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1.
The electrochemical behavior of nandrolone decanoate (ND) at gold nanoparticles modified indium tin oxide (ITO) electrode was investigated. Oxidation of ND has been carried out in phosphate containing supporting electrolyte in the pH range 2.1-9.2 and a well-defined oxidation peak was noticed. The peak potential (Ep) of the oxidation peak decreases linearly with increasing pH. Linear calibration curve is obtained over the nandrolone decanoate concentration range of 50 nM to 1.5 μM at pH 7.2 with a detection limit of 1.36 × 10−7 M. The proposed method is effectively applied to detect the concentration of ND in human blood serum and urine samples after 24 and 72 h of intramuscular injection. The method is rapid and does not require any pre-treatment.  相似文献   

2.
A graphene, chitosan and Fe3O4 nanoparticles (nano-Fe3O4) modified glassy carbon electrode (graphene-chitosan/nano-Fe3O4/GCE) was fabricated. The modified electrode was characterized by scanning electron microscope and electrochemical impedance spectroscopy. The electrochemical oxidation behavior of guanosine was investigated in pH 7.0 phosphate buffer solution by cyclic voltammetry and differential pulse voltammetry. The experimental results indicated that the modified electrode exhibited an electrocatalytic and adsorptive activities towards the oxidation of guanosine. The transfer electron number (n), transfer proton number (m) and electrochemically effective surface area (A) were calculated. Under the optimized conditions, the oxidation peak current was proportional to guanosine concentration in the range of 2.0 × 10−6 to 3.5 × 10−4 mol L−1 with the correlation coefficient of 0.9939 and the detection limit of 7.5 × 10−7 mol L−1 (S/N = 3). Moreover, the modified electrode showed good ability to discriminate the electrochemical oxidation response of guanosine, guanine and adenosine. The proposed method was further applied to determine guanosine in spiked urine samples and traditional Chinese medicines with satisfactory results.  相似文献   

3.
Monolayers of 3,3′-dithiodipropionic acid (DTDPA) were prepared on a polycrystalline gold electrode through a self-assembly procedure to produce a gold 3,3′-dithiodipropionic acid self-assembled monolayer (AuDTDPA) modified electrode. The characterization of the AuDTDPA electrode was investigated by cyclic voltammetry and ac impedance using the [Fe(CN)6]3−/4− redox couple. The electrochemical behavior of DA on the modified electrode AuDTDPA was studied by cyclic and square-wave voltammetries, using phosphate buffer as supporting electrolyte. The oxidation peak current for DA increases linearly with concentration in the range of 0.35 × 10−5 to 3.4 × 10−5 mol L−1. The performance of the AuDTDPA modified electrode was evaluated for the electroanalytical determination of dopamine (DA) in a pharmaceutical formulation. The AuDTDPA modified electrode showed a stable behavior and the presence of surface-COOH groups avoided the passivation of the electrode surface during the dopamine oxidation.  相似文献   

4.
A simple procedure has been used for preparation of modified glassy carbon electrode with carbon nanotubes and copper complex. Copper complex [Cu(bpy)2]Br2 was immobilized onto glassy carbon (GC) electrode modified with silicomolybdate, α-SiMo12O404− and single walled carbon nanotubes (SWCNTs). Copper complex and silicomolybdate irreversibly and strongly adsorbed onto GC electrode modified with CNTs. Electrostatic interactions between polyoxometalates (POMs) anions and Cu-complex, cations mentioned as an effective method for fabrication of three-dimensional structures. The modified electrode shows three reversible redox couples for polyoxometalate and one redox couple for Cu-complex at wide range of pH values. The electrochemical behavior, stability and electron transfer kinetics of the adsorbed redox couples were investigated using cyclic voltammetry. Due to electrostatic interaction, copper complex immobilized onto GC/CNTs/α-SiMo12O404− electrode shows more stable voltammetric response compared to GC/CNTs/Cu-complex modified electrode. In comparison to GC/CNTs/Cu-complex the GC/CNTs/α-SiMo12O404− modified electrodes shows excellent electrocatalytic activity toward reduction H2O2 and BrO3 at more reduced overpotential. The catalytic rate constants for catalytic reduction hydrogen peroxide and bromate were 4.5(±0.2) × 103 M−1 s−1 and 3.0(±0.10) × 103 M−1 s−1, respectively. The hydrodynamic amperommetry technique at 0.08 V was used for detection of nanomolar concentration of hydrogen peroxide and bromate. Detection limit, sensitivity and linear concentration range proposed sensor for bromate and hydrogen peroxide detection were 1.1 nM and 6.7 nA nM−1, 10 nM-20 μM, 1 nM, 5.5 nA nM−1 and 10 nM-18 μM, respectively.  相似文献   

5.
The electrochemical behaviors of guanosine on the ionic liquid of N-butylpyridinium hexafluorophosphate (BPPF6) modified carbon paste electrode (CPE) was studied in this paper and further used for guanosine detection. Guanosine showed an adsorption irreversible oxidation process on the carbon ionic liquid electrode (CILE) with the oxidation peak potential located at 1.12 V (vs. SCE) in a pH 4.5 Britton-Robinson (B-R) buffer solution. Compared with that on the traditional carbon paste electrode, small shift of the oxidation peak potentials appeared but with a great increment of the oxidation peak current on the CILE, which was due to the presence of ionic liquid in the modified electrode adsorbed the guanosine on the surface and promoted the electrochemical response. The electrochemical parameters such as the electron transfer coefficient (α), the electron transfer number (n), and the electrode reaction standard rate constant (ks) were calculated as 0.74, 1.9 and 1.26 × 10−4 s−1, respectively. Under the optimal conditions the oxidation peak current showed a good linear relationship with the guanosine concentration in the range from 1.0 × 10−6 to 1.0 × 10−4 mol/L by cyclic voltammetry with the detection limit of 2.61 × 10−7 mol/L (3σ). The common coexisting substances showed no interferences to the guanosine oxidation. The CILE showed good ability to distinguish the electrochemical response of guanosine and guanine in the mixture solution. The urine samples were further detected by the proposed method with satisfactory results.  相似文献   

6.
The electrochemical properties of valacyclovir, an antiviral drug, were investigated in pH range 1.8-12.0 by cyclic, differential pulse and square-wave voltammetry. The drug was irreversibly oxidized at a glassy carbon electrode in one or two oxidation steps, which are pH-dependent. For analytical purposes, a very resolved diffusion controlled voltammetric peak was obtained in Britton-Robinson buffer at pH 10.0 using differential pulse and square-wave modes. Limits of detection were 1.04 × 10−7 and 4.60 × 10−8 M for differential pulse and square-wave voltammetry, respectively. The applicability to direct assays of tablets, spiked human serum and simulated gastric fluid, was described.  相似文献   

7.
Boron-doped diamond (BDD) films are excellent electrode materials, whose electrochemical activity for some analytes can be tuned by controlling their surface termination, most commonly either to predominantly hydrogen or oxygen. This tuning can be accomplished by e.g. suitable cathodic or anodic electrochemical pretreatments. Recently, it has been shown that amorphous carbon nitride (a-CNx) films may present electrochemical characteristics similar to those of BDD, including the influence of surface termination on their electrochemical activity toward some analytes. In this work, we report for the first time a complete electroanalytical method using an a-CNx electrode. Thus, an a-CNx film deposited on a stainless steel foil by DC magnetron sputtering is proposed as an alternative electrode for the simultaneous determination of dopamine (DA) and ascorbic acid (AA) in synthetic biological samples by square-wave voltammetry. The obtained results are compared with those attained using a BDD electrode. For both electrodes, a same anodic pretreatment in 0.1 mol L−1 KOH was necessary to attain an adequate and equivalent separation of the DA and AA oxidation potential peaks of about 330 mV. The detection limits obtained for the simultaneous determination of these analytes using the a-CNx electrode were 0.0656 μmol L−1 for DA and 1.05 μmol L−1 for AA, whereas with the BDD electrode these values were 0.283 μmol L−1 and 0.968 μmol L−1, respectively. Furthermore, the results obtained in the analysis of the analytes in synthetic biological samples were satisfactory, attesting the potential application of the a-CNx electrode in electroanalysis.  相似文献   

8.
Goyal RN  Singh SP 《Talanta》2006,69(4):932-937
C60-modified glassy carbon electrode has been found to exhibit excellent electrocatalytic activity towards atenolol oxidation for its voltammetric determination at physiological pH. Lowering of overpotential associated with atenolol oxidation indicates electrocatalytic nature of electrode. Determination of atenolol was carried out at pH 7.2 at modified electrode and a well-defined oxidation peak has been observed ∼1040 mV versus Ag/AgCl electrode for atenolol oxidation. Calibration plot having good co-linearity with a correlation coefficient 0.997 was obtained in the concentration range of 0.25-1.5 mM atenolol and the sensitivity of the method has been found to be 8.58 μA mM−1. The detection limit is found to be 0.16 mM. The method developed is applicable for atenolol determination in pharmaceutical preparations and urine samples. The modified electrode showed a good surface coverage (∼85%) with C60.  相似文献   

9.
Shuqing Dong  Yuzhi Fang 《Talanta》2009,80(2):809-303
In the paper, a new kind of vitamin B12 (acquo-cobalamine) chemically modified electrode was fabricated and applied in capillary zone electrophoresis coupled with amperometric detection (CZE-AD) for simultaneous determination of six antioxidants in fruits and vegetables. The catalytic electrochemical properties of the chemically modified electrode could obviously enhance oxidation peak heights responses by about five times to glutathione, ascorbic acid, vanillic acid, chlorogenic acid, salicylic acid, and caffeic acid compared with common carbon disk electrode. Furthermore, the effects of working electrode potential, pH and concentration of running buffer, separation voltage and injection time on CZE-AD were investigated. Under the optimum conditions, the six analytes could be completely separated and detected in a borate-phosphate buffer (pH 8.4) within 15 min. Their linear ranges were from 2.5 × 10−7 to 1.0 × 10−4 mol L−1 and the detection limits were as low as 10−8 mol L−1 magnitude (S/N = 3). The proposed method has been successfully employed to monitor the six analytes in practical samples with recoveries in the range 96.0-106.0% and RSDs less than 5.0%. Above results demonstrate that capillary zone electrophoresis coupled with electrochemical detection using vitamin B12 modified electrode as detector is of convenient preparation, high sensitivity, good repeatability, and could be used in the rapid determination of practical samples.  相似文献   

10.
A simple electrochemical method was developed for the single and simultaneous determination of butylated hydroxyanisole (BHA) and butylated hydroxytoluene (BHT) in food samples using square-wave voltammetry (SWV). A carbon composite electrode modified (MCCE) with copper (II) phosphate immobilized in a polyester resin was proposed. The modified electrode allowed the detection of BHA and BHT at potentials lower than those observed at unmodified electrodes. A separation of about 430 mV between the peak oxidation potentials of BHA and BHT in binary mixtures was obtained. The calibration curves for the simultaneous determination of BHA and BHT demonstrated an excellent linear response in the range from 3.4 × 10−7 to 4.1 × 10−5 mol L−1 for both compounds. The detection limits for the simultaneous determination of BHA and BHT were 7.2 × 10−8 and 9.3 × 10−8 mol L−1, respectively. In addition, the stability and repeatability of the electrode were determined. The proposed method was successfully applied in the simultaneous determination of BHA and BHT in several food samples, and the results obtained were found to be similar to those obtained using the high performance liquid chromatography method with agreement at 95% confidence level.  相似文献   

11.
Yardım Y  Levent A  Keskin E  Sentürk Z 《Talanta》2011,85(1):441-448
Benzo[a]pyrene (BaP), a member of the polycyclic aromatic hydrocarbon (PAH) class, is one of the most potent PAH carcinogens. The electrochemical oxidation of BaP was first studied by cyclic voltammetry at the boron-doped diamond electrode in non-aqueous solvent (dimethylsulphoxide with lithium perchlorate). The compound was irreversibly oxidized in a single step at high positive potential, resulting in the well-resolved formation of a couple with a reduction and re-oxidation wave at much lower potentials. Special attention was given to the use of adsorptive stripping voltammetry together with a medium exchange procedure in aqueous and aqueous/surfactant solutions over the pH range of 2.0-8.0. The technique in aqueous solutions had little value in practice because of too small oxidation peak current. This problem was solved when surfactants were added into the sample solution, by which the oxidation peak currents of BaP were found enhanced dramatically. The employed surfactants were sodium dodecylsulfate (anionic, SDS), cetyltrimethylammonium bromide (cationic, CTAB) and Tween 80 (non-ionic). Using square-wave stripping mode, the compound yielded a well-defined voltammetric response in Britton-Robinson buffer, pH 2.0 containing 2.5 × 10−4 M SDS at +1.07 V (vs. Ag/AgCl) (after 120 s accumulation at +0.10 V). The process could be used to determine BaP in the concentration range of 16-200 nM (4.04-50.46 ng mL−1), with a detection limit of 2.86 nM (0.72 ng mL−1). This method was also applied to determine BaP in model water sample prepared by adding its different concentrations into tap water.  相似文献   

12.
A highly sensitive NOx sensor was designed and developed by electrochemical incorporation of copper nanoparticles (CuNP) on single-walled carbon nanotubes (SWCNT)-polypyrrole (PPy) nanocomposite modified Pt electrode. The modified electrodes were characterized by scanning electron microscopy and energy dispersive X-ray analysis. Further, the electrochemical behavior of the CuNP-SWCNT-PPy-Pt electrode was investigated by cyclic voltammetry. It exhibited the characteristic CuNP reversible redox peaks at −0.15 V and −0.3 V vs. Ag/AgCl respectively. The electrocatalytic activity of the CuNP-SWCNT-PPy-Pt electrode towards NOx is four-fold than the CuNP-PPy-Pt electrode. These results clearly revealed that the SWCNT-PPy nanocomposite facilitated the electron transfer from CuNP to Pt electrode and provided an electrochemical approach for the determination of NOx. A linear dependence (r2 = 0.9946) on the NOx concentrations ranging from 0.7 to 2000 μM, with a sensitivity of 0.22 ± 0.002 μA μM−1 cm−2 and detection limit of 0.7 μM was observed for the CuNP-SWCNT-PPy-Pt electrode. In addition, the sensor exhibited good reproducibility and retained stability over a period of one month.  相似文献   

13.
A multi-wall carbon nanotubes (MWNTs)-dihexadecyl hydrogen phosphate (DHP) film-coated glassy carbon electrode (GCE) was fabricated, and the electrochemical behaviors of acyclovir on the MWNTs-DHP film-coated GCE were investigated by using cyclic voltammetry (CV), linear sweep voltammetry (LSV), electrochemical impedance spectroscopy (EIS) and chronocoulometry (CC). The oxidation peak current of acyclovir increased significantly and the peak potential shifted negatively at the MWNTs-DHP film-modified GCE, compared with that at a bare GCE. The results showed that this nano-structured film electrode exhibited excellent enhancement effects on the electrochemical oxidation of acyclovir. Consequently, a simple and sensitive electroanalytical method was developed for the determination of acyclovir. The oxidation peak current was proportional to the concentration of acyclovir from 8.0 × 10−8 to 1.0 × 10−5 mol/L. The detection limit was about 3.0 × 10−8 mol/L for 60 s accumulation at 0.00 V. The proposed method was demonstrated by using acyclovir tablets and the result was satisfying.  相似文献   

14.
A new rapid, convenient and sensitive electrochemical method based on a gold nanoparticles modified ITO (Au/ITO) electrode is described for the detection of dopamine and serotonin in the presence of a high concentration of ascorbic acid. The electrocatalytic response was evaluated by differential pulse voltammetry (DPV) and the modified electrode exhibited good electrocatalytic properties towards dopamine and serotonin oxidation with a peak potential of 70 mV and 240 mV lower than that at the bare ITO electrode, respectively. The selective sensing of dopamine is further improved by applying square wave voltammetry (SWV) which leads to the lowering of its detection limit. A similar effect on the detection limit of serotonin was observed on using SWV. Linear calibration curves are obtained in the range 1.0 × 10−9-5.0 × 10−4 M and 1.0 × 10−8-2.5 × 10−4 M with a detection limit of 0.5 nM and 3.0 nM for dopamine and serotonin, respectively. The Au/ITO electrode efficiently determines both the biomolecules simultaneously, even in the presence of a large excess of ascorbic acid. The adequacy of the developed method was evaluated by applying it to the determination of the content of dopamine in dopamine hydrochloride injections. The proposed procedure was also successfully applied to simultaneously detect dopamine and serotonin in human serum and urine.  相似文献   

15.
Santos LS  Landers R  Gushikem Y 《Talanta》2011,85(2):1213-1216
This work describes the in situ immobilization of Mn(II) phthalocyanine (MnPc) in a porous SiO2/SnO2 mixed oxide matrix obtained by the sol gel processing method. The chemically modified matrix SiO2/SnO2/MnPc, possessing an estimated amount of 8 × 10−10 mol cm−2 of MnPc on the surface, was used to prepare an electrode to analyze dissolved oxygen in water by an electrochemical technique. The electrode was prepared by mixing the material with ultrapure graphite and evaluated using differential pulse voltammetry. Dissolved O2 was reduced at −0.31 V with a limit of detection (LOD) equal to 7.0 × 10−4 mmol L−1. A mechanism involving four electrons in O2 reduction was determined by the rotating disk electrode technique.  相似文献   

16.
Gazy AA 《Talanta》2004,62(3):575-582
The adsorptive and electrochemical behavior of amlodipine besylate on a glassy carbon electrode were explored in Britton-Robinson buffer solution by using cyclic and square-wave voltammetry. Cyclic voltammetric studies indicated the oxidation of amlodipine besylate at the electrode surface through a single two-electron irreversible step and fundamentally controlled by adsorption. The solution conditions and instrumental parameters were optimized for the determination of the authentic drug by adsorptive square-wave stripping voltammetry. Amlodipine besylate gave a sensitive adsorptive oxidation peak at 0.510 V (versus Ag/AgCl). The oxidation peak was used to determine amlodipine besylate in range 4.0×10−8 to 2.0×10−6 with a detection limit of 1.4×10−8 M. The procedure was successfully applied for the assay of amlodipine besylate in tablets (Norvasc)®. The percentage recoveries were in agreement with those obtained by the reference method. Applicability to assay the drug in urine and serum samples was illustrated. The mean percentage recoveries were 96.31±1.18 and 96.98±1.17, respectively. The proposd method used for monotoring clinically relevant concntrations of drug in human urine and serum.  相似文献   

17.
α-Fe2O3 nanoparticles prepared using a simple solution-combusting method have been dispersed in chitosan (CH) solution to fabricate nanocomposite film on glass carbon electrode (GCE). The as-prepared α-Fe2O3 nanoparticles were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM). The nanocomposite film exhibits high electrocatalytic oxidation for nitric oxide (NO) and reduction for hydrogen peroxide (H2O2). The electrocatalytic oxidation peak is observed at +0.82 V (vs. Ag/AgCl) and controlled by diffusion process. The electrocatalytic reduction peak is observed at −0.45 V (vs. Ag/AgCl) and controlled by diffusion process. This α-Fe2O3-CH/GCE nanocomposite bioelectrode has response time of 5 s, linearity as 5.0 × 10−7 to 15.0 × 10−6 M of NO with a detection limit of 8.0 × 10−8 M and a sensitivity of −283.6 μA/mM. This α-Fe2O3-CH/GCE nanocomposite bioelectrode was further utilized in detection of H2O2 with a detection limit of 4.0 × 10−7 M, linearity as 1.0 × 10−6 to 44.0 × 10−6 M and with a sensitivity of 21.62 μA/mM. The shelf life of this bioelectrode is about 6 weeks under room temperature conditions.  相似文献   

18.
Yan Wang  Zhen-zhen Chen 《Talanta》2010,82(2):534-621
This report described the direct voltammetric detection of peroxynitrite (ONOO) at a novel cyanocobalamin modified glassy carbon electrode prepared by electropolymeriation method. The electrochemical behaviors of peroxynitrite at the modified electrode were studied by cyclic voltammetry. The results showed that this new electrochemical sensor exhibited an excellent electrocatalytic activity to oxidation of peroxynitrite. The mechanism of catalysis was discussed. Based on electrocatalytic oxidation of peroxynitrite at the poly(cyanocobalamin) modified electrode, peroxynitrite was sensitively detected by differential pulse voltammetry. Under optimum conditions, the anodic peak current was linear to concentration of peroxynitrite in the range of 2.0 × 10−6 to 3.0 × 10−4 mol L−1 with a detection limit of 1.0 × 10−7 mol L−1 (S/N of 3). The proposed method has been applied to determination of peroxynitrite in human serum with satisfactory results. This poly(cyanocobalamin) modified electrode showed high selectivity and sensitivity to peroxynitrite determination, which could be used in quantitative detection of peroxynitrite in vivo and in vitro.  相似文献   

19.
Goyal RN  Chatterjee S  Rana AR 《Talanta》2010,83(1):149-155
Electrochemical sensor employing edge-plane pyrolytic graphite electrode (EPPGE) for the sensitive detection of hydrocortisone (HC) is delineated for the first time. The electrochemical properties are investigated exercising the cyclic voltammetry and square-wave voltammetry (SWV). When equating with the bare basal-plane pyrolytic graphite electrode (BPPGE), the EPPGE gave better response towards the detection of HC both in terms of sensitivity and detection limit. The voltammetric results indicated that EPPGE remarkably enhances the reduction of HC which leads to considerable amelioration of peak current with shift of peak potential to less negative values. The difference in the surface morphology of two electrodes has been studied. Also, the EPPGE delivered an analytical performance for HC with a sensitivity of 45 nA nM−1 and limit of detection of 88 nM in the concentration range 100-2000 nM. The method has been utilized for the determination of HC in pharmaceuticals and real samples. The electroanalytical method using EPPGE is the most sensitive method for determination of HC with lowest limit of detection to date. The major metabolites present in blood plasma did not intervene with the present investigation as they did not exhibit reduction peak in the experimental range used. A comparison of results with high performance liquid chromatography (HPLC) signalizes a good agreement.  相似文献   

20.
Liu AL  Zhang SB  Chen W  Huang LY  Lin XH  Xia XH 《Talanta》2008,77(1):314-318
The electrochemical behavior of isorhamnetin (ISO) at a glassy carbon electrode was studied in a phosphate buffer solution (PBS) of pH 4.0 by cyclic voltammetry (CV) and differential pulse voltammetric method (DPV). A well-defined redox wave of ISO involving one electrons and one proton appeared. The electrode reaction is a reactant weak adsorption-controlled process with a charge transfer coefficient (α) of 0.586. Based on the understanding of the electrochemical process of ISO at the glassy carbon electrode, analysis of ISO can be realized. Under optimal conditions, the oxidation peak current showed linear dependence on the concentration of ISO in the range of 1.0 × 10−8 to 4.0 × 10−7 M and 1.0 × 10−6 to 1.0 × 10−5 M. The detection limit is 5.0 × 10−9 M. This method has been successfully applied to the detection of ISO in tablets.  相似文献   

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