Differential pulse voltammetric simultaneous determination of ascorbic acid,dopamine and uric acid on a glassy carbon electrode modified with electroreduced graphene oxide and imidazolium groups

A glassy carbon electrode (GCE) was anodically oxidized by cyclic voltammetry (CV) in 0.05 M sulfuric acid to introduce hydroxy groups on its surface (GCE_ox). Next, an imidazolium alkoxysilane (ImAS) is covalently tethered to the surface of the GCE_ox via silane chemistry. This electrode is further modified with graphene oxide (GO) which, dispersed in water, spontaneously assembles on the electrode surface through electrostatic interaction and π-interaction to give an electrode of type GO/ImAS/GCE. Electroreduction of GO and GCE_ox by CV yields electroreduced GO (erGO) and an electrode of the type erGO/ImAS/GCE. This electrode displays excellent electrocatalytic activity for the oxidation of ascorbic acid (AA), dopamine (DA) and uric acid (UA). Three fully resolved anodic peaks (at ?50 mV, 150 mV and 280 mV vs. Ag/AgCl) are observed during differential pulse voltammetry (DPV). Under optimized conditions, the linear detection ranges are from 30 to 2000 μM for AA, from 20 to 490 μM for UA, and from 0.1 to 5 μM and from 5 μM to 200 μM (two linear ranges) for DA. The respective limits of detection (for an S/N of 3) are 10 μM, 5 μM and 0.03 μM. The GCE modified with erGO and ImAS performs better than a bare GCE or a GCE modified with ImAS only, and also outperforms many other reported electrodes for the three analytes. The method was successfully applied to simultaneous analysis of AA, DA and UA in spiked human urine.

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Graphical abstract Differential pulse voltammetric simultaneous determination of ascorbic acid, dopamine and uric acid is achieved on a glassy carbon electrode modified with electroreduced graphene oxide and imidazolium groups, through anodic treatment of glassy carbon and silane chemistry.

     

Determination of zearalenone with a glassy carbon electrode modified with nanocomposite consisting of palladium nanoparticles and a conductive polymeric ionic liquid

A glassy carbon electrode (GCE) modified with polymeric nanocomposite consisting of palladium nanoparticles and a conductive polymeric ionic liquid was prepared. The modified GCE was applied to sensitive and fairly selective electrochemical determination of the mycotoxin zearalenone. Electrocatalytic oxidation is performed in a solution containing 20 % (V/V) acetonitrile and 80 % (V/V) of 1 M perchloric acid. Cyclic voltammetry and square wave voltammetry revealed a well-defined electrocatalytic peak current at overpotential of +0.69 V versus Ag/AgCl. Under optimized experimental conditions, there is a linear relationship between anodic peak current and zearalenone concentration in the range from 0.03 to 35 ng?mL￣¹, and the detection limit is 0.01 ng?mL￣¹. The method was successfully applied to the analysis of zearalenone in spiked food samples and gave recoveries between 95.6 and 104.0 %.

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Graphical abstract The nanocomposite (PdVC-PIL) was prepared by polymerization of ionic liquid monomer (PIL) in presence of Pd nanoparticles on Vulcan XC-72R carbon (PdVC). The solution containing nanocomposite was placed on the glassy carbon electrode (GCE). The voltammetry activity of modified electrode (PdVC-PIL/GCE) was compared to a bare GCE for zearalenone determination.

     

Evaluation of a novel composite based on functionalized multi-walled carbon nanotube and iron phthalocyanine for electroanalytical determination of isoniazid

A novel platform for electroanalysis of isoniazid based on graphene-functionalized multi-walled carbon nanotube as support for iron phthalocyanine (FePc/f-MWCNT) has been developed. The FePc/f-MWCNT composite has been dropped on glassy carbon forming FePc/f-MWCNT/GC electrode, which is sensible for isoniazid, decreasing substantially its oxidation potential to +200 mV vs Ag/AgCl. Electrochemical and electroanalytical properties of the FePc/f-MWCNT/GC-modified electrode were investigated by cyclic voltammetry, electrochemical impedance spectroscopy, scanning electrochemical microscopy, and amperometry. The sensor presents better performance in 0.1 mol L^?1 phosphate buffer at pH 7.4. Under optimized conditions, a linear response range from 5 to 476 μmol L^?1 was obtained with a limit of detection and sensitivity of 0.56 μmol L^?1 and 0.023 μA L μmol^?1, respectively. The relative standard deviation for 10 determinations of 100 μmol L^?1 isoniazid was 2.5%. The sensor was successfully applied for isoniazid selective determination in simulated body fluids.     

Synthesis and characterization of manganese diselenide nanoparticles (MnSeNPs): Determination of capsaicin by using MnSeNP-modified glassy carbon electrode

A new type of manganese diselenide nanoparticles (MnSeNPs) was synthesized by using a hydrothermal method. Their surface morphology, crystallinity and elemental distribution were characterized by using transmission electron microscopy, X-ray diffraction, energy dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy which scrutinize the formation of the NPs. The NPs were coated on a glassy carbon electrode (GCE), and electrochemical impedance spectroscopy, cyclic voltammetry and differential pulse voltammetry were applied to study the electroanalytical properties towards the oxidation of the food additive capsaicin. The modified GCE displays lower charge transfer resistance (R _ct ?=?29.52 Ω), a larger active surface area (0.089 cm²/g, and more efficient electrochemical oxidation of capsaicin compared to a MnS₂/GCE and a bare GCE. The oxidation peak potential is 0.43 V (vs. Ag/AgCl) which is lower than that of previously reported GCEs. The sensor has a detection limit as low as 0.05 μM and an electrochemical sensitivity of 2.41 μA μM^?1 cm^?2. The method was applied to the determination of capsaicin in pepper samples.

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Graphical abstract Electrochemical determination of capsaicin in pepper extract by using MnSeNPs modified electrode.

     

Highly sensitive electrocatalytic determination of pyrazinamide using a modified poly(glycine) glassy carbon electrode by square-wave voltammetry

A new voltammetric sensor based on electropolymerization of glycine at glassy carbon electrode (GCE) was developed and applied to determine of pyrazinamide (PZA) by square-wave voltammetry (SWV). The initial cyclic voltammetric studies showed an electrocatalytic activity of poly(Gly)/GCE on redox system of pyrazinamide in 0.1 mol L^?1 phosphate buffer solution pH 7.5, with E _Pc and E _Pa in ?0.85 and ?0.8 V (versus E _Ag/AgCl), respectively. Studies at different scan rates suggest that the redox system of pyrazinamide at poly(Gly)/GCE is a process controlled by diffusion in the interval from 10 to 100 mV s^?1. Square-wave voltammetry-optimized conditions showed a linear response of PZA concentrations in the range from 0.47 to 6.15 μmol L^?1 (R?=?0.998) with a limit of detection (LOD) of 0.035 μmol L^?1 and a limit of quantification (LOQ) of 0.12 μmol L^?1. The developed SWV-poly(Gly)/GCE method provided a good intra-day (RSD?=?3.75 %) and inter-day repeatability (RSD?=?4.96 %) at 4.06 μmol L^?1 PZA (n?=?10). No interference of matrix of real samples was observed in the voltammetric response of PZA, and the method was considered to be highly selective for the compound. In the accuracy test, the recovery was found in the range of 98.2 and 104.0 % for human urine samples and pharmaceutical formulation (tablets). The PZA quantification results in pharmaceutical tablets obtained by the proposed SWV-poly(Gly)/GCE method were comparable to those found by official analytical protocols.     

Application of graphene oxide nanosheets as probe oligonucleotide immobilization platform for DNA sensing

In this work, a simple and novel electrochemical biosensor based on a glassy carbon electrode (GCE) modified with graphene oxide nanosheets (GO) was developed for detection of DNA sequences. The morphology of prepared nanoplatform was investigated by scanning electron microscopy, infrared (FTIR) and UV/Vis absorption spectra. The fabrication processes of electrochemical biosensor were characterized with cyclic voltammetry and electrochemical impedance spectroscopy (EIS) in an aqueous solution. The optimization of experimental conditions such as immobilization of the probe BRCA1 and its hybridization with the complementary DNA was performed. Due to unique properties of graphene oxide nanosheets such as large surface area and high conductivity, a wide liner range of 1.0 × 10^?17–1.0 × 10^?9 M and detection limit of 3.3 × 10^?18 M were obtained for detection of BRCA1 5382 mutation by EIS technique. Under the optimum conditions, the proposed biosensor (ssDNA/GO/GCE) revealed suitable selectivity for discriminating the complementary sequences from non-complementary sequences, so it can be applicable for detection of breast cancer.     

Electrochemical sensing of <Emphasis Type="SmallCaps">D</Emphasis>-penicillamine on modified glassy carbon electrode by using a nanocomposite of gold nanoparticles and reduced graphene oxide

A new electrochemical sensor was developed for determination of D-penicillamine using glassy carbon electrode which had been modified by gold nanoparticles–reduced graphene oxide nanocomposite (AuNPs/RGO/GCE) in aqueous solution. Cyclic voltammetry, transmission electron microscopy and electrochemical impedance spectroscopy were used for characterization of the modified electrode. The results indicated that the kinetic of oxidation reaction of D-penicillamine at the surface of the electrode was controlled by both diffusion and adsorption processes. In 0.1 mol L^?1 phosphate buffer (pH 2.0), the oxidation current increased linearly with concentration of D-penicillamine with a linear range of 5.0 × 10^?6 to 1.1 × 10^?4 mol L^?1 and regression coefficient of R ² = 0.9972. Theoretical detection limit, defined based on 3σ of the blank signal (n = 9) divided by the slope of the linear regression equation, was 3.9 × 10^?6 mol L^?1 D-penicillamine using differential pulse voltammetry. The developed method was successfully applied to the determination of D-penicillamine in pharmaceutical formulation and blood serum samples.     

A glassy carbon electrode modified with graphene oxide decorated silver phosphate nanodentrites for amperometric determination of dissolved hydrazine

The authors describe an electrochemical approach for the preparation of a glassy carbon electrode (GCE) modified with graphene oxide and silver nanodentrites (AgNDs). The coating was obtained by using an aqueous solution containing silver nitrate, phosphate and ammonia. The phosphate anions act as a scaffold for the improved deposition of AgNDs. The effects of deposition potential and time and concentration of electrolyte on the formation of the AgNDs were optimized. The modified GCE displays good electrocatalytic activity towards the oxidation of dissolved hydrazine. The electron transfer coefficient and diffusion coefficient are 0.60 and 4.64 × 10^?5 cm² s^?1 respectively. The electrode exhibits a linear response over the 100 nM to 670 μM hydrazine concentration range and a detection limit (LOD) of 33 nM. The sensitivity of the modified electrode is 2077 μA mM^?1 cm^?2 at a typical working voltage of 0.1 V (vs Ag/AgCl). This LOD is much lower than that of the allowable concentration of hydrazine in drinking water as defined by the US EPA and the WHO.

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Graphical abstract Schematic of the 2-step fabrication of a glassy carbon electrode (GCE) modified with graphene oxide (GO) and silver nanodendrites (AgND) for use in a hydrazine sensor. First, Ag₃PO₄ is formed by adding AgNO₃ and phosphate. Secondly, the formed Ag₃PO₄ is converted to a colorless complex by adding ammonia and by electrolytic growth of AgND on the GO/GCE.

     

<Emphasis Type="Italic">cis</Emphasis>-Dioxomolybdenum(VI) complexes of sterically encumbered phenol-based tetradentate N<Subscript>2</Subscript>O<Subscript>2</Subscript> ligands: Structural,spectroscopic, and electrochemical studies

Two cis-dioxomolybdenum(VI) complexes [MoO₂L] (L: L ¹, 2 and L: L ², 3) in a phenol-based sterically encumbered N₂O₂ ligand environment have been synthesized, and their crystallographic characterizations are reported. The orange crystals of 2 are monoclinic, space group P2₁/a with unit cell dimensions as a=16.2407(17) Å, b=7.2857(8) Å, c=18.400(2) Å, β=98.002(9)°, Z=4, and d _cal=1.486 g cm^?3. The light orange crystals of 3, however, are orthorhombic, space group, Pbcn, with unit cell dimensions a=8.3110(12) Å, b=12.637(3) Å, c=34.673(5) Å, Z=4, and d _cal=1.187 g cm^?3. The structures were refined by a full-matrix least-squares procedure on F ² to a final R=0.046 (0.055 for 3) using 4944 (3677) all independent data. In both the cases, the Mo atom exists in a distorted octahedral geometry defined by a N₂O₄ donor set, which features a cis-Mo(–O)₂ and a trans-Mo(OPh)₂ arrangement. Compound 2 undergoes a quasireversible one-electron reduction at ?1.3 V vs Ag/AgCl reference due to Mo^VIO₂/Mo^VO₂ electron transfer and thus providing a rare example of steric solution to the comproportionation–dimerization problem encountered frequently in the development of valid biomimetic models for the active sites of oxomolybdenum enzymes.     

Ag nanoparticles decorated Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>/chitosan nanocomposite: synthesis,characterization and application toward electrochemical sensing of hydrogen peroxide

We studied a rapid, sensitive and selective amperometric sensor for determination of hydrogen peroxide by electrodeposited Ag NPs on a modified glassy carbon electrode (GCE). The modified GCE was constructed through a step by step modification of magnetic chitosan functional composite (Fe₃O₄–CH) and high-dispersed silver nanoparticles on the surface. The resulted Ag@Fe₃O₄–CH was characterized by various analytical methods including Fourier transform infrared spectroscopy, X-ray diffraction, transmission electron microscopy, scanning electron microscopy and cyclic voltammetry. The proposed sensor employed Ag@Fe₃O₄–CH/GCE as the working electrode with a linear current response to the hydrogen peroxide concentration in a wide range from 0.01 to 400 µM with a low limit of detection (LOD = 0.0038 µM, S/N = 3). The proposed sensor showed superior reproductivity, sensitivity and selectivity for the detection of hydrogen peroxide in environmental and clinical samples.     

A one-dimensional silver(I) coordination polymer with saccharin and pyrazine: synthesis,crystal structure,thermal analysis,FTIR spectra,and DFT studies

A silver(I) complex of saccharinate (sac) with pyrazine (pyz), [Ag(sac)(pyz)] _n , has been synthesized and characterized by elemental analysis, IR, thermal analysis, and single-crystal X-ray diffractometry. The complex crystallizes orthorhombic space group Pnma with unit cell parameters of a = 13.0073(9) Å, b = 6.4907(6) Å, c = 13.4007(9) Å, V = 1131.37(15) Å³, and Z = 4. [Ag(sac)(pyz)] _n is a one-dimensional coordination polymer, in which the sac ligand acts as a monodentate ligand through the N atom and the trigonal silver centers are linked by the bridging pyz ligands. The individual chains are connected into two-dimensional supramolemular network by aromatic π(sac)···π(pyz) stacking interactions. The FTIR spectrum of [Ag(sac)(pyz)] _n has been recorded in the region and 4,000–400 cm^?1. The optimized geometry, frequency, and intensity of the vibrational bands of [Ag(sac)(pyz)] _n were obtained by density functional theory (DFT) at the B3LYP level. The vibrational frequencies were calculated and the scaled values have been compared with the experimental FTIR data. The observed and calculated frequencies are found to be in good agreement.     

Glassy carbon electrode modified with poly-Neutral Red for photoelectrocatalytic oxidation of NADH

A new approach is described for the photoelectrocatalytic oxidation of Reduced ß-Nicotinamide Adenine Dinucleotide (NADH). It is based on a glassy carbon electrode (GCE) modified with a film of poly-Neutral Red (poly-NR) that is obtained by electropolymerization. Electrochemical measurements revealed that the modified electrode displays electrocatalytic and photo-electrocatalytic activity towards oxidation of NADH. If irradiated with a 250-W halogen lamp, the electrode yields a strongly increased electrocatalytic current compared to the current without irradiation. Amperometric and photo-amperometric detection of NADH was performed at +150 mV vs. Ag/AgCl/KCl_sat and the currents obtained are linearly related to the concentration of NADH. Linear calibration plots are obtained in the concentration range from 1.0 μM to 1.0 mM for both methods. However, the slope of the current-NADH concentration curve of the photo-electrocatalytic procedure was 2-times better than that obtained without irradiation.

Silver-based coordination complexes of carboxylate ligands: crystal structures,luminescence and photocatalytic properties

The complexes [Ag₄(dpe)₄]·(btec) (1) and [Ag₄(bpy)₄]·(btec)·12H₂O (2) (dpe = 1,2-di(4-pyridyl)ethylene, bpy = 4,4′-bipyridine, H₄btec = 1,2,4,5-benzenetetracarboxylic acid) have been synthesized in aqueous alcohol/ammonia by slow evaporation at room temperature and characterized by elemental analysis, single-crystal X-ray diffraction, FTIR, UV–Vis and luminescence spectroscopies. Both complexes are composed of 1D infinite cationic [Ag/dpe(bpy)] _n ⁿ⁺ chains and discrete btec^4? anions. Their three-dimensional supramolecular structures are built up of cationic sheets formed from [Ag/dpe(bpy)] _n ⁿ⁺ units via weak Ag…Ag and Ag…N interactions, plus anionic btec^4? sheets featuring electrostatic, π–π and hydrogen bonding interactions. Both complexes exhibited photocatalytic activity for the decomposition of methyl orange under UV light irradiation.     

Amperometric determination of the insecticide fipronil using batch injection analysis: comparison between unmodified and carbon-nanotube-modified electrodes

The electrochemical oxidation of fipronil is investigated on unmodified and multi-walled carbon-nanotube (MWCNT)-modified glassy carbon electrodes (GCEs), and its amperometric determination using batch injection analysis (BIA) is demonstrated. An oxidation peak was observed at 1.5 V in a 0.1 mol L^?1 HClO₄/acetone solution (50:50, v/v) on both surfaces. Although MWCNT-modified GCE provided greater sensitivity, the unmodified GCE showed low RSD value, wider linear range, and reduced adsorption of fipronil or its oxidized products on the electrode surface. A detection limit of 4.7 μmol L^?1 and linear range of 25–300 μmol L^?1 were obtained using a bare GCE. The method was applied in veterinary formulations with results in agreement with those obtained by high-performance liquid chromatography.     

Cetyltrimethylammonium bromide assisted self-assembly of phosphotungstic acid on graphene oxide nanosheets for selective determination of tryptophan

A one-step method was developed to prepare cetyltrimethylammonium bromide (CTAB) and phosphotungstic acid (PTA)-modified graphene oxide (GO) (PTA/CTAB/GO). In a system containing CTAB, GO, and PTA, negatively charged GO forms stable complex with positively charged CTAB, which assembled on the GO nanosheet surface. And then, with CTAB molecules as the molecular linker, PTA was loaded on CTAB/GO hybrid by electrostatic interaction. The PTA/CTAB/GO was characterized with Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM) and subsequently used in the construction of tryptophan (Trp) sensor. Compared with the CTAB/GO, PTA/CTAB/GO exhibits better electrocatalytic activity towards the oxidation of Trp, which is attributed to the synergistic effect of PTA and GO. The differential pulse voltammetry (DPV) curve of Trp at PTA/CTAB/GO/glassy carbon electrode (GCE) exhibited two linear dynamic ranges with a detection limit of 0.02 μM (S/N = 3). In addition, the proposed sensor is successfully employed to detect Trp in the real samples with satisfactory results.     

Synthesis,experimental and theoretical characterization,and antimicrobial studies of some Fe(II), Co(II), and Ni(II) complexes of 2-(4,6-dihydroxypyrimidin-2-ylamino)naphthalene-1,4-dione

The work reported the synthesis and characterisation of Fe²⁺, Co²⁺, and Ni²⁺ complexes of 2-(4,6-dihydroxypyrimidin-2-ylamino)naphthalene-1,4-dione (HL). The spectroscopic and elemental analysis results obtained were consistent with the adoption of the formulas, [ML₂] (M = Fe and Co) and [ML₂(H₂O)] (M = Ni) for the metal complexes. Electronic spectra and magnetic moments of the metal complexes corroborated octahedral geometry for Ni(II) complex and tetrahedral geometry for Fe(II) and Co(II) complexes. However, quantum-chemical calculations using density functional theory predicted trigonal bipyramidal geometry for Ni(II) complex and provided corroborative explanations for the structures of the other complexes. Conductance measurements in dimethylsulfoxide indicate that the complexes are non-electrolytes. The antimicrobial potential of the compounds was evaluated against Staphylococcus aureus, Pseudomonas aeruginosa, Escherichia coli, Bacillus cereus, Proteus mirabilis, Klebsiella oxytoca, Aspergillus niger, A. flavus, and Rhizopus stolonifer. The compounds gave moderate to good antimicrobial activity. However, the bacterial and fungal organisms were more susceptible to the cobalt complex and ligand respectively than the other compounds at concentration of 10 mg/mL. The compounds were also assessed for their antioxidant potential using 1, 1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging assay. The compounds displayed good DPPH radical scavenging activities. The nickel complex exhibited the best DPPH radical scavenging activity compared to the other compounds.     

Titanium dioxide anchored graphene oxide nanosheets for highly selective voltammetric sensing of dopamine

The authors report on an efficient method for the voltammetric sensing of dopamine (DA) by using an electrode modified with alternating monolayers of graphene oxide (GO) and Titanium dioxide (TiO₂) nanoparticles anchored GO nanosheets (NSs)). The as-prepared nanostructures were characterized by photoluminescence spectroscopy, powder X-ray diffraction, Raman spectroscopy, FT-IR spectroscopy, transmission electron microscopy, scanning electron microscopy, atomic force microscopy and Energy Dispersive X-ray Analysis (EDAX) techniques. The GO/TiO₂ nanocomposite (NC) was deposited on a glassy carbon electrode (GCE), where it displayed an excellent electrocatalytic activity toward the oxidation of DA, owing to its excellent conductivity, high specific surface area, enhanced interfacial contact and more negative zeta potential. Figures of merit include (a) a fast response (5 s), (b) a wide linear range (between 0.2 and 10 μM of DA) (c) a particularly low detection limit (27 nM), (d) a working potential as low as 0.25 V (vs. Ag/AgCl) and (e) a sensitivity of 1.549 μA·μM^?1·cm^?2. The GO/TiO₂/GCE exhibited excellent selectivity over the other interferences as revealed by the differential pulse voltammetric and amperometric studies. The analysis of spiked urine samples resulted in recoveries in the range of 96 to 106%, with RSDs between 3.8 and 5.2%.

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Graphical abstract A GO/TiO₂ (graphene oxide/titanium dioxide) nanocomposite (NC) was prepared and exploited as electrochemical probes in DA detection. It displays a low detection limit, wide linear range and excellent selectivity.

     

Determination of prazosin in pharmaceutical samples by flow injection analysis with multiple-pulse amperometric detection using boron-doped diamond electrode

This work describes the development of a simple, fast and low-cost method for determining prazosin (PRA) in pharmaceutical samples by flow injection analysis with multiple-pulse amperometric (FIA-MPA) detection using a boron-doped diamond film electrode. Electrochemical detection of PRA was optimized in phosphate buffer pH 4.0 by cyclic voltammetry, in which PRA presented two oxidation processes around at 0.97 and 1.40 V versus Ag/AgCl (3.0 mol L^?1 KCl). In these conditions, PRA also showed one reduction process at ?0.75 V that is dependent on the oxidation processes. Thus, the determination of PRA by FIA-MPA detection consisted on the application of a two-potential waveform, E ₁ (generator potential)?=?1.6 V/400 ms and E ₂ (collector potential)?=??1.0 V/30 ms, with sample loop of 150 μL and flow rate of 3.0 mL min^?1. The method showed good repeatability (RSD?<?3.0 %) and high analytical frequency (70 injections per h). The working linear range was obtained from 2 to 200 μmol L^?1 with a limit of detection of 0.5 μmol L^?1. The recovery tests in all samples were approximately 100 %, and the results were compared with chromatographic methods.     

Electrochemical synthesis of metal nanoparticles using a polymeric mediator,whose reduced form is adsorbed (deposited) on an electrode

Efficient mediated electrosynthesis of nanocomposite Au@р(MVCA⁸⁺-co-St) (~6 nm), in which ultrasmall Au nanoparticles (Au-NP) were bound in nanocapsules of water-soluble nanoparticles of соpolymer р(MVCA⁸⁺-co-St) of tetraviologen calix[4]resorcinol (MVCA⁸⁺) with styrene (St), was accomplished by the reduction of Au^I in aqueous medium. The quanti- tative reduction of Au^I was carried out using the theoretically necessary amount of electricity and was not accompanied by the deposition of metal on the electrode. Radical cations of viologen units MV^?+ of the molecule р(MVCA^4?+-co-St) adsorbed on the electrode and π-dimers MV^?+···MV^?+ of π-polymers [р(MVCA^4?+-co-St)] _n deposited on the electrode act- ed as the reducing agents with respect to Au^I. During electrolysis, the nanoparticles agglo- merated to 37—50 nm. The nanocomposite particles dispersed in ethanol had sizes of 72±16 nm and also contained Au-NP with sizes of 51±8 and 19±3 nm. The catalytic activity of the nanocomposite in the reduction of p-nitrophenol with sodium borohydride was demon- strated. A similar reduction of AgCl nanoparticles (~250 nm) led to the formation of silver nanoparticles with crystallite sizes in the range of 7—11 nm, the process was inefficient, however, even when using 250% of electricity, an incomplete reduction of AgCl was still observed.     

Electrochemical determination of dopamine and uric acid using a glassy carbon electrode modified with a composite consisting of a Co(II)-based metalorganic framework (ZIF-67) and graphene oxide

A composite was prepared from a Co(II)-based zeolitic imidazolate framework (ZIF-67) and graphene oxide (GO) by an in situ growth method. The material was electrodeposited on a glassy carbon electrode (GCE). The modified GCE was used for the simultaneous voltammetric determination of dopamine (DA) and uric acid (UA), typically at working potentials of 0.11 and 0.25 V (vs. SCE). The morphology and structure of the nanocomposite were characterized by scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy and X-ray diffraction. The modified electrode exhibits excellent electroanalytical performance for DA and UA owing to the synergistic effect of the high electrical conductivity of GO and the porosity of ZIF-67. By applying differential pulse voltammetry, a linear response is found for DA in the 0.2 to 80 μM concentration range, and for UA between 0.8 and 200 μM, with detection limits of 50 and 100 nM (at S/N =?3), respectively. Further studies were performed on the effect of potential interferents, and on electrode stability and reproducibility. The modified GCE was applied to the simultaneous detection of DA and UA in spiked human urine and gave satisfying recoveries.

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Graphical abstract Schematic of the preparation procedure of GO-ZIF67 and electrochemical reaction mechanisms of UA and DA at the GO-ZIF67-modified glassy carbon electrode (GCE). GO: graphene oxide; ZIF-67: Co(II)-based zeolitic imidazolate framework.