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Öğe A novel, extreme simple modification of low-cost pencil graphite electrode (PGE) by single-walled carbon nanotube/pyrenebutyric acid (SWCNT/PBA) nanostructure for sensitive and selective detection of adrenaline(Springer, 2025) Mahmoudi, Ghodrat; Hosseinifard, Mojtaba; Moghadam, Ahmad Jamali; Gargari, Masoumeh Servati; Alizadeh, ValiThe electrochemical carbon nanotube (CNT)-based sensors may provide an effective answer to the growing need for qualitative and quantitative determination of biomolecules. However employing CNTs as interface nanomaterials in various electrode matrices has been challenging for researchers. The most important issues are uniform dispersion of CNTs due to their agglomeration and their interfacial connection with electrode matrices. The superiority of this work lies in its ability to overcome these shortcomings by simple and rapid procedures while remaining negligible sensor surface fouling, but also provides high sensitive, inexpensive, and selective determination of AD molecule. Our work presents the non-covalent functionalization of Single Wall Carbon Nanotubes (SWCNTs) by Pyrenebutyric Acid (PBA) through simple pi-stacking interaction for preserving their electronic structure and preventing their agglomeration in the dispersion step to develop a novel disposable sensor with many attractive analytical performance characteristics for Adrenaline (AD) determination. SWCNTs/PBA hybrid film on a low-cost PGE support have been developed involving soaking of greatly simplified solvent-treated GPE without any further pretreatment step into successfully dispersed SWCNTs/PBA in ethanol, which is a green solvent. The surface morphology of the SWCNTs/PBA nanostructured films were evaluated using Field-emission scanning electron microscopy (FE-SEM), being correlated with the electrochemical characteristics observed by cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS) techniques. The heterogeneous electron transfer rate constant (ks) values 0.09, 0.15 and 0.40 s-1 were obtained for Bare PGE, PGE/SWCNT, and PGE/SWCNT/PBA electrodes, respectively. The obtained ks values have been shown that modification of SWCNTs with PBA improves the analytical properties of the sensor more than those obtained at bare PGE and SWCNTs/PGE due to synergistic effects. The analytical performance of SWCNTs/PBA/PGE was evaluated for AD oxidation in optimum pH 7.0 of phosphate buffer solution in the presence of an excess amount of interfering compounds by DPV technique. The fabricated sensor showed good response with high sensitivity, low detection limit (40 nM), wide linear range (0.25-9 mu M), and excellent reproducibility and repeatability. Also, the simultaneous analyses of AD and Uric Acid (UA) reveal that the fabricated sensor could separate the electrooxidation peaks of these two mixtures and good response with low detection limit (95nM) was also obtained for UA detection. The practical applicability of the fabricated sensor has been successfully tested for the determination of AD in human serum and injection ampoule samples with 98-110% recoveries.Öğe Anion driven tetrel bonding dictated supramolecular architectures of lead(ii) with a zwitterionic form of polydentate N′-(piperidine-1-carbonothioyl)picolinohydrazonamide(Royal society of chemistry, 2024) Mahmoudi, Ghodrat; Garcia-Santos, Isabel; Castineiras, Alfonso; Fernandez-Vazquez, Roi; Gargari, Masoumeh Servati; Gomila, Rosa M.; Frontera, AntonioTwo novel supramolecular heteroleptic complexes [Pb2L2(NO3)(2)](n) (1) and {[Pb3L3](ClO4)(3)}(n)3.25nH(2)O (23.25nH(2)O), obtained from N '-(piperidine-1-carbonothioyl)picolinohydrazonamide (HL) and Pb(NO3)(2) or Pb(ClO4)(2) in aqueous methanol are reported. A crucial role of the auxiliary ligand (NO3- vs. ClO4-) was revealed as a driving force for the formation of the resulting architecture of complexes, which, in turn, are dictated by the formation of tetrel bonds. Complex 1 is constructed from heteroleptic dinuclear centrosymmetric species [Pb2L2(NO3)(2)], which, in turn, are formed from the heteroleptic mononuclear symmetry related [PbL(NO3)] units, linked through a pair of bonds formed between the metal cations and the thioamide nitrogen atoms. The metal cations form a weaker tetrel bond with the symmetry related nitrate atoms, yielding a 1D polymeric chain structure. These chains are interlinked through N-H & ctdot;O hydrogen bonds, formed between the covalently coordinated nitrate oxygen atom and the NH2 hydrogen atom, yielding a 2D supramolecular architecture. Complex 23.25nH(2)O is constructed from the trinuclear species [Pb3L3](ClO4)(3). The trinuclear cation is constructed from three [PbL](+) cations interlinked through two Pb-S and two Pb-N bonds, formed with the thiocarbonyl sulfur atoms and the amide nitrogen atoms. The cations [Pb3L3](3+) are interlinked through two Pb-N and two Pb-S bonds yielding a 1D supramolecular polymeric cationic chain {[Pb3L3](3+)}(n). The two metal cations corresponding to two [PbL](+) units, linked through a pair of the Pb-S bonds, are additionally bridged by two oxygen atoms of one of the perchlorate anions with the formation of two Pb & ctdot;O tetrel bonds. The coordination spheres of the metal cations are filled by one of the oxygen atoms of two different perchlorate anions with the formation of tetrel bonds. One of these perchlorates also forms the N-H & ctdot;O hydrogen bond within the trinuclear unit [Pb3L3](ClO4)(3). 1D supramolecular chains {[Pb3L3](3+)}(n) are interlinked through a myriad of hydrogen bonds formed by the perchlorate anions and crystallized water molecules. The tetrel bonds involving the counterions (Pb & ctdot;O) have been also analysed by DFT calculations via a MEP surface plot and 2D maps of electron localization function (ELF), Laplacian of electron density (del(2)rho) and reduced density gradient (RDG), confirming their noncovalent nature.Öğe Discrete versus polymeric structures of coordination compounds of copper (II) with (pyridin-2-yl)methylenenicotinohydrazide and a library of dicarboxylic acids(ELSEVIER, 05.10.2024) Benito, Monica; Mahmoudi, Ghodrat; Molins, Elies; Zangrando, Ennio; Gargari, Masoumeh Servati; Frontera, Antonio; Safin, Damir A.A series of copper(II) discrete and polymeric coordination compounds, namely [{CuL(H2O)}(2)(fum)] (1), [{CuL(H2O)}(2)(mes)] (2), [Cu2L2(glu)](n)2n(H2O) (32n(H2O)) and [Cu3L2(adi)(2)](n) (4) were fabricated from (pyridin-2-yl)methylenenicotinohydrazide (HL) and a library of dicarboxylic acids, namely fumaric acid (H(2)fum), mesaconic acid (H(2)mes), glutaric acid (H(2)glu) and adipic acid (H(2)adi), using evaporative crystallization, grinding and slurry synthesis methods. The obtained coordination compounds have been fully characterized by single crystal X-ray diffraction revealing different types of complexes depending on the linker length, viz. from dinuclear complexes for the shorter linkers (fumaric and mesaconic acids) to 1D and 2D coordination polymers for longer glutaric and adipic acids. Thermal stability and spectroscopic features (FTIR and diffuse reflectance) of complexes were also studied. For the nonpolymeric compounds 1 and 2, the supramolecular assemblies driven by a combination of antiparallel pi-stacking and hydrogen bonding interactions have been studied and compared using DFT calculations, MEP surface analysis and a combination of QTAIM and NCIplot computational tools.Öğe In-situ synthesis of SnO/CuSnO 3 nanostructures to catalyze azo dye degradation, CO 2 reduction, and amines direct alkylation reactions under visible light(Elsevier, 2024) Padervand, Mohsen; Bargahi, Alireza; Eftekhari-Sis, Bagher; Saadi, Mina; Ghasemi, Shahnaz; Dawi, Elmuez A.; Labidi, Abdelkader; Mahmoudi, Ghodrat; Gargari, Masoumeh ServatiThe extensive use of photocatalysis to address environmental concerns, energy production, and organic transformations has attracted attention in recent decades. The SnO/CSO photocatalytic materials were fabricated through a single-step hydrothermal method and comprehensively characterized using a muti-technique approach to demonstrate the physicochemical, morphological, and electronic features. According to the photocatalytic experiments, the SnO/CSO could remove >96% of acid blue 92 (AB92) azo dye under optimum conditions , with rate constant 2.37 x 10(-2) min(-1). Furthermore, the photocatalyst significantly outperformed commercial TiO2 (P25), in reducing CO2 to CO and CH4 with a production rate of 10.8 and 1.18 mu mol.g(-1).h(-1), respectively, under visible light irradiation. The successful direct alkylation of amines to valuable organic compounds within 10 min of the reaction time with a conversion selectivity of >90% was another capability of the materials, making it a good candidate for pharmaceutical synthesis purposes.