrystalline cellulose, cellulose-polyethyleneimine, and cellulose-hydrazine were 57.13.8 %, 57.29 %, and 52.62 %, respectively. Cellulose-polyethyleneimine (5 %) and cellulose-hydrazine (1:1) displayed the highest adsorption capacities for calmagite (an anionic dye). At equilibrium, the maximum adsorption capacities for calmagite achieved 104 mg/g for cellulose-polyethyleneimine (5 %), 45 mg/g for cellulose-hydrazine (1:1), and only 12.4 mg/g for untreated cellulose. Adsorption kinetics complied well with the pseudo-second-order kinetic model. The adsorption isotherm fitted well with the Langmuir isotherm. Overall, the functionalized cellulosic samples could be considered potential materials for the treatment of contaminated waters.
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Corantes , Poluentes Químicos da Água , Corantes/química , Polietilenoimina/química , Espectroscopia de Infravermelho com Transformada de Fourier , Adsorção , Celulose/química , Hidrazinas , Poluentes Químicos da Água/química , Cinética , Concentração de Íons de HidrogênioRESUMO
A highly selective and ultra-sensitive electrochemical sensing probe was proposed by combining sulfated-carboxymethyl cellulose (CMC-S) and a functionalized-multiwalled carbon nanotube (f-MWNT) nano-composite with high conductivity and durability. The CMC-S/MWNT nanocomposite was impregnated on a glassy carbon electrode (GCE) to construct the non-enzymatic and mediator-free electrochemical sensing probe for trace detection of As(iii) ions. The fabricated CMC-S/MWNT nanocomposite was characterized by FTIR, SEM, TEM, and XPS. Under the optimized experimental conditions, the sensor exhibited the lowest detection limit of 0.024 nM, a high sensitivity (69.93 µA nM-1 cm-2) with a good linear relationship in the range of 0.2-90 nM As(iii) concentration. The sensor demonstrated strong repeatability, with the current response continuing at 84.52% after 28 days of use, in addition to good selectivity for the determination of As(iii). Additionally, with recovery ranging from 97.2% to 107.2%, the sensor demonstrated comparable sensing capability in tap water, sewage water, and mixed fruit juice. The electrochemical sensor for detecting trace levels of As(iii) in actual samples is anticipated to be produced by this effort and is expected to possess great selectivity, good stability, and sensitivity.
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[This corrects the article DOI: 10.1039/D3RA03808D.].
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Thiazol-based molecules have practically infinite biological implementation. Today, there are many medical applications for compounds containing the thiazole moiety owing to their presence in most clinically applied anticancer drugs, such as dasatinib, dabrafenib, ixabepilone, patellamide A and epothilone. In this study, the polycondensation, of a new group of thiazole-containing polyamides with the formulas PA1-4 was carried out by the interaction of 2-aminothiazole diphenyl sulfide and variable diacid chlorides in dimethyl formamide in the presence of potassium carbonate anhydrous as a catalyst. Fourier transform-infrared spectroscopy (FTIR) was initially used to figure out the PA1-4 structures, which were further characterized using solubility, gel permeation chromatography (GPC), X-ray diffraction analyses (XRD) and scanning electron microscopy (SEM). The solubility results revealed that the presence of heteroaromatic thiazole ring units and sulfur content in the polyamides main chain, made the solubility easier as it increases the chain packing distance. From the values of average molecular weight, it was clear that all synthesized polyamides have almost the same chain length which ranged from 37,561.80 to 39,827.66. Moreover, the thermogravimetric analysis (TGA) confirm that PA1-4 were thermally stable even at high temperatures especially the polyamides which were synthesized from aromatic diacid chlorides. Furthermore, the newly synthesized polyamides were investigated for their antimicrobial properties against different species of Gram-positive and Gram-negative bacteria and also against different fungi. The results revealed that compound PA2 showed the highest antibacterial activity. Also, their inhibitory activity against breast carcinoma cells (MCF-7 cell line) and colon carcinoma cells (HCT cell line) was evaluated. It was clear that there was an enhancement in the anticancer activity for the synthesized polyamides owing to the presence of the thiazole moiety as well as sulfur linkage. According to the results of the 50% inhibitory concentration (IC50), the synthesized polymers were found to be more active against the MCF-7 cell line than the HCT cell line.
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MnO2 and MnO2 blended with 1 and 2 weight percent of activated carbon (AC), MnO2/AC1 and MnO2/AC2 were synthesized through the sol-gel method. The pure chitosan (CS) films were cast in the form of films. Similarly, 5 weight% of each MnO2, AC, MnO2/AC1 and MnO2/AC2 was intermingled with the CS to produce different films, such as CS-AC, CS-MnO2, CS-MnO2/AC1 and CS-MnO2/AC2. Zero-valent Co NPs were then supported on these films through the chemical reduction method and expressed as CS@Co, CS-AC@Co, CS-MnO2@Co, CS-MnO2/AC1@Co and CS-MnO2/AC2@Co NPs. All the catalysts were characterized by field emission scanning electron microscopy (FESEM), energy-dispersive spectroscopy (EDS) and X-ray diffraction (XRD) techniques. The synthesized catalysts were used as a dip catalyst against the hydrogenation of 4-nitrophenol (4NP), and for the degradation of methyl orange (MO) and Congo red (CR) dyes. The kapp and R2 values were deduced from pseudo-first-order kinetics for 4NP and MO and zero-order kinetics for CR dye. The kapp values of CS-AC@Co and CS-MnO2/AC1@Co NPs for 4NP hydrogenation were higher than those for any other member of the series, at 1.14 × 10-1 and 1.56 × 10-1 min-1 respectively. Similarly, the rate of CR degradation was highest with CS-AC@Co. The R2 values for 4NP, MO and CR dyes were above 0.9, which indicated that the application of pseudo-first- and zero-order models were appropriate for this study. Furthermore, the antibacterial activity of all the catalysts was evaluated against Pseudomonas aeruginosa and Escherichia coli. The CS-AC@Co NPs exhibited the highest zone of inhibition compared to other catalysts against P. aeruginosa, while all the catalysts were inactive against E. coli. This study reveals that the catalyst can be used for the degradation of other pollutants and for microbial inhibition.
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Cadmium sulfide (CdS) quantum dots (QDs) were homogeneously embedded into chitosan (CTS), denoted as CdS@CTS, via an in situ hydrothermal method. The intact structure of the synthesized materials was preserved using freeze-drying. The materials were characterized using X-ray diffraction (XRD), X-ray photoelectron spectroscopy, transmission electron microscopy, high-resolution TEM, scanning TEM, dispersive energy X-ray (EDX) for elemental analysis and mapping, Fourier transform infrared spectroscopy, nitrogen adsorption-desorption isotherms, thermogravimetric analysis, UV-vis spectroscopy, and diffuse reflectance spectroscopy (DRS). The synthesis procedure offered CdS QDs of 1-7 nm (average particle size of 3.2 nm). The functional groups of CTS modulate the in situ growth of CdS QDs and prevent the agglomeration of CdS QDs, offering homogenous distribution inside CTS. CdS@CTS QDs can also be used for naked-eye detection of heavy metals with high selectivity toward copper (Cu2+) ions. The mechanism of interactions between Cu2+ ions and CdS@CTS QDs were further studied.
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The evolution and development of solid-matrix are considered a backbone for supporting and stabilizing of metal nanoparticles (NPs) and are the soul of the catalytic system. In the current study, the alginate-starch microsphere (Alg-St) was cross-linked using CaCl2 as a cross-linker. In addition, the Alg-St microsphere was blended with different percentages of activated carbon (AC). The microspheres adsorbed Cu+2 was reduced to zero-valent copper NPs through NaBH4 and used as a dip-catalyst. The supported Cu NPs cum NaBH4 system was used as dip-catalyst for the hydrogenation of 4-nitrophenol (4NP), 2-nitroanilline (2NA), and degradation of methylene blue (MB) and Congo red (CR) dyes. Among the different kinetics models, the experimental data were well-fitted in the zero-order kinetic model. Moreover pH, and recyclability were studied for 4NP, where the best activity was achieved at pH 7.0 for 4NP. No leaching was observed after 3rd cycle in the catalyst.
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Corantes , Nanopartículas Metálicas , Carvão Vegetal , Microesferas , Hidrogenação , Alginatos , Amido , CatáliseRESUMO
Novel thiazole derivatives possessing phenyl sulfonyl moiety were designed and synthesized as B-RAFV600E kinase inhibitors based on the clinically-approved anticancer drug, dabrafenib. All target compounds showed significant inhibition of B-RAFV600E kinase enzyme at nanomolar levels. Compounds 7b and 13a revealed excellent B-RAFV600E inhibitory activity, superior to that of dabrafenib with IC50 values of 36.3 ± 1.9, 23.1 ± 1.2, and 47.2 ± 2.5 nM, respectively. Moreover, the title compounds were much more selective toward B-RAFV600E kinase than B-RAF wild type. In addition, the most potent compounds were further evaluated for their anticancer activity against B-RAFV600E-mutated and wild type melanoma cells. A positive correlation between the cytotoxic activity and selectivity for B-RAF V600E over B-RAF wild type was clearly observed for compounds 7b, 11c, 13a, and 17. All the screened compounds potently inhibited the growth of WM266.4 melanoma cells with IC50 values in the range from 1.24 to 17.1 µM relative to dabrafenib (IC50 = 16.5 ± 0.91 µM). Compounds 7b, 11a and 11c, 13a, and 17 were much more potent than dabrafenib against B-RAFV600E-mutated WM266.4 melanoma cells. Furthermore, compound 7b suppressed the phosphorylation of downstream ERK1/2 from WM266.4 cells. Also, the docking study revealed the proper orientation and well-fitting of the title compounds into the ATP binding site of B-RAFV600E kinase.
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Hydrogels are three-dimensional, cross-linked, and supramolecular networks that can absorb significant volumes of water. Hydrogels are one of the most promising biomaterials in the biological and biomedical fields, thanks to their hydrophilic properties, biocompatibility, and wide therapeutic potential. Owing to their nontoxic nature and safe use, they are widely accepted for various biomedical applications such as wound dressing, controlled drug delivery, bone regeneration, tissue engineering, biosensors, and artificial contact lenses. Herein, this review comprises different synthetic strategies for hydrogels and their chemical/physical characteristics, and various analytical, optical, and spectroscopic tools for their characterization are discussed. A range of synthetic approaches is also covered for the synthesis and design of hydrogels. It will also cover biomedical applications such as bone regeneration, tissue engineering, and drug delivery. This review addressed the fundamental, general, and applied features of hydrogels in order to facilitate undergraduates, graduates, biomedical students, and researchers in a variety of domains.
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Different films comprising pure chitosan (CS) and chitosan coated sodium zeolites composites films designated as CSZ1, CSZ2, CSZ3 and CSZ4 respectively are presented here for the sequestration of MO dye. The as-synthesized films were characterized by using FSESM, XPS XRD, and TGA analysis. The sequestration of methyl orange dye (MO) was studied under various adsorption parameters i.e. pH effect, reaction temperature, catalytic dosage, interaction period, and original dye concentration in batch experiments. The adsorption power of MO dye sequestration in the presence of CSZ3 was 287 mg g-1 higher than the fine CS (201 mg g-1), and lowest for CSZ4 (173 mg g-1). The experimental data is fitted in the pseudo-second order of chemical kinetics. The Freundlich and Langmuir adsorption models were used on behalf of the analysis of experimental data that revealed multilayered adsorption of MO dye. Kinetics, equilibrium and thermodynamic process were discussed in detailed, suggesting the endothermic and spontaneous process of the adsorption of MO dye on the exterior of films. The present work is general for the MO adsorption, however, it can be applied on large scale applications and can be easily adjustable in the water purification assemblies.
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Compostos Azo/química , Quitosana/química , Purificação da Água/métodos , Adsorção , Compostos Azo/isolamento & purificação , Corantes/química , Concentração de Íons de Hidrogênio , Cinética , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Temperatura , Termodinâmica , Água/química , Poluentes Químicos da Água/químicaRESUMO
Cellulose substrate waste has demonstrated great potential as a biosorbent of pollutants from contaminated water. In this study, Neriumoleander fruit, an agricultural waste biomaterial, was used for the biosorption of methylene blue from synthetic solution. Fourier-transform infrared (FTIR) spectroscopy indicated the presence of the main absorption peak characteristics of cellulose, hemicellulose, and lignin compositions. X-ray diffraction (XRD) pattern exhibited peaks at 2θ = 14.9° and 2θ = 22°, which are characteristics of cellulose I. Scanning electron microscopy (SEM) showed a rough and heterogeneous surface intercepted by some cavities. Thermogravimetric analysis (TGA) showed more than a thermal decomposition point, suggesting that Nerium fruit is composed of cellulose and noncellulosic matters. The pHpzc value of Nerium surface was experimentally determined to be 6.2. Nerium dosage, pH, contact time, dye concentration, and temperature significantly affected the adsorption capacity. The adsorption capacity reached 259 mg/g at 19 °C. The mean free energy ranged from 74.53 to 84.52 KJ mol-1, suggesting a chemisorption process. Thermodynamic parameters define a chemical, exothermic, and nonspontaneous mechanism. The above data suggest that Nerium fruit can be used as an excellent biomaterial for practical purification of water without the need to impart chemical functionalization on its surface.
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In this paper, three adsorption isotherms of N719 dye on two different adsorbents, ZnO nanopowder and ZnO nanorods, at three different thicknesses have been fitted using a monolayer model with three types of receptor sites treated by statistical physics. The model involved parameters are: three coefficients (n 1, n 2 and n 3) indicating the numbers of adsorbed dye molecules per site, three parameters (N m1, N m2 and N m3) indicating the receptor site densities and three adsorption energies ((-ε 1), (-ε 2) and (-ε 3)). The evolution of these parameters in relation with thickness of ZnO was discussed. The pore size distribution (PSD) of ZnO nanopowder and ZnO nanorods as a function of the thickness has been studied using the chosen adequate model. The molecular electrostatic potential (MEP) has been investigated to optimize the different adsorbed geometries of the complex N719 dye@ZnO. The intermolecular interactions between the N719 dye and the ZnO surface have been studied by using the quantum theory of atoms in molecules (AIM) and reduced density gradient RDG. The results of the MEP, topological AIM and RDG are in agreement with the results of statistical physics.
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In this study, we investigated a novel aflatoxin biosensor based on acetylcholinesterase (AChE) inhibition by aflatoxin B1 (AFB1) and developed electrochemical biosensors based on a sodium alginate biopolymer as a new matrix for acetylcholinesterase immobilization. Electrochemical impedance spectroscopy was performed as a convenient transduction method to evaluate the AChE activity through the oxidation of the metabolic product, thiocholine. Satisfactory analytical performances in terms of high sensitivity, good repeatability, and long-term storage stability were obtained with a linear dynamic range from 0.1 to 100 ng/mL and a low detection limit of 0.1 ng/mL, which is below the recommended level of AFB1 (2 µg/L). The suitability of the proposed method was evaluated using the samples of rice supplemented with AFB1 (0.5 ng/mL). The selectivity of the AChE-biosensor for aflatoxins relative to other sets of toxic substances (OTA, AFM 1) was also investigated.