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1.
Chem Commun (Camb) ; 60(23): 3146-3149, 2024 Mar 14.
Artigo em Inglês | MEDLINE | ID: mdl-38348482

RESUMO

Two π-extended cobalt porphyrins are synthesized and one of them is crystallographically characterized. The nanocomposites of nonplanar (curved) porphyrin immobilized multi-walled carbon nanotubes were thoroughly characterized spectroscopically and microscopically, showing ∼200 mV positive shift in the O2 reduction peak potential in aqueous media and ∼100 mV shift in the onset potential of the O2 reduction relative to the control meso-tetraphenylporphyrinatocobalt(II) nanocomposite. Both the π-extended cobalt porphyrin immobilized nanocomposites efficiently catalyze selective 4e-/4H+ O2 reduction under ambient conditions with excellent methanol tolerance and high stability due to effective π-π interactions, and could be an alternative for expensive Pt-based cathode materials in fuel cells.

2.
Sci Rep ; 14(1): 2204, 2024 01 25.
Artigo em Inglês | MEDLINE | ID: mdl-38273022

RESUMO

In the present study, ZnO nanoparticles have been synthesized using an aqueous extract of shilajit. The nanoparticles were characterized using different techniques such as UV (ultraviolet-visible spectrophotometer), FTIR (Fourier transform infrared), XRD (X-ray diffraction), particle size analysis, SEM (scanning electron microscope) and EDAX (Energy-dispersive X-ray) analysis. The UV absorption peak at 422.40 nm was observed for ZnO nanoparticles. SEM analysis showed the shape of nanoparticles to be spherical, FTIR spectrum confirmed the presence of zinc atoms, particle size analysis showed the nanoparticle size, EDAX confirmed the purity of ZnO nanoparticles whereas XRD pattern similar to that of JCPDS card for ZnO confirmed the presence of pure ZnO nanoparticles. The in vitro anticancer activity of ZnO nanoparticles against the HeLa cell line showed the IC50 value of 38.60 µg/mL compared to reference standard cisplatin. This finding confirms that ZnO nanoparticles from shilajit extract have potent cytotoxic effect on human cervical cancer cell lines.


Assuntos
Nanopartículas Metálicas , Minerais , Nanopartículas , Resinas Vegetais , Óxido de Zinco , Humanos , Óxido de Zinco/farmacologia , Óxido de Zinco/metabolismo , Células HeLa , Antibacterianos/farmacologia , Extratos Vegetais/farmacologia , Difração de Raios X , Espectroscopia de Infravermelho com Transformada de Fourier , Testes de Sensibilidade Microbiana
3.
Chemphyschem ; 24(19): e202300117, 2023 Oct 04.
Artigo em Inglês | MEDLINE | ID: mdl-37464546

RESUMO

In the present work, the oxygen reduction reaction (ORR) is explored in an acidic medium with two different catalytic supports (multi-walled carbon nanotubes (MWCNTs) and nitrogen-doped multi-walled carbon nanotubes (NMWCNTs)) and two different catalysts (copper phthalocyanine (CuPc) and sulfonic acid functionalized CuPc (CuPc-SO3 - )). The composite, NMWCNTs-CuPc-SO3 - exhibits high ORR activity (assessed based on the onset potential (0.57 V vs. reversible hydrogen electrode) and Tafel slope) in comparison to the other composites. Rotating ring disc electrode (RRDE) studies demonstrate a highly selective four-electron ORR (less than 2.5 % H2 O2 formation) at the NMWCNTs-CuPc-SO3 - . The synergistic effect of the catalyst support (NMWCNTs) and sulfonic acid functionalization of the catalyst (in CuPc-SO3 - ) increase the efficiency and selectivity of the ORR at the NMWCNTs-CuPc-SO3 - . The catalyst activity of NMWCNTs-CuPc-SO3 - has been compared with many reported materials and found to be better than several catalysts. NMWCNTs-CuPc-SO3 - shows high tolerance for methanol and very small deviation in the onset potential (10 mV) between the linear sweep voltammetry responses recorded before and after 3000 cyclic voltammetry cycles, demonstrating exceptional durability. The high durability is attributed to the stabilization of CuPc-SO3 - by the additional coordination with nitrogen (Cu-Nx ) present on the surface of NMWCNTs.

4.
RSC Adv ; 13(25): 17179-17187, 2023 Jun 05.
Artigo em Inglês | MEDLINE | ID: mdl-37304784

RESUMO

Here, we report an inkjet-printed graphene paper electrode (IP-GPE) for the electrochemical analysis of mercuric ions (Hg(ii)) in industrial wastewater samples. Graphene (Gr) fabricated on a paper substrate was prepared by a facile solution-phase exfoliation method in which ethyl cellulose (EC) behaves as a stabilizing agent. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were utilized to determine the shape and multiple layers of Gr. The crystalline structure and ordered lattice carbon of Gr were confirmed by X-ray diffraction (XRD) and Raman spectroscopy. The nano-ink of Gr-EC was fabricated on the paper substance via an inkjet printer (HP-1112) and IP-GPE was exploited as a working electrode in linear sweep voltammetry (LSV) and cyclic voltammetry (CV) for the electrochemical detection of Hg(ii). The electrochemical detection is found to be diffusion-controlled illustrated by obtaining a correlation coefficient of 0.95 in CV. The present method exhibits a better linear range of 2-100 µM with a limit of detection (LOD) of 0.862 µM for the determination of Hg(ii). The application of IP-GPE in electrochemical analysis shows a user-friendly, facile, and economical method for the quantitative determination of Hg(ii) in municipal wastewater samples.

5.
Langmuir ; 39(23): 8075-8082, 2023 Jun 13.
Artigo em Inglês | MEDLINE | ID: mdl-37264648

RESUMO

Recently, researchers are seeking alternatives to replace Pt-based oxygen reduction reaction (ORR) catalysts used in fuel cells due to their high cost and certain stability and selectivity issues. For this purpose, we have synthesized a nanoconjugate, cobalt(II) porphyrin (5,10,15-triphenyl-20-(4-aminophenyl)porphyrinatocobalt(II), CoTPP-NH2) covalently attached to the acid-functionalized multiwalled carbon nanotubes and characterized by various techniques including UV-vis spectroscopy, FTIR, TGA, FESEM, TEM, and Raman spectroscopy. The oxygen reduction performance of the nanoconjugate is checked in basic medium. The ORR onset potential of the nanoconjugate-modified electrode is nearly the same as that of the state-of-the-art platinum-carbon electrode and stable for more than 3000 CV cycles with a 20 mV difference in the onset potential before and after the 3000 CV cycles. The above extrapolations reveal that the nanoconjugate has efficient performance for the ORR in basic medium.

6.
Chem Asian J ; 17(12): e202200160, 2022 Jun 15.
Artigo em Inglês | MEDLINE | ID: mdl-35445785

RESUMO

Sulfoximine-based metal complexes have gained much interest in recent years owing to their promising properties in synthetic organic chemistry. These sulfoximines have been recently introduced in the field of organometallics. However, the coordination properties of pincer sulfoximine ligands and their metal complexes have not been reported. Here, a C2 -symmetric bissulfoximine-based pincer ligand ((pyridine-2,6-diylbis(methylene))bis(azaneylylidene))bis(diphenyl-λ6 -sulfanone), namely S-P ligand and its metal [M(SP)2 ]2+ {M=Fe (SC-1), Co (SC-2), Ni (SC-3), Cu (SC-4)} complexes, were synthesized. The complexes were characterized by different spectroscopic techniques like UV-Vis, IR, NMR, ESI-MS, and single-crystal XRD. Complexes SC-1 and SC-3 exhibited octahedral geometry irrespective of the metal center. The complexes were systematically explored for electrocatalytic oxygen reduction reaction (ORR) by immobilizing them on a glassy carbon electrode using Nafion. These complexes showed selective two-electron catalytic reduction of O2 to H2 O2 in which complex SC-2 showed the highest selectivity (≈90%) and complex SC-4 showed the highest onset potential (0.75 V).

7.
Environ Sci Pollut Res Int ; 29(53): 79995-80004, 2022 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-35199267

RESUMO

In this study, a simple, one-pot, and eco-friendly biosynthesis of silver nanoparticles (AgNPs) was accomplished with the use of aqueous leaves extract of Cestrum nocturnum L.(AECN). Different techniques like ultraviolet-visible (UV-Vis) spectrophotometry, Fourier transform infrared (FTIR), X-ray diffraction (XRD), transmission electron microscopy (TEM), and scanning area electron diffraction were used to investigate the optical, operational, and physical properties of the green synthesized AECN-AgNPs.The AECN-AgNPs were further used for the detection of Hg2+ by UV-Vis and electrochemical methods. The disintegration of the AECN-AgNPs solution caused the formation of an Ag-Hg amalgam, which caused discoloration of the solution. Sensing performance for a variety of metals such as Na+, K+, Mg2+, Ca2+, Ni2+, Cu 2+, Fe3+, Zn2+, Co2+, Cd2+, Pb2+, As3+, and Mn2+ at 10-mM concentrations was measured in order to determine the selectivity of the sensor towards the Hg2+. For the electrochemical determination of 2 + Hg2+ , AECN-AgNPs were immobilized on a glassy carbon (GC) electrode, and the resulting modified electrode (GC/AECN-AgNPs) was characterized by cyclic voltammetry. This phenomenon is advantageously used for the sensitive determination of trace level Hg2+. GC/AECN-AgNPs demonstrated a linear calibration range of 100 nM to 10 µM and a limit of detection of 21 nM for Hg2+ determination.


Assuntos
Cestrum , Mercúrio , Nanopartículas Metálicas , Prata/química , Nanopartículas Metálicas/química , Verde de Metila , Cádmio , Chumbo , Água/química , Difração de Raios X , Extratos Vegetais/farmacologia , Carbono , Espectroscopia de Infravermelho com Transformada de Fourier
8.
Dalton Trans ; 50(40): 14362-14373, 2021 Oct 19.
Artigo em Inglês | MEDLINE | ID: mdl-34568879

RESUMO

The electrochemical water splitting by transition metal complexes is emerging very rapidly. The nickel complexes also play a very vital role in various biological activities. Here, three new ligands {H2mbhce = N'-(4-methyl-benzoyl), H2pchce = N'-(pyridine-carbonyl) and H2hbhce = N'-(2-hydroxy-benzoyl) hydrazine carbodithioic acid ethyl ester} and their corresponding Ni(II) complexes [Ni(Hmbhce)2(py)2] (1), [Ni(pchce)(o-phen)2]·CH3OH·H2O (2) and [Ni(hbhce)(o-phen)2]·1.75CHCl3·H2O (3) have been synthesized and fully characterized by various physicochemical and X-ray crystallography techniques. The photoluminescence study and thermal degradations were also examined. The treatment of K562 cells with the increasing concentrations of the nickel salts, ligands, and complexes 1, 2, and 3 showed dose-dependent cytotoxicity. The cytotoxic activity of ligands reveals that ligand H2mbhce is more potent in inhibiting the growth of tumor cells in comparison to other ligands H2pbhce and H2hbhce. Cytotoxicity assay results indicate that all complexes have remarkable cytotoxic potential in comparison to either nickel salts or the free ligands. Among these complexes, complex 1 has significantly better anti-tumor activity as compared to complexes 2 and 3. The electrochemical study of complexes 1, 2, and 3 for water oxidation reveals that all the complexes possess admirable electrocatalytic activity towards oxygen evolution reaction (OER) and have lower overpotential (328, 338, and 370 mV, respectively) than many previously reported complexes and RuO2 (390 mV). Among complexes 1, 2, and 3, complex-2 shows a better water oxidation response. Consequently, these complexes have great potential to be utilized in fuel cells. The more reliable electrochemical parameter TOF is also calculated for all three complexes.


Assuntos
Antineoplásicos/farmacologia , Complexos de Coordenação/farmacologia , Técnicas Eletroquímicas , Hidrazinas/farmacologia , Níquel/farmacologia , Oxigênio/química , Tiocarbamatos/farmacologia , Antineoplásicos/síntese química , Antineoplásicos/química , Proliferação de Células/efeitos dos fármacos , Complexos de Coordenação/síntese química , Complexos de Coordenação/química , Ensaios de Seleção de Medicamentos Antitumorais , Humanos , Hidrazinas/química , Células K562 , Estrutura Molecular , Níquel/química , Tiocarbamatos/química
9.
3 Biotech ; 11(1): 10, 2021 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-33442509

RESUMO

This study summarizes the response of a hot spring cyanobacterium Fischerella sp. strain HKAR-14, under simulated light conditions of ultraviolet radiation (UVR), photosynthetically active radiation (PAR), PAR + UV-A (PA) and PAR + UV-A + UV-B (PAB). Exposure to UVR caused a decline in growth and Chl a while total carotene content increased under PA and PAB. Maximum photochemical efficiency of photosystem II (F v /F m) and relative electron transport rate decreased significantly in PA and PAB exposure. Higher non-photochemical quenching and lower photochemical quenching values were observed in UVR-exposed samples as compared to the control. Levels of intracellular reactive oxygen species (ROS) increased significantly in PAB and PA. Fluorescence microscopic images showed an increase in green fluorescence, indicating the generation of ROS in UVR. The antioxidant machinery including superoxide dismutase, catalase and peroxidase showed an increase of 1.76-fold and 2.5-fold superoxide dismutase, 2.4-fold and 3.7-fold catalase, 1.83-fold and 2.5-fold peroxidase activities under PA and PAB, respectively. High-performance liquid chromatography equipped with photodiode array detector, electrospray ionization mass spectrometry, Fourier-transform infrared spectroscopy and nuclear magnetic resonance spectroscopy analyses reveal the occurrence of a single mycosporine-like amino acid, shinorine (λ max 332.3 ± 2 nm, m/z 333.1), with a retention time of 1.157 min. The electrochemical characterization of shinorine was determined by cyclic voltammetry. The shinorine molecule possesses electrochemical activity and represents diffusion-controlled process in 0.1 M (pH 7.0) phosphate buffer. An antioxidant assay of shinorine showed its efficient activity as antioxidant which increased in a dose-dependent manner.

10.
Langmuir ; 36(41): 12202-12212, 2020 Oct 20.
Artigo em Inglês | MEDLINE | ID: mdl-32970946

RESUMO

In the search for alternative sources to replace fossil fuels, carbon nitride materials can be used in a variety of ways. In the present work, porosity is introduced to the carbon nitride material using mesoporous silica material, MCM-41, as a hard template, and a mesoporous carbon nitride (MCN) material is synthesized. Further, the MCN is modified by immobilizing metal phthalocyanine (MPc, where M = Mn, Fe, Co, Ni, Cu, and Zn). The resulting MPc-incorporated MCN materials (MPc@MCN) were tested for the electrocatalytic oxygen reduction reaction (ORR) in acidic and basic media. Detailed studies reveal that the FePc@MCN and CoPc@MCN materials exhibit higher ORR activity than the other composites in 0.1 M KOH. FePc@MCN follows a direct four-electron oxygen reduction mechanism and shows ORR onset potential (vs RHE) at 0.93 V (in 0.1 M KOH), which is very close to the onset potential exhibited by the state-of-the-art material, Pt-C (1.0 V), and higher than several similar composites of MPc with carbon supports tested in similar environments. Besides, due to the inherent property of coordination through nitrogen present on the MCN, FePc@MCN shows excellent stability even after 3000 cyclic voltammetry (CV) cycles. FePc@MCN was found to have a better methanol tolerance in comparison to Pt-C in basic medium. CoPc@MCN shows a highly selective two-electron reduction reaction in both acidic and basic media at lower overpotential than many of the reported catalysts for the two-electron oxygen reduction. Therefore, these materials (FePc@MCN and CoPc@MCN) can be used as suitable alternatives to replace Pt and other expensive materials in ORR and related applications.

11.
Dalton Trans ; 49(11): 3592-3605, 2020 Mar 17.
Artigo em Inglês | MEDLINE | ID: mdl-32129347

RESUMO

Four new heteroleptic Ni(ii) complexes with general formula [Ni(ii)(LL')] (L = 2-(methylene-1,1'-dithiolato)-5-phenylcyclohexane-1,3-dione (L1) and 2-(methylene-1,1'-dithiolato)-5,5'-dimethylcyclohexane-1,3-dione (L2); L' = 1,2-bis(diphenylphosphino)ethane (dppe) and bis(diphenylphosphino)monosulphide methane (dppms) have been synthesized and characterized by elemental analysis and spectroscopy (IR, UV-Vis, 1H, 13C{1H} and 31P{1H} NMR). All complexes 1-4 have also been characterized by PXRD and single crystal X-ray crystallography. The solid state molecular structures revealed distorted square planar geometry about the four-coordinate Ni(ii) metal centre together with rare NiH-C intra/intermolecular anagostic interactions in axial positions. In these complexes supramolecular structures have been sustained by non-covalent C-HO, C-OH-O, C-Hπ, C-Hπ (NiCS2, chelate), ππ and HH interactions. Their electrocatalytic properties have been investigated for oxygen evolution reaction (OER) in which complex 2 showed the highest activity with 10 mA cm-2 at the potential of 1.58 V vs. RHE. In addition, complex 2 also exhibits an OER onset potential at 1.52 V vs. RHE.

12.
Biosens Bioelectron ; 103: 113-129, 2018 Apr 30.
Artigo em Inglês | MEDLINE | ID: mdl-29289816

RESUMO

Introduction of novel functional nanomaterials and analytical technologies signify a foremost possibility for the advance of electrochemical sensor and biosensor platforms/devices for a broad series of applications including biological, biomedical, biotechnological, clinical and medical diagnostics, environmental and health monitoring, and food industries. The design of sensitive and selective electrochemical biological sensor platforms are accomplished conceivably by offering new surface modifications, microfabrication techniques, and diverse nanomaterials with unique properties for in vivo and in vitro medical analysis via relating a sensibly planned electrode/solution interface. The advantageous attributes such as low-cost, miniaturization, energy efficient, easy fabrication, online monitoring, and the simultaneous sensing capability are the driving force towards continued growth of electrochemical biosensing platforms, which have fascinated the interdisciplinary research arenas spanning chemistry, material science, biological science, and medical industries. The electrochemical biosensor platforms have potential applications in the early-stage detection and diagnosis of disease as stout and tunable diagnostic and therapeutic systems. The key aim of this review is to emphasize the newest development in the design of sensing and biosensing platforms based on functional nanomaterials for biological and biomedical applications. High sensitivity and selectivity, fast response, and excellent durability in biological media are all critical aspects which will also be wisely addressed. Potential applications of electrochemical sensor and biosensor platforms based on advanced functional nanomaterials for neuroscience diagnostics, clinical, point-of-care diagnostics and medical industries are also concisely presented.


Assuntos
Técnicas Biossensoriais/tendências , Técnicas Eletroquímicas/tendências , Nanoestruturas/química , Humanos , Sensibilidade e Especificidade
13.
J Oral Maxillofac Pathol ; 21(2): 317, 2017.
Artigo em Inglês | MEDLINE | ID: mdl-28932048

RESUMO

BACKGROUND: Ethanol has satisfactorily been used as cyto-fixative. Owing to its limitations, pathologists have always searched for new fixatives. The present study was conducted to evaluate the efficacy of two natural sweeteners as cyto-fixatives. An attempt has also been made to understand the underlying mechanism by which these fixatives fix the oral mucosal cells. MATERIALS AND METHODS: Three smears were collected from 25 healthy volunteers. One smear was fixed in ethanol and the other two in 20% aqueous honey solution and 30% aqueous jaggery solution for 15-30 min followed by Papanicolaou staining. Slides were evaluated for nuclear staining, cytoplasmic staining, cell morphology, clarity of staining and uniformity of staining randomly irrespective of the fixatives. Chi-square test and Bonferroni post hoc test were done using SPSS software. P < 0.05 was considered to be statistically significant. In addition, cytological fixatives were analyzed for the pH and amount of reducing sugars. RESULTS: It was found that for all the characteristics studied, no statistically significant difference was seen between the three fixatives. The pH of the both tested fixatives remained acidic even after 1 week. The amount of reducing sugars in 20% aqueous honey solution and 30% aqueous jaggery solution was 19.3 g/100 mL and 2.07 g/100 mL, respectively. CONCLUSION: Both the test fixatives gave results equivalent to ethanol and thus can be used as alternative fixatives for oral smears. It is proposed that 20% aqueous honey and 30% aqueous jaggery fix the oral smears satisfactorily in a mechanism akin to ethanol by coagulating and denaturing proteins.

14.
Sci Rep ; 7(1): 9407, 2017 08 24.
Artigo em Inglês | MEDLINE | ID: mdl-28839274

RESUMO

Replacing platinum (Pt) metal-based electrocatalysts used in the oxygen reduction reaction (ORR) in fuel cells is an important research topic due to the high cost and scarcity of Pt, which have restricted the commercialization of these clean-energy technologies. The ABO3-type perovskite family of an ACu3Ti4O12 (A = Ca, Y, Bi, and La) polycrystalline material can serve as an alternative electrocatalyst for the ORR in terms of low-cost, activity, and stability. These perovskite materials may be considered the next generation electro-catalyst for the ORR because of their photocatalytic activity and physical and chemical properties capable of containing a wide range of A- and B-site metals. This paper reports the ORR activity of a new Y2/3Cu3Ti4O12 perovskite, synthesized via a rapid and facile automatic flame synthesis technique using rotating disk electrode (RDE) measurements. Y2/3Cu3Ti4O12/C has superior ORR activity, stability, and durability compared to commercial Pt/C. The results presented in this article will provide the future perspectives to research based on ACu3Ti4O12 (A = Ca, Y, Bi, Sm, Cd, and La) perovskite as the next generation electro-catalyst for the ORR in various electrochemical devices, such as fuel cells, metal-air batteries, and electrolysis.

15.
Anal Chem ; 89(1): 776-782, 2017 01 03.
Artigo em Inglês | MEDLINE | ID: mdl-27966881

RESUMO

A simple, low cost and user-friendly method for the fabrication of paper electrode (PE) using silver nanoparticles capped with octylamine (AgNPs-OA) is reported for detection of hydrogen peroxide (H2O2) in wastewater samples. The PE was prepared by direct writing onto the photo paper using a ball-point pen filled with nanoink (10 wt % of AgNPs-OA in chloroform). The prepared electrode was sintered at 100 °C for 1 h to make it conductive. The PE/AgNPs-OA was used as a working electrode in cyclic voltammetry (CV) for the detection of H2O2. The PE/AgNPs-OA exhibited a wide linear calibration range from 1.7 µM to 30 mM for the determination of H2O2 with a low limit of detection, 0.5 µM. The good recovery percentage (95.2-96.2%) and interference study for determination of H2O2 in wastewater samples demonstrated the selectivity of the method from the complex sample matrices. The PE/AgNPs-OA electrode is found to be economic, facile and user-friendly for multiple analyses (n = 60) of H2O2 in CV compared to other commercially available electrodes and custom-made modified electrodes.

16.
Phys Chem Chem Phys ; 18(33): 23365-73, 2016 Aug 17.
Artigo em Inglês | MEDLINE | ID: mdl-27498920

RESUMO

Four polypyridyl redox catalysts Fe(bp)3(2+), Fe(ph)3(2+), Fe(dm)3(2+), and Fe(tm)3(2+) (with bp, ph, dm, and tm representing 2,2'-bipyridine, 1,10-phenanthroline, 4,4'-dimethyl-2,2'-bipyridine, and 3,4,7,8-tetramethyl-1,10-phenanthroline, respectively) are investigated for the electrocatalytic oxidation of three analytes (nitrite, arsenite, and isoniazid). The poly-pyridyl iron complex is exchanged into a Nafion film immobilized on a glassy carbon electrode, which is then immersed in 0.1 M Na2SO4. Cyclic voltammetry is employed for the evaluation of the mechanism and estimation of kinetic parameters. The electrocatalytic behaviour going from low to high substrate concentration is consistent with the Albery-Hillman cases of "LEty" switching to "LEk" (changing from the first order in the substrate to half order in the substrate), denoting a process that occurs in a reaction zone close to the electrode surface with diffusion of charge (from the electrode surface into the film) and of anionic or neutral analyte (from the Nafion-solution interface into the film). The relative hydrophobicity of the iron polypyridyl catalyst within the film is shown to affect both the diffusion of charge/electrons and analyte within the film with Fe(tm)3(2+) providing the mildest catalyst. All three analytes, nitrite, isoniazid, and arsenite, exhibit linear calibration ranges beneficial for analytical applications in the micro-molar to the milli-molar range.

17.
Bioelectrochemistry ; 101: 120-5, 2015 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-25260015

RESUMO

Fe(dmbpy)3(2+) (where dmbpy is 4,4'-dimethyl-2,2'-bipyridine) was immobilized by ion-exchange in a bentonite clay film coating on a glassy carbon electrode. Cyclic voltammetry characteristics of the immobilized Fe(dmbpy)3(2+) were stable and reproducible corresponding to the Fe(dmbpy)3(2+/3+) redox process. In the presence of isoniazid (IZ), the electrogenerated in film Fe(dmbpy)3(3+) oxidized IZ efficiently producing large anodic current. This current was linearly proportional to the IZ concentration in the solution. The process was described by an EC' electrocatalysis mechanism allowing for sensitive determination of IZ with a wide linear dynamic concentration range of 10.0µM to 10.0mM. The electrode was tested for its analytical suitability and possible discrimination of interferences by determining IZ in a commercially available pharmaceutical product. The paper reports on a simple, cheap, and easy to fabricate chronoamperometric chemical sensor for determination of IZ. Kinetic parameters, such as the catalytic rate constant (2.3×10(3)M(-1)s(-1)) and diffusion coefficient of IZ (5.42×10(-5)cm(2)s(-1)), were determined using CV, chronoamperometry, and chronocoulometry.


Assuntos
Técnicas Eletroquímicas/instrumentação , Técnicas Eletroquímicas/estatística & dados numéricos , Isoniazida/análise , Silicatos de Alumínio , Bentonita , Catálise , Argila , Eletrodos , Desenho de Equipamento , Cinética , Oxirredução , Piridinas/química , Reprodutibilidade dos Testes , Rifampina/química , Sensibilidade e Especificidade
18.
Carbohydr Polym ; 110: 388-95, 2014 Sep 22.
Artigo em Inglês | MEDLINE | ID: mdl-24906771

RESUMO

Graft copolymers based on dextran (Dx) and 2-acrylamido-2-methyl-1-propane sulphonic acid (AMPS) were synthesized by free radical initiated solution polymerization technique using ceric ammonium nitrate as initiator. These graft copolymers were used to prepare Cu(II) and Ni(II) chelates by reactions with Cu(II) and Ni(II) metal ions respectively. Graft copolymer and metal chelates were characterized by elemental analysis, intrinsic viscosity, FT-IR, scanning electron microscopy (SEM), atomic force microscopy (AFM), thermogravimetric analysis (TGA) and powder X-ray diffraction (XRD). Elemental analysis, intrinsic viscosity and FT-IR studies revealed the incorporation of metal ions to form metal chelates. SEM studies showed the change in morphology due to metal incorporation. From AFM studies it was observed that there was increase in Root mean square (RMS) roughness values in case of metal complexes. Metal chelates were observed to be thermally more stable than graft copolymer from TGA. UV-vis spectroscopy study revealed increase in absorbance values and cyclic voltammetric (CV) studies showed more than tenfold increase in redox current due to formation of Cu(II) and Ni(II) metal chelates. The binding constants of each complex determined by using UV-visible spectroscopy revealed that Cu(II) has more binding ability than Ni(II).


Assuntos
Acrilamidas/química , Quelantes/química , Cobre/química , Dextranos/química , Níquel/química , Ácidos Sulfônicos/química , Acrilamidas/síntese química , Quelantes/síntese química , Dextranos/síntese química , Técnicas Eletroquímicas , Metilação , Espectroscopia de Infravermelho com Transformada de Fourier , Ácidos Sulfônicos/síntese química , Viscosidade , Difração de Raios X
19.
Analyst ; 135(10): 2711-6, 2010 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-20714523

RESUMO

In this work, we report the fabrication and characterization of silver nanoelectrode ensembles (Ag-NEEs) on a glassy carbon electrode. For this purpose, Ag nanoparticles (NPs) were anchored to the mercaptopropyl functionalized MCM-41 type silica spheres utilizing the chemisorption property of Ag NPs by -SH groups. The successful anchoring of Ag NPs into the silica matrix is characterized by several techniques including UV-vis diffuse reflectance and X-ray powder diffraction methods. The surface morphology of the Ag-NEEs was assessed by scanning and transmission electron microscopy (SEM and TEM respectively). Further, nitrite (NO(2)(-)) is electrocatalytically oxidized at Ag-NEEs, which leads to a sensitive determination of NO(2)(-). The fabrication, characterization, and efficient sensing of NO(2)(-) at the Ag-NEEs are presented.


Assuntos
Técnicas Eletroquímicas/métodos , Nanopartículas Metálicas/química , Nitritos/análise , Prata/química , Óxido de Alumínio/química , Carbono/química , Eletrodos , Nanopartículas Metálicas/ultraestrutura , Oxirredução , Dióxido de Silício/química
20.
Chem Commun (Camb) ; 46(33): 6156-8, 2010 Sep 07.
Artigo em Inglês | MEDLINE | ID: mdl-20652181

RESUMO

Fe(bpy)(3)(2+) (where bpy = 2,2' bipyridyl) immobilized Nafion (Nf) modified glassy carbon electrodes were prepared and they showed excellent electrocatalytic oxidation of nitrite (NO(2)(-)) which leads to the sensitive determination of NO(2)(-). Electrostatic repulsion between NO(2)(-) and Nf film is greatly decreased when Nf film is fully exchanged with cations.


Assuntos
2,2'-Dipiridil/química , Polímeros de Fluorcarboneto/química , Compostos de Ferro/química , Nitritos/análise , Catálise , Eletrodos , Microscopia Eletrônica de Varredura , Oxirredução , Soluções , Eletricidade Estática , Propriedades de Superfície , Água/química
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