Determination of trace amount of antimony (Ⅲ) by adsorption voltammetry on carbon paste electrode

A sensitive method is described for the determination of trace antimony based on the antimony-bromopyrogallol red (BPR) adsorption at a carbon paste electrode (CPE). Three steps were involved in the overall analysis: preconcentration,reduction and stripping. Optimal conditions were found to be an electrode containing 25% paraffin oil and 75% high purity graphite powder as working electrode;a 0.10 mol/L HCl solution containing 40 μmol/L BPR as accumulation medium;a 0.20 mol/L HCl solution as reduction and stripping electrolyte;accumulation time,150 s;reduction potential and time,-0.50 V,60 s;scan range from -0.50 to 0.20 V. Interferences by other ions were studied as well. The detection limit was found to be 0.5 nmol/L for 150 s preconcentration. The linear range was from 1.0 nmol/L to 0.50 μmol/L. Application of the proposed method to the determination of antimony in water and human hair samples gave good results.

Effects of MK-801 and Schizandrol A on DA/DOPAC Measured by Voltammetry in Ischemic Rat Striatum

The time course of changes in the levels of extracellular DA/DOPAC in rat striatum during brain ischemia and reperfusion was measured by the method ofin vivo differential normal pulse voltammetry(DNPV).Acute cerebral ischemia of rats was pro- duced by four—vessel occlusion.The effects of(+)MK-801 and schizandrol A on the change of DA/DOPAC were investigated.The results showed that the DA/DOPAC peak in- creased markedly during 6 min of ischemia and,after reperfusion,the peak height decreased gradually.Both(+)-MK-801 and schizandrol A significantly inhibited the DA release after ischemia jn the striatum.

Trace Determination of Scandium Using Adsorption Voltammetry of Mix-Polynuclear Complex of Scandium-Calcium-Alizarin Red S at Carbon Paste Electrode

A novel method was described for the determination of ultra trace amount of scandium based on the cathodic adsorptive voltammetry of the mix-polynuclear complex of scandium-calcium-alizarin red S at a carbon paste electrode (CPE). The 2nd-order derivative linear scan voltammograms of the adsorbed complex were recorded by model JP-303 polarographic analyzer from 0.0 to -1.0 V (vs. SCE). The experimental conditions of the working procedure were optimized. The results show that the complex can be adsorbed on the surface of the CPE, yielding one peak at -0.61 V, corresponding to the reduction of the alizarin red S in the mix-polynuclear complex at the electrode. The detection limit of Sc^(3+) is 1.0×10^(-10) mol·L^(-1) for 3 min of accumulation time. The procedure was successfully applied to the determination of trace amount of scandium in the sample ores.

Voltammetric behavior of sedative drug midazolam at glassy carbon electrode in solubilized systems

Redox behavior of midazolam was studied at a glassy carbon electrode in various buffer systems,supporting electrolytes and pH using differential paise,square-wave and cyclic voltammetry.Based on its reduction behavior,a direct differential pulse voltammetric method has been developed and validated for the determination of midazolam in parenteral dosage.Three welldefined peaks were observed in 0.1％ SLS,Britton-Robinson (BR) buffer of pH 2.5.The effect of surfaetants like sodium lauryl sulfate (SLS),cetyl trimethyl ammonium bromide (CTAB) and Tween 20 was studied.Among these surfactants SLS showed significant enhancement in reduction peak.The cathodic peak currents were directly proportional to the concentration of midazolam with correlation coetfficient of 0.99.

Sensitive Voltammetric Determination of Captopril Using a Carbon Paste Electrode Modified with Nano-TiO_2/Ferrocene Carboxylic Acid

A carbon paste electrode (CPE) modified with ferrocene carboxylic acid (FcCA) and TiO2 nanoparticles was constructed by incorporating TiO2 nanoparticles and ferrocene carboxylic acid into the carbon paste matrix. The electrochemical behavior of captopril (CAP) at the surface of the modified electrode was investigated using electroanalytical methods. The modified electrode showed excellent electrocatalytic activity for the oxidation of CAP in aqueous solutions at physiological pH values. Cyclic voltammetric curves showed that the oxidation of CAP at the surface of the modified electrode reduced its overpotential by more than 290 mV. The modified electrode was used for detecting captopril using cyclic voltammetry and square wave voltammetry techniques. A calibration curve in the range of 0.03 to 2400 μmol/L was obtained that had a detection limit of 0.0096 μmol/L (3?) under the optimized conditions. The modified electrode was successfully used for the determination of captopril in pharmaceutical and biological samples.

Investigation of the interaction of carbofuran and DNA by voltammetry and fluorescence with the aid of chemometrics

The interactions of carbofuran and DNA were studied using voltammetry and fluorescence spectroscopy.The formation of carbofuran-DNA makes the current peak of DNA decreased by voltammetry method.The binding number（n） and constant（Ka） for complex carbofuran-DNA were calculated to be 1.06±0.04 and 0.11±0.03mol^-1 L,respectively by fluorescence measurement.Chemometrics approach,such as singular value decomposition（SVD） was used to evaluate the number of spectral species in the drug-DNA binding process.And the pure spectra and concentration profiles in the kinetic system were clearly deduced by multivariate curve resolution alternating least squares（MCR-ALS） with the initial estimates by evolving factor analysis（EFA）.

Simultaneous Voltammetric Determination of Three Herbicides in Food and Water Samples with the Aid of Chemometrics

Differential pulse stripping voltammetry method（DPSV） was applied to the determination of three herbicides, ametryn, cyanatryn, and dimethametryn. It was found that their voltammograms overlapped strongly, and it is difficult to determine these compounds individually from their mixtures. With the aid of chemometrics, classical least squares（CLS）, principal component regression（PCR） and partial least squares（PLS）, voltammogram resolution and quantitative analysis of the synthetic mixtures of the three compounds were successfully performed. The proposed method was also applied to the analysis of some real samples with satisfactory results.

Electrooxidation of sulfanilamide and its voltammetric determination in pharmaceutical formulation,human urine and serum on glassy carbon electrode

For the first time, sulfanilamide(SFD) was determined in otologic solution, human urine and serum by electroanalytical techniques on glassy carbon electrode(GCE). The cyclic voltammetry(CV) experiments showed an irreversible oxidation peak at t 1.06 V in 0.1 mol/L BRBS(p H ? 2.0) at 50 m V/s. Different voltammetric scan rates(from 10 to 250 m V/s) suggested that the oxidation of SFD on the GCE was a diffusioncontrolled process. Square-wave voltammetry(SWV) method under optimized conditions showed a linear response to SFD from 5.0 to 74.7 μmol/L(R ? 0.999) with detection and quantification limits of 0.92 and3.10 μmol/L, respectively. The developed SWV method showed better results for detection limit and linear range than the chronoamperometry method. It has been successfully applied to determine SFD concentration in pharmaceutical formulation, human urine and serum samples with recovery close to 100%.

Determination of trace amounts of morphine in human plasma by anodic adsorptive stripping differential pulse voltammetry

New adsorptive anodic differential pulse stripping voltammetry method for the direct determination of morphine at trace levels in human plasma of addicts is proposed.The procedure involves an adsorptive accumulation of morphine on a HMDE,followed by oxidation of adsorbed morphine by voltammetry scan using differential pulse modulation.The optimum conditions for the analysis of morphine are pH 10.5,Eacc of -100 mV（vs.Ag/AgCl）,and tacc of 120 s.The peak current is proportional to the concentration of morphine,and a Linear calibration graph is obtained at 0.01-3.10μg mL^-1.A relative standard deviation of 1.06%（n=5）was obtained,and the limit of detection was 3 ng mL^-1.The capabiLity of the method for the analysis of real samples was evaluated by the determination of morphine in spiked human plasma and addicts human plasma with satisfactory results.

Interaction between Eu-phenylalanine and DNA Using Cyclic Voltammetry and UV Spectroscopy

The interaction between DNA and the Eu(Phe) 3+ 3 complex ion has been studied by means of cyclic voltammetry and differential UV spectroscopy The results depicted an obvious decrease of peak current in CV plot after the reaction between the two species studied The observed peak potential separation was increased but the diffusion coefficient of Eu complex ion was decreased Hypochromicity was observed at 226 and 258 nm after the predicted interaction of them A preliminary interpretation is proposed for discussion

Amperometric detection of gold by differential pulse voltammetry using a DNA biosensor

A DNA biosensor with [Ru（DA-bpy）3]Cl2（DA-bpy：4,4＇-diamino-2,2＇-bipyridine） （RuL） as the electrochemical probe was prepared on pyrolytic graphite electrode （PGE） through the supramolecular interaction between RuL complex and DNA template. Cyclic voltammetry of RuL-DNA film showed a pair of stable and reversible peaks corresponding to the Ru（Ⅲ）/Ru（Ⅲ） redox potential of-0.165 V versus AglAgCl in pa 7.4 0.1 mol·L^-1Tris-HCl. The electron transfer was expected across the double-strand DNA by an ＂electron tunneling＂ mechanism. When the DNA biosensor was immerged in gold （Ⅲ） buffer solution, the current peak signal （I） of the RuL-DNA supramolecular depressed and △I was linear in the concentration range of Au ion from 1×10^-7 to 2×10^-5 mol·L^-1 with a regression coefficient of 0.9879. The detection limit was 5×10^-8 mol·L^-1. The developed procedures were applied to the analysis of synthetic samples of real materials with good sensitivity and selectivity.

Determination of Metamizole Sodium by Cyclic Voltammetry Under Microwave Activation

Microwave radiation was applied to the detection of metamizole sodium by cyclic voltammetry. The electrochemical characteristics of metamizole sodium were studied by cyclic voltammetry at GC electrode under microwave radiation and a considerable current enhancement was observed for metamizole sodium in aqueous 0.05 mol/L H2SO4. Under the optional conditions, metamizole sodium was determined in the absence and presence of microwave activation. In the absence of microwave activation cyclic voltammogram of metamizole sodium shows good linear relationship in a concentration range of 8.0×10^-5-1.0×10^-3 mol/L in aqueous 0.05 mol/L H2SO4 with a detection limit of 6.75× 10^-6 mol/L（S/N=3） and the equation of linear regression is Ip=12.973c-0.1905（R^2=0.9996, n=6）; in the presence of 80 W microwave activation cyclic voltammogram of metamizole sodiumin shows good linear relationship in a concentration range of 4.0× 10^-5-1.0×10^-3 mol/L in aqueous 0.05 mol/L H2SO4 with a detection limit of 4,41 × 10^-6 mol/L（S/N=3） and the equation of linear regression is Ip=25.107c-0.1193（R^2=0.9973, n=7）. The current in the presence of 80 W microwave activation increases to about 2 orders of magnitude compared with that in the absence of microwave activation. The proposed method in the presence of microwave activation showed high selectivity and sensitivity, and the sampling of the disposal method is simple. The method was verified by the determination of Metamizole Sodium tablet with satisfactory results.

Studies on the Voltammetric Behavior of Nicardipine Hydrochloride and its Voltammetric Determination at the Co/GC Modified Electrode

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Square Wave Voltammetry for Analytical Determination of Cadmium in Natural Water Using Ca10(PO4)6(OH)2-Modified Platinum Electrode

This paper reports on the development of a novel electrochemical assay for cadmium (II) in natural water, which involves the use of disposable hydroxyapatite modified platinum electrode (HAP/Pt). Cadmium (II) was preconcentrated on the surface of the modified electrode and adsorbed onto HAP and oxidized at E = –680 mV. The HAP-modified platinum electrode exhibited superior performance in comparison to the plati- num electrode and surprisingly, yielded a higher electrochemical response. The best defined anodic peak was obtained with 0.2 mol L-1 KNO3 pH 5.0 after 25 min of accumulation time. Using these conditions, the cali- bration plot was linear over the range 1 × 10?8 to 5 × 10?6 mol L-1 Cd2+. The precision was examined by car- rying out eight replicate measurements at a concentration of 2.5 ×10?5 mol L-1;the coefficient of variation was 2.9%. The method was applied to the determination of the analyte in river water samples. The interfere- ence of other metal ions on the voltammetric response of Cd(II) was studied. The HAP films was clearly ob- served in the SEM images and characterized by X-ray diffraction, IR spectroscopy and chemical analysis.

Cyclic Voltammetry Determination of Epinephrine with a Nano-gold Modified Glassy Carbon Electrode in the Presence of High Concentration Ascorbic Acid

Nano-gold (NG) modified glassy carbon electrodes (GCEs) were used for determination of epinephrine (EP) in the presence of high concentration ascorbic acid (AA) by cyclic voltammetry (CV). This modified electrode can not only catalytically oxidize EP and AA, but also separate the catalytic peak potentials of EP and AA by about 183.5 mV. In pH = 7.0 ogisogate byffer solution, the linear range of epinephrine was 5 106 ~ 1 ?10-4 mol/L.

Voltammetric sensor based on cobalt-poly(methionine)-modified glassy carbon electrode for determination of estriol hormone in pharmaceuticals and urine

A voltammetric sensor based on the electropolymerization of cobalt-poly(methionine)(Co-poly(Met)) on a glassy carbon electrode (GCE) was developed and applied for the determination of estriol by differential pulse voltammetry (DPV) for the first time. The electrochemical properties of the Co-poly(Met)/GCE were analysed by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) were used to characterize the polymers on the GCE surface. The deposition of the Co-poly(Met) film on the GCE surface enhanced the sensor electronic transfer. CV studies revealed that estriol exhibits an irreversible oxidation peak at t0.58 V for the Co-poly(Met)/GCE (vs. Ag/AgCl reference electrode) in 0.10 mol/L Britton-Robinson buffer solution (pH=7.0). Different voltammetric scan rates (10-200 mV/s) suggested that the estriol oxidation on the Co-poly(Met)/GCE surface is controlled by adsorption and diffusion processes. Based on the optimized DPV conditions, the linear responses for estriol quantification were from 0.596 μmol/L to 4.76 μmol/L (R2 =0.996) and from 5.66 μmol/L to 9.90 μmol/L (R2 =0.994) with a limit of detection (LOD) of 0.0340 μmol/L and a limit of quantification (LOQ) of 0.113 μmol/L. The DPV-Co-poly(Met)/GCE method provided good intra-day and inter-day repeatability with RSD values lower than 5%. Also, no interference of real sample matrices was observed on the estriol voltammetric response, making the DPV-Copoly( Met)/GCE highly selective for estriol. The accuracy test showed that the estriol recovery was in the ranges 96.7%-103% and 98.7%-102% for pharmaceutical tablets and human urine, respectively. The estriol quantification in pharmaceutical tablets performed by the Co-poly(Met)/GCE-assisted DPV method was comparable to the official analytical protocols.

Voltammetric Studies on Heteropoly Phosphotungstovanadate Anions Across the Liquid/Liquid Interface

Electrochemical transfer behavior of V ⅤW 11 -V Ⅴ 3W 9 heteropoly anions on the water/nitrobenzene interface was investigated by means of cyclic voltammetry. The effect of the solution acidity on the transfer behavior and the stable pH range for the heteropoly anions were studied. The stability of mixed tungstovanadate decreases with increasing the number of vanadium atoms. The main transfer species within the potential window have the negative charges of 4 and the transfer process is diffusion controlled. The apparent transfer potential Δ w o Ψ 0 and the free energy Δ G 0 w→o tr for the heteropoly anions can be obtained from the experimental data. For the different anions, the Δ w o Ψ 1/2 pH relationship can be expressed as: Δ w o Ψ 1/2 =constant-53pH.

Voltammetric studies on the interaction of amikacin with methyl blue and its analytical application

A new method to determine the concentration of amikacin （AMK） using methyl blue （MB） as electrochemical probe was developed in this paper. In pH 4.5 Britton-Robinson （B-R） buffer solution, the MB reacted with AMK to form ion association complexes, which led to the reductive peak current of MB at -0.275 V （versus SCE） to decrease, and the decreases were linear with the concentration of AMK in the range of 1.0-60.0 mg/L, the regression of equation is AIp （hA） = -8.48 ＋ 102.36c （rag/L）, correlation coefficient yis 0.997. The conditions for determining the concentration of AMK using linear sweep voltammetry （SLV） were optimized. The method was used to determine the content of amikacin commercially available with satisfactory results.

Electrochemical Determination of Alkaline Phosphatase in Human Serum by Differential Pulse Voltammetry

Differential pulse voltammetry(DPV) was applied to the determination of alkaline phosphatase(ALP) activity in human serum with phenyl phosphate as the substrate. Phenyl phosphate can enzymatically be hydrolyzed to produce phenol which is quantified by DPV at +660 mV(vs.Ag/AgCl) in the concentration range of 2.0_100 μmol/L. The standard curve for ALP is linear over the range from 0.06 to 1000 U/L with a relative standard deviation of 3.0%. The conditions for the enzymatic reaction and voltammetric detection were optimized and the kinetic constants were also examined.The human serum samples were tested by this method and the results were in good agreement with those obtained by the routine p-nitrophenyl phosphate spectrophotometric method.

Carbon Paste Electrode Modified by Surfactant for Anodic Stripping Voltammetric Determination of Sulphadiazine

he present paper covers the construction and behaviour of a mixed binder car-bon paste electrode modified by surfactant system appropriate for the anodic strip-ping voltammetric quantitation of sulphadiazine. The mixed binder consisted ofglycerol and liquid paraffin. On this electrode in a PH 8. 20 buffer solution sulpha-diazine yields a sensitive anodic stripping voltammetric wave at 0. 82 V. It can beused for the determination of trace amounts of drug, the linear range of the peakcurrent to the sulphadiazine concentration being from 1. 0 x 10-7 to 5. 0 x 10-5mol/L, and the detection limit being 6. 6 x 10-9 mol/L with a relative standard de-viation of 2. 6% (n= 15).The proposed method was used to determine the drug inurine samples.