ABSTRACT
In the present work,a chemically modified electrode has been fabricated utilizing Bi2O3/ZnO nano-composite.The nanocomposite was synthesized by simple sonochemical method and characterized for its structural and morphological properties by using XRD,FESEM,EDAX,HRTEM and XPS techniques.The results clearly indicated co-existence of Bi2O3 and ZnO in the nanocomposite with chemical interaction between them.Bi2O3/ZnO nanocomposite based glassy carbon electrode(GCE)was utilized for sensitive voltammetric detection of an anti-biotic drug(balofloxacin).The modification amplified the electroactive surface area of the sensor,thus providing more sites for oxidation of analyte.Cyclic and square wave voltammograms revealed that Bi2O3/ZnO modified electrode provides excellent electrocatalytic action towards balofloxacin oxidation.The current exhibited a wide linear response in concentration range of 150-1000 nM and detection limit of 40.5 nM was attained.The modified electrode offered advantages in terms of simplicity of preparation,fair stability(RSD 1.45％),appreciable reproducibility(RSD 2.03％)and selectivity.The proposed sensor was applied for determining balofloxacin in commercial pharmaceutical formulations and blood serum samples with the mean recoveries of 99.09％and 99.5％,respectively.
ABSTRACT
Objective: The aim of this study was to develop a simple, reliable voltammetric method and its validation for determination of nonsteroidal anti-inflammatory drug diclofenac (DFC). Methods: The proposed method was based on electro-oxidation of DFC at poly (erichrome black T) modified glassy carbon electrode (PEBT/GCE) in 0.2 M phosphate buffer solution of pH 7.0. Cyclic voltammetry and differential pulse voltammetric techniques were employed to study electro-oxidation behavior. Under the optimal conditions, variations of EBT concentration, effect of pH, scan rate on the oxidation of DFC was studied. Results: A well-defined oxidation peak at about +0.59 V vs. standard calomel electrode was observed for voltammetric detection of DFC. pH effect shows the participation of an equal number of protons and electrons in the mechanism. The relation between a logarithm of peak current with the logarithm of scan rate indicated adsorption controlled behavior of electrode process. Concentration variations show a good linear response in the range 0.05 µM to 40 µM with the detection limit of 5.25 × 10-8 M. Conclusion: The prepared sensor exhibited good selectivity, sensitivity, and stability for the detection of DFC in the pharmaceutical dosage form and real samples. The developed method could possibly be adopted for pharmacokinetic studies and also in clinical and quality control laboratories where time and economy were important.
ABSTRACT
MnO2nanowires-reduced graphene oxide composite (MnO2-RGO) was used to modify glassy carbon electrodes (GCE) and applied for the electrochemical determination of dopamine (DA). The microstructure of MnO2nanowires and MnO2-RGO nanocomposite material was characterized by scanning microscope and X-ray powder diffraction. Then the electrochemical reduction condition for preparing MnO2-RGO/GCE and experimental conditions for determining DA were optimized systematically. The electrochemical behavior of DA on the bare electrode and RGO or MnO2-RGO modified electrodes was also investigated in pH 3.5 phosphate buffer solution (PBS) by cyclic voltammetry. The results shows that the oxidation peaks of ascorbic acid (AA), dopamine (DA) and uric acid (UA) can be well separated and the peak to peak separations were 268 mV (AA-DA) and 128 mV (DA-UA), respectively. Moreover, the linear response ranges for the determination of DA were 0.06-1.0 μmol/L and 1.0-80 μmol/L with the detection limit of 1.0 nmol/L (S/N=3). The proposed method has been applied to the determination of dopamine in human blood serum sample with satisfactory results.
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ABSTRACT A new modified electrode for indirect sensing of OH· and radical scavengers was described. The electrochemical polymerization of methylene blue in aqueous solutions and the properties of the resulting films on a glassy carbon electrode were carried out using cyclic voltammetry. A surface coverage of 1.11 × 109mol cm2 was obtained, revealing a complete surface coverage of the polymeric film on the electrode surface. OH· was able to destroy the poly(methylene blue) film by exposure to a Fenton solution. The loss of the electrochemical signal of the residual polymeric film attached to the electrode surface was related to the extent of its dissolution. The applicability of the sensor was demonstrated by evaluating the OH radical scavenging effect on different concentrations of ascorbic acid. The obtained radical scavenging capacity were 31.4%, 55.7%, 98.9% and 65.7% for the ascorbic acid concentrations of 5, 10, 30 and 50 mM, respectively.
Subject(s)
Free Radical Scavengers/chemistry , Methylene Blue/chemistry , Structure-Activity Relationship , Electrodes , Electrochemical TechniquesABSTRACT
La propiedad electroactiva de hidroquinona (HQ) se estudió sobre un electrodo de carbono vítreo modificado con quitosano, nanotubos de carbono de pared múltiple (Ch-MWCNT-GCE). La HQ se depositó a un potencial controlado sobre la superficie del electrodo y la oxidación de la HQ se midió por voltametría de onda cuadrada (SWV, por sus siglas en inglés). Se observó una corriente de oxidación a 0,39 V y una corriente de reducción a 0,21 V con un ΔV de 0,18 V; ello indicó un proceso reversible. Un aumento en las corrientes de oxidación y de reducción de casi 50% se observó cuando el Ch-MWCNT-GCE se recubrió con líquido iónico (LI). El electrodo se caracterizó por voltamperometría cíclica (CV, por sus siglas en inglés) en presencia y sin la presencia de diferentes líquidos iónicos con distinto anión, siendo el más óptimo el líquido iónico (LI) 1-butil-3-metilimidazolio hexafluorofosfato (BMIMPF6). Se estudiaron las variables experimentales como pH, tiempo de adsorción (t ads) y potencial de adsorción (Eads), así como también las potenciales interferencias. Bajo las óptimas condiciones (pH 3,0; t acc 60s; Eacc 0,10 V), el pico de la corriente es proporcional a la concentración de HQ entre 4,20 * 10-6 y 30,0 * 10-6 mol L-1, con un límite de detección de 2,45 * 10-7 mol L-1. La desviación estándar relativa para una solución que contiene 1,0 * 10-4 mol L-1 de HQ, fue de 1,5% para siete medidas iguales. El método se validó con una muestra de agua dopada con HQ.
Property of the electroactive hydroquinone (HQ) was studied on a glassy carbon electrode modified chitosan, multi wall carbon nanotubes (Ch-MWCNT-GCE). HQ is deposited at a controlled potential to the electrode surface and oxidation of HQ is measured by square wave voltammetry (SWV). An oxidation current to 0.39 V and a reduction current to 0.21 V with a 0.18 ΔV indicating a reversible process were observed. An increase in the flow of oxidation and reduction of almost 50% was observed when the Ch-MWCNT-GCE was coated with ionic liquid (LI). The electrode was characterized by cyclic voltammetry (CV) in the presence and without the presence of different ionic liquids with different anion being the most optimal ionic liquid (LI) 1-butyl-3-methyllimidazolio hexafluorophosphate (BMIMPF6). Experimental variables such as pH, adsorption time (TADs) and adsorption potential (Eads), as well as potential interference, were studied. Under optimal conditions (pH 3.0; t acc 60s; Eacc 0.10 V) the peak current is proportional to the concentration of HQ between 4.20 * 10-6 and 30.0 * 10-5 mol L-1 with a detection limit of 2.45 * 10-7 mol L-1. The relative standard deviation for a solution containing 1.0 * 10-4 mol L-1 HQ was 1.5% for seven equal measures. The method was validated with a water sample doped with HQ.
ABSTRACT
ZnO nanotubes were prepared via electrospinning the Zn ( AC ) 2-polyacrylonitrile-polyvinylpyrrolidone ( PAN-PVP) precursor, followed by thermal decomposition of the above polymers from the precursor fibers. SEM and XRD characterization confirmed that the as-prepared ZnO nanofibers presented the hollow nanotube form, which was composed of ZnO nanoparticles with the size of about 40 nm in wurtzite crystal structure. By mixing with graphene, the obtained ZnO-graphene composite modified glassy carbon electrode ( ZnO-RGO/GCE ) was successfully constructed by dip-coating, which was used for the determination of Pb2+in water. With the sensitive response of the ZnO-RGO/GC electrode to Pb2+in solution was demonstrated by square wave stripping voltammetry, the response pctential was at -0. 4V. Under the optimized conditions, a good linear relationship between peak current and Pb2+ concentration was obtained in the range of 2. 4×10-9-4. 8×10-7 mol/L (R=0. 9970) by 10 min preconcentration at -1. 0 V in 0. 1 mol/L HAc-NaAc buffer solution (pH=4. 6). The detection limit was 4. 8×10-10 mol/L (S/N>3). The ZnO-RGO/GC electrode had good stability. The practical analytical application of the ZnO-RGO modified electrode was assessed by the measurement of the actual water sample and the result was consistent with that obtained by ICP-MS.
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A multi-walled carbon nanotube (MWCNT)-cetyltrimethylammonium bromide (CTAB) surfactant composite modified glassy carbon electrode (GCE) was developed as a novel system for the determination of 4-aminoantipyrine(AAP). The oxidation process was irreversible over the pH range studied and exhibited a diffusion controlled behavior. All experimental parameters were optimized. The combination of MWCNT-CTAB endows the biosensor with large surface area, good biological compatibility, electricity and stability, high selectivity and sensitivity. MWCNT-CTAB /GCE electrode gave a linear response for AAP from 5.0 × 10-9 to 4.0 × 10-8 M with a detection limit of 1.63 × 10-10 M. The modified electrode showed good selectivity against interfering species and also exhibited good reproducibility. The present electrochemical sensor based on the MWCNT-CTAB/GCE electrode was applied to the determination of AAP in real samples.
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Through a series of chemical reactions, a kind of quaternary ammonium salt derivative of nanodiamond, ND-CO-NH-CH2-CH2-N ( CH3 ) 3+· I-( QAS-ND ) , was obtained , which was confirmed by FTIR, element analysis experiment and the electrochemistry measurements. Mixed myoglobin ( Mb) and QAS-ND solution was dropped on the surface of the glassy carbon ( GC ) electrode to prepare QAS-ND/Mb/GC modified electrode. In 0. 1 mol/L phosphate buffer solution (PBS) (pH 7. 0), Mb in the membrane exhibited direct electrochemical properties and showed good stability. The electrocatalytic property of the modified electrode toward H2 O2 was investigated, the results showed that the modified electrode could be used as the H2O2 biosensor to achieve fast, accurate detection of H2O2, with a detection limit of 3. 5 mmol/L (S/N=3).
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Anelectrochemicallyreducedgrapheneoxide/goldnanoparticle-chitosan(ERGO/AuNP-CS) composite film modified glassy carbon electrode ( GCE) was constructed by directly electrochemical reduction of GO, and then assembly of AuNP-CS polycation on the surface. The surface morphologies of different modified electrodes including bare GCE, GCE/GO, GCE/ERGO and GCE/ERGO/AuNP-CS were characterized by scanning electron microscopy ( SEM ) . The differential pulse voltammetric behaviors of the electrodes were investigated, and the results indicated that the composite of ERGO/AuNP-CS exhibited excellent electrocatalytic oxidation activity to uric acid ( UA) molecule. In 0. 10 mol/L of phosphate buffer solution (pH=6. 5) with a scanning rate of 100 mV/s, the proposed composite film modified electrode showed a linear electrochemical response to UA in the range of 0 . 05-110 μmol/L with a detection limit of 12. 4 nmol/L ( S/N = 3 ). The electrode displayed good selectivity, reproducibility and stability in the determination of UA in human serum and urine samples with a recovery of 93 . 8%-104 . 1%. The detection results were agreed with those of conventional spectrophotometry and uricase Kit methods.
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A ZnO nanofibers carrier on the Pt electrode via electrospinning technology was prepared and then the Keggin phosphotungstic acid was deposited on the ZnO/Pt electrode using electrodeposition technology. The scanning electron microscopy showed that the zinc oxide fibers presented net structure and the diameter of its fiber was about 300 nanometers. The fourier transform infrared spectroscopy confirmed that the phosphotungstic acid adhered to the fiber surface. The electrochemical property of the modified electrode showed that it exhibited rapid response, excellent sensitivity and good stability, achieving rapid and accurate determination. The electrode responded linearly to ascorbic acid ( AA) in a concentration range from 8. 8 × 10-7 to 3. 3 × 10-4 mol/L with a low detection limit of 2. 5 × 10-7 mol/L. The method is promising for the development of AA detecting instrument.
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The silver doped poly ( L-lysine ) modified glassy carbon electrode was fabricated by cyclic voltammetry, the surface of the electrode was characterized by scanning electron microscopy and electrochemical impedance spectroscopy. The electrochemical behaviors and the simultaneous detection of xanthine and uric acid were studied by cyclic voltammetry and differential pulse voltammetry. The results indicated that this modified electrode exhibited excellent electrocatalytic activity towards the oxidation of xanthine and uric acid. The stable oxidation peaks of xanthine and uric acid appeared with the peak potential of 0. 980V and 0. 600V respectively at the modified electrode in pH 3. 0 phosphate buffer solution. The oxidation peaks of xanthine and uric acid were separated at 380 mV. Under the optimum conditions, the linear ranges for the determination of xanthine and uric acid were 1 . 00 × 10-6-2 . 50 × 10-4 mol/L respectively by differential pulse voltammetry. The detection limits were 5. 0×10-7mol/L. The method has been applied to the simultaneous detection of xanthine and uric acid in healthy human urine with satisfactory results.
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A novel hydrogen peroxide sensor was fabricated by the seed-mediated growth method. First, polyethyleneimine(PEI) functionalized multiwalled carbon nanotubes(MWNTs) were used as growth scaffold on the glass carbon electrode ( GCE). Then, Au nanoparticles were electrodeposited uniformly as seeds. Finally, Pt nanoparticles ( PtNPs ) grew on Au nanoparticles to form Pt @ Au core-shell structure nanocomposite. A new type of electrochemical sensor based on Pt @ Au / PEI-MWNTs nanocomposites for detection of hydrogen peroxide was developed, and the designed Pt@ Au / PEI-MWNTs/ GCE was characterized by electrochemical methods and field emission scanning electron microscopy (FESEM). The Differential pulse experimental results showed that the modified electrode exhibited excellent electrocatalytic activity towards the reduction of H2 O2 with the wide linear range from 9. 2 ×10-8 mol/ L to 1. 3 ×10-3 mol/ L. The correlation coefficient was 0. 9994 and the low detection limit was 3. 1×10-8 mol/ L at the signal-to-noise of 3.
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Praseodymium hexacyanoferrate film was modified on the graphite electrode by cyclic voltammetry in the solution of PrCl_3 and K_3Fe(CN)_6. Its electrochemical properties, including the influence of different scan rates, ions, and K~+ concentrations on the film, were studied. The membrane was characterized by IR and XPS. In IR spectrum, the vibration of cyano group verified from the formation of the film on the electrode. In XPS spectrum, the splitting of Fe2p_(1/2) )and Fe2p_(3/2)) showed that the valence of iron has been changed in the film formation, and a proper electropolymerization mechanism was put forward. The results showed the PrHCF film have some electrocatalytic activity to the oxidation of cysteine. The detection conditions for cysteine such as the potential and pH were also discussed.
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The silver doped poly(L-aspartic acid) modified electrode was prepared by cyclic voltammetric method. The voltammetric behavior of dopamine and cyclic voltammetric method for the determination of dopamine were studied on the silver doped poly(L-aspartic acid) modified electrode. In pH 7.0 phosphate buffer solution, the peak potential was 0.191 V of Epa and 0.161 V of Epc(vs.Ag/AgCl) at the scan rate of 50 mV/s. The linear ranges for the determination of dopamine were 3.0×10-7-1.0×10-5 mol/L and 1.0×10-5-5.0×10-4 mol/L. The detection limit was 5.0×10-8 mol/L. The method was applied to the determination of dopamine in drug and urine with satisfactory results.
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Vitamin B1 self-assembled monolayer modified electrode (VB1-Au/SAMs/CME) was prepared and its electrochemical behavior was studied by cyclic voltammetry. The results showed that a self-assembled monolayer (SAM) was formed on the surface of gold electrode. \3-/4-redox couple was used as the electrochemical probe to study the electrochemical characteristics of SAM modified gold electrode and the results indicated that the existence of Vitamin B1 membrane on gold surface hindered the electron transfer. The electrochemical behaviors of dopamine(DA) and uric acid (UA) were investigated at VB1-Au/SAMs/CME. The results showed that the electrochemical oxidation of DA and UA could be electrocatalyzed. There were linear relationships between the anodic peak current and the concentration of DA(8.0×10-6-4.0×10-4 mol/L) and UA (6.0×10-5-2.2×10-4mol/L) respectively in differential pulse voltammograms. This modified electrode was effective to detect DA and UA in simultaneous determination of these species in a mixture.
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The electrochemical behaviors of parathion(PT) on nano-Al2O3 film modified electrode(nano-Al2O3/GCE/CME) were investigated. It was found that the redox peak currents of PT remarkably increased and the oxidation peak potential negatively shifted at the nano-Al2O3/GCE/CME. All the experimental parameters were optimized and a simple and sensitive electroanalytical method was developed for the determination of PT. The oxidation peak current was linear with the concentration of PT over the range from 2.5×10-9 to 1.0×10-7 mol/L and 1.0×10-7 to 1.0×10-5 mol/L. A low detection limit of 1.0×10-9 mol/L was obtained for 30 s accumulation at open circuit(S/N=3). The relative standard deviation(n=10) was 3.8% for 1×10-5 mol/L PT. The proposed method was used for the quantitative analysis of PT in some vegetables and the results were satisfactory.
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Molecular imprinted film modified glassy carbon electrode was prepared by electrochemical polymerization of pyrrole with the cyclic voltammetry in the presence of template molecular, salicylic acid. The template molecules were removed from the modified electrode surface by over-oxidized at 1.3V in the solution of 0.2 mol/L Na2HPO4 for 10 min. The modified electrodes can effectively promote electrochemical oxidation process of salicylic acid in the surface of electrode and avoid interference of structural similar substance such as benzoic acid. Cyclic voltammetry was employed in the electrochemical measurements. The experimental results show that the optimum acidity of background solution is pH 6.86 and the optimum incubation is 10 min. The linear response curve was obtained from 1.0×10-6 mol/L to 2.0×10-3 mol/L, with the detection limit of 8.0×10-7 mol/L. The imprinted electrode has been applied to the analysis of salicylic acid in the simulated samples with recovery rates ranging from 94.6% to 103.4%.
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The cyclic voltammetric behaviors of sodium selenite on the gold electrode modified by L-cysteine self-assembled monolayer (L-Syc,Au/SAMs) has been investigated in 0.05 mol/L H_2SO_4 solutions with sodium selenite. Sensitive anodic stripping current of selenium (Se) with the peak potential at 0.99 V (vs. SCE) has been observed. In comparison with the electrochemical properties of sodium selenite on the modified electrode with those on the naked gold electrode, it was found that selenite was reduced to selenium by the redox interaction with sulfur on the monolayer and the monolayer catalytically oxidizes Se as the electrode was positively scanned. According to the electrochemical properties of sodium selenite both on the naked and modified gold electrode, the Se deposition mechanism and catalytic mechanism as well as bionic membrane model were proposed for the bio-utilization of selenite through nano scale selenium.
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A poly(amino black 10B)/Nafion modified glassy carbon(GC) electrode for the detection of dopamine(DA) has been developed. The modified electrode showed an excellent electrocatalytic effect on the oxidation of DA. In cyclic votammetric measurements, the redox peak current increased linearly with the concentration of DA in the range of 2.0×10~(-7) 3.0×10~(-5) mol/L in PBS of pH 6.0, with a correlation coefficient of 0.9993 and 0.9991, respectively. The detection limit(S/N=3) was 1.0×10~(-7) mol/L. Moreover, the modified electrode exhibited good repeatability and long-time stability, and avoided the interference of ascorbic acid. The modified electrode has been used for the determination of DA in the injections and calf serum with good recovery and reproducibility.
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A malária é a endemia tropical mais devastadora do mundo e esse quadro é agravado pela ausência de tratamento eficaz. Entretanto, a resistência dos plasmódios à artemisinina não apresenta relevância clínica e seu mecanismo de ação está associado ao grupo heme, com formação de radicais livres e rompimento da ponte endoperóxido. O comportamento voltamétrico da artemisinina foi estudado por voltametria cíclica e voltametria de onda quadrada. O fármaco é irreversivelmente reduzido em eletrodos de carbono vítreo e os valores de potencial de pico não sofrem influência da acidez do meio, porém observou-se o maior valor de corrente em pH 6,0. O comportamento voltamétrico da artemisinina foi significativamente alterado na presença do grupo heme, provocando uma antecipação de seu pico de redução em cerca de 600 mV. Por voltametria de onda quadrada observou-se que este novo pico foi sensível à adição crescente de concentração de hemina, atingindo valor de corrente cerca de 10 vezes maior em relação ao pico original da artemisinina, numa relação de concentração de 20 mmol/L para o primeiro e 50 mmol/L do segundo. Além disso, resultados indicaram que esse processo eletrocatalítico ocorreu pela formação de Fe(II)-hemina na superfície do eletrodo, com provável processo de eletro-polimerização da hemina sobre o eletrodo de carbono vítreo. Esse efeito adsortivo foi avaliado a partir da estimativa da concentração superficial (G) de hemina sobre o eletrodo de trabalho em pH 6,0. A modificação do eletrodo de carbono vítreo por hemina mostrou que a interação entre artemisinina e o grupo heme ocorre predominantemente sobre a superfície do eletrodo e não em solução. Portanto, esclarecer o mecanismo de ação da artemisinina é importante para o planejamento e desenvolvimento de novos agentes antimaláricos.
Malaria is the tropical disease most devastating of the world and this situation is worsened by the absence of effective treatment. However, the plasmodium resistance to artemisinin does not show clinical relevance. The drug mechanism of action is associated to the heme group, with free radical formation and endoperoxide moiety breakage. The voltammetric behavior of artemisinin was studied by cyclic and square-wave voltametries. This drug was irreversibly reduced on glassy carbon electrode and the peak potential values are pH independent, however the biggest value of current peak was observed at pH 6.0. The voltammetric behavior of artemisinin was significantly changed in the heme group presence, provoking an anticipation of about 600 mV on cathodic peak. By square-wave voltammetry it was observed that this new peak was sensitive to the hemin concentration, reaching a value around 10 times larger regarding the original cathodic peak of artemisinin, being the concentration of 20 mmol/L for the former and 50 mmol/L for the latter. In addition, results indicated that this electro-catalytic process depends on the Fe(II)-hemin formation on the electrode surface, indicating the possible electro-polymerization of hemin on the glassy carbon electrode. This adsorptive effect was evaluated from the superficial concentration (G) estimation of the hemin on the working electrode at pH 6.0. The modification of the glassy carbon electrode using hemin showed that the interaction between artemisinin and the heme group predominantly occurs on the electrode surface and not in solution. Therefore, clarifying artemisinin mechanism of action is important in order to contribute for the design and development of new antimalarial agents.