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1.
A novel carbon paste electrode modified with ZnO nanorods and 2-(4-oxo-3-phenyl-3,4-dihydroquinazolinyl)-N′-phenyl-hydrazinecarbothioamide (2PHCZNCPE) was fabricated and employed to study the electrocatalytic oxidation of droxidopa, using cyclic voltammetry, chronoamperometry and square wave voltammetry as diagnostic techniques. It has been found that the oxidation of droxidopa at the surface of modified electrode occurs at a potential of about 435 mV less positive than that of an unmodified carbon paste electrode. Square wave voltammetry exhibits a linear dynamic range from 7.0 × 10–8 to 3.0×10?4 M and a detection limit of 45.0 nM for droxidopa. Finally this modified electrode was used for simultaneous determination of droxidopa and carbidopa.  相似文献   

2.
A new sensor was developed using a screen-printed carbon electrode modified with single-walled carbon nanotubes (SWCNTs) and Prussian blue (PB) coated with chitosan. The modified electrode allowed the oxidation and reduction of rutin at 0.25 and 0.096 V, respectively, with a ΔE of 0.154 V. Furthermore, the peak currents increase nearly 100% compared with the electrode without modification. The process was more reversible compared with the electrode modified with only SWCNTs or PB. Cyclic voltammetry was used to characterize the modified electrode surface. The quantification of rutin was more sensitive with adsorptive stripping voltammetry than with anodic stripping voltammetry. Adsorption potential, adsorption time and pH were optimized based on the oxidation of rutin: Eads =–0.10 V, tads = 60 s, pH 3.0. The detection limit (3σ/b) was 0.01 μM and the relative standard derivation was 3%. The new sensor was used in the quantification of rutin in black tea, coffee and synthetic drink of tea with satisfactory results.  相似文献   

3.
A new composite electrode is described for anodic stripping voltammetry determination of Pb(II) at trace level in aqueous solution. The electrode is based on the use of multiwalled carbon nanotubes and Amberlite IR-120. The anodic stripping voltammograms depend, to a large extent, on the composition of the modified electrode and the preconcentration conditions. Under optimum conditions, the anodic peak current at around ?0.57 V is linearly related to the concentration of Pb(II) in the range from 9.6?×?10?8 to 1.7?×?10?6 mol L?1 (R?=?0.998). The detection limit is 2.1?×?10?8 mol L?1, and the relative standard deviation (RSD) at 0.24?×?10?6 mol L?1 is 1.7% (n?=?6). The modified electrode was applied to the determination of Pb(II) using the standard addition method; the results showed average relative recoveries of 95% for the samples analysed.
Figure
A new composite electrode is described for anodic stripping voltammetry determination of Pb(II) at trace level in aqueous solution. The electrode is based on the use of MWCNT and Amberlite IR-120. The method showed a good linearity for 9.6?×?10?8 - 1.7?×?10?6 mol L?1 and detection limit of 2.1?×?10?8 mol L?1.  相似文献   

4.
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   

5.
The electrochemical behaviour of dacarbazine [5-(3,3-dimethyl-1-triazenyl) imidazole-4-carboxamide; DTIC] was investigated by Tast and differential pulse polarography (d.p.p.) at the dropping mercury electrode, by cyclic and differential pulse voltammetry at the hanging mercury drop electrode and by anodic voltammetry at the glassy carbon electrode. Calibration graphs were obtained for 2×10?8?2×10?5 M DTIC by d.p.p., for 5×10?9?1×10?5 M by adsorptive stripping voltammetry ar a hanging mercury drop electrode, and for 1?10×10?5 M by high-performance liquid chromatography with oxidative amperometric detection at a glassy carbon electrode. The methods are compared and applied to determine DTIC added to blood serum after a simple clean-up procedure.  相似文献   

6.
A carbon paste electrode (CPE) was modified with multi-wall carbon nanotubes and successfully applied to the determination of silver ion by differential pulse anodic stripping voltammetry. Compared to a conventional CPE, a remarkably improved peak current response and sensitivity is observed. The analytical procedure consisted of an open circuit accumulation step for 2?min in ?0.4?V, this followed by an anodic potential scan between +0.2 and?+?0.6?V to obtain the voltammetric peak. The oxidation peak current is proportional to the concentration of silver ion in the range from 1.0?×?10?8 to 1.0?×?10?5?mol?L?1, with a detection limit of 1.8?×?10?9?mol?L?1 after an accumulation time of 120?s. The relative standard deviation for 7 successive determinations of Ag(I) at 0.1???M concentration is 1.99%. The procedure was validated by determining Ag(I) in natural waters.
Figure
Differential pulse voltammogram (DPV) of Ag+ solution at MCPE  相似文献   

7.
A film of single-wall carbon nanotubes (SWNTs) and didodecyldimethylammonium bromide (DDAB) is prepared by casting a solution of SWNTs and DDAB onto the surface of a gold electrode. The electrochemical behavior of the film is investigated by electrochemical impedance spectroscopy and cyclic voltammetry. In a 0.10 M phosphate buffer solution of pH 7.0, the film-modified electrode gives a pair of redox peaks in cyclic voltamograms, with the anodic and cathodic peak potentials of 0.095 and 0.042 V. The peak currents change linearly with the scan rate at 30–500 mV/s. The modified electrode has an excellent electrocatalytic activity towards the oxidation of ascorbic acid (AA). The catalysis currents are proportional to the AA concentration in the range of 5.0 × 10−4 to 3.2 × 10−2 M. The linear-regression equation is i (μA) = 1.2079 + 1.3987 × 103 c AA (M), with a correlation coefficient of 0.9995. The detection limit is 2.2 × 10−4 M (signal-to-noise ratio of 3). The Michaelis-Menten constant (K m) is 1.0 × 10−4 M by the Lineweaver-Burk equation. __________ From Elektrokhimiya, Vol. 41, No. 10, 2005, pp. 1193–1199. Original English Text Copyright ? 2005 by Cheng, Jin, Zhang. The text was submitted by the authors in English.  相似文献   

8.
Flavoxate hydrochloride, 2-piperidinoethyl 3-methyl-4-oxo-2-phenyl-4-H-chromene-8-carboxylate, is a smooth muscle antispasmodic. Its electrochemical behavior was studied at the mercury electrode in buffered solutions containing 30% (v/v) methanol using dc-polarography, differential-pulse polarography, cyclic voltammetry, and linear sweep-and square-wave adsorptive stripping voltammetry. Sensitive and precise procedures were developed for determination of bulk flavoxate hydrochloride and in the pharmaceutical formulation Genurin® S.F, without sample pretreatment or extraction. Limits of quantitation (LOQ) of 1 × 10?5, 5 × 10?6, 1 × 10?8 and 1 × 10?9 M flavoxate hydrochloride were achieved by dc-polarography, differential-pulse polarography, linear sweep and square-wave adsorptive stripping voltammetric, respectively.   相似文献   

9.
We describe a silver(I)-selective carbon paste electrode modified with multi-walled carbon nanotubes and a silver-chelating Schiff base, and its electrochemical response to Ag(I). Effects of reduction potential and time, accumulation time, pH of the solution and the stripping medium were studied by differential pulse anodic stripping voltammetry and optimized. The findings resulted in a method for the determination of silver over a linear response range (from 0.5 to 235 ng?mL?1) and with a detection limit as low as 0.08 ng?mL?1. The sensor displays good repeatability (with the RSD of ±?2.75 % for 7 replicates) and was applied to the determination of Ag(I) in water samples and X-ray photographic films.
Figure
Open circuit accumulation of Ag(I) onto a surface of EHPO-MCPE and determination by Differential pulse anodic stripping voltammetry  相似文献   

10.
The electrochemical behavior of vardenafil HCl (VRL) at a carbon paste electrode (CPE) was investigated by cyclic voltammetry, and the mechanism of its oxidation was suggested and discussed. A simple Nujol-based CPE in combination with a sensitive square-wave adsorption anodic stripping voltammetry method was described for trace determination of VRL. The described method showed excellent performance for trace determination of VRL in its formulation “Levitra® tablets” without interference from excipients. The results were statistically compared with those obtained with an established HPLC method; nonsignificant differences were found between the described voltammetric and HPLC methods. The described stripping voltammetric method is highly sensitive (limit of detection?=?3?×?10?10?mol?L?1 and limit of quantitation?=?1?×?10?9?mol?L?1). It was successfully applied for the determination of VRL in spiked human serum without the necessity for pretreatment and/or time-consuming extraction steps prior to the analysis.  相似文献   

11.
Poly(o-toluidine) (sodium dodecyl sulfate) (POT(SDS)) film was electrosynthesized on carbon paste electrode (CPE) by using the cyclic voltammetry technique in aqueous solution containing o-toluidine (OT), sulfuric acid and SDS. Then, copper oxide was incorporated by immersion of POT(SDS)/CPE in a solution of copper sulfate and using constant potential method. Then, the electrochemical characterization of the modified electrode is presented in alkaline solution. For the first time, electrochemical behaviour of amoxicillin (AMX) at the Cu/POT(SDS)/CPE has been investigated using cyclic voltammetry (CV) and chronoamperometric method. The experimental results suggest that the modified electrode exhibits electrocatalytic effect on the oxidation of AMX resulting in a marked enhancement of the anodic peak current response. Under the selected conditions, the anodic peak current was linearly dependent on the concentration of AMX in the range 80–200 and 5–150 μM with CV and amperometric method, respectively. The detection limits (2δ) were also estimated to be 60 and 3 μM. Some kinetic parameters such as the transfer second-order rate constant (k = 4.9 × 106 cm3 mol–1 s–1) of AMX was calculated. Therefore, this modified electrode was a simple, rapid and new electrode to determine AMX in pharmaceutical preparations.  相似文献   

12.
A carbon paste electrode, modified with N,N′-bis-(2-hydroxy-1-naphthalidene)ethylenediamine and multi-walled carbon nanotubes (HNED-MWCNPE), was used for the determination of acetaminophen (ACOP) and propranolol (PP). Cyclic voltammetry (CV), chronocoulometry, chronoamperometry and differential pulse voltammetry (DPV) techniques were employed to study electro-oxidation of ACOP. The results revealed that the modified electrode showed an electrocatalytic activity toward the anodic oxidation of acetaminophen by a marked enhancement in the current response in buffered solution at pH 8.0. Some kinetic parameters such as the electron transfer coefficient (α) were also determined for the ACOP oxidation. The linear concentration range of 1 × 10?3?1 × 10?6 M with a detection limit of 4.6 × 10?8 M (n = 16) for ACOP was obtained using DPV (pH 8.0). The modified electrode shows good sensitivity, selectivity and stability. The prepared electrode was also applied for the determination of ACOP in human blood serum.  相似文献   

13.
《Electroanalysis》2006,18(2):158-162
Optimum conditions have been found for voltammetric determination of mutagenic 5‐aminoquinoline, 6‐aminoquinoline and 3‐aminoquinoline by differential pulse voltammetry and adsorptive stripping differential pulse voltammetry on carbon paste electrode. The lowest limits of determination were found for adsorptive stripping differential pulse voltammetry in 0.1 mol dm?3 H3PO4 (5×10?7 mol dm?3 , 1×10?7 mol dm?3, and 1×10?7 mol dm?3 for 5‐aminoquinoline, 6‐aminoquinoline and 3‐aminoquinoline, respectively). The possibility to determine mixtures of 8‐aminoquinoline with 3‐aminoquinoline or 5‐aminoquinoline or 6‐aminoquinoline, and mixtures of 5‐aminoquinoline with 3‐aminoquinoline or 6‐aminoquinoline by differential pulse voltammetry was verified. Binary mixtures of 8‐aminoquinoline with 3‐aminoquinoline or 6‐aminoquinoline, and of 3‐aminoquinoline with 5‐aminoquinoline could be successfully analyzed.  相似文献   

14.
This research introduces the design of an adsorptive stripping voltammetric method for the cerium(III) determination at a carbon paste electrode, chemically modified with dipyridyl‐functionalized nanoporous silica gel (DPNSG‐CPE). The electroanalytical procedure comprised two steps: the Ce(III) chemical accumulation at ?200 mV followed by the electrochemical detection of the Ce(III)/dipyridyl complex, using anodic stripping voltammetry. The factors, influencing the adsorptive stripping performance, were optimized including the modifier quantity in the paste, the electrolyte concentrations, the solution pH and the accumulation potential or time. The resulting electrode demonstrated a linear response over a wide range of Ce(III) concentration (1.0–28 ng mL?1). The precision for seven determinations of 4 and 10 ng mL?1 Ce(III) was 3.2% and 2.5% (relative standard deviation), respectively. The prepared electrode was used for the cerium determination in real samples and very good recovery results were obtained.  相似文献   

15.
A glassy carbon electrode (GCE) modified with carbon Printex 6L (Printex6L/GCE) as a novel sensor is proposed. A morphological study was carried out using scanning electron microscopy, and an electrochemical characterization of the proposed electrode was performed by cyclic voltammetry (CV) using [Fe(CN)6]4? as a redox probe. With the incorporation of the carbon Printex 6L film onto the GCE surface, the [Fe(CN)6]4? analytical signal was substantially increased and the difference between the oxidation and reduction potentials (ΔE p) decreased, a characteristic of the electrocatalytic effect. Furthermore, the use of carbon Printex 6L film resulted in an 84 % increase in the oxidation current and a 123 % increase in the reduction current. Faster charge transfer was observed at the proposed electrode/electrolyte interface during CV when compared with GCE. The Printex6L/GCE was tested for ranitidine (RNT) sensing and showed a decrease in the working potential and an increase in the analytical signal, when compared with GCE, again demonstrating an electrocatalytic effect. Under optimized experimental conditions, the developed square-wave adsorptive anodic stripping voltammetry (SWAdASV) method presented an analytical curve that was linear in RNT concentration range from 1.98 × 10?6 to 2.88 × 10?5 mol L?1 with a detection limit of 2.44 × 10?7 mol L?1. The developed Printex6L/GCE was successfully applied to the determination of RNT concentrations in human body fluid samples (urine and serum).  相似文献   

16.
The adsorptive stripping voltammetry of telmisartan was investigated with a hanging mercury drop electrode. This compound produced a catalytic hydrogen wave at ?1.5 V in Britton Robinson buffer of pH 10.38, and the peak current increased with adsorptive accumulation at the electrode. Adsorptive stripping voltammetry with the catalytic hydrogen wave could provide a sensitive novel method for the determination of telmisartan. Various chemical and instrumental parameters affecting the monitored electroanalytical response were investigated and optimized for telmisartan determination. Under these optimized conditions the square-wave adsorptive stripping voltammetric (SW-AdSV) peak current showed a linear dependence on drug concentration over the range 0.05–3.00 μg/mL (1 × 10?7?6 × 10?6 M) (r = 0.999) with accumulation for 120 s at ?1.0 V vs. Ag/AgCl. The proposed electrochemical procedure was successfully applied for the determination of telmisartan in pharmaceutical tablets and human plasma. The results of the developed SW-AdSV method were comparable with those obtained by reported analytical procedures.  相似文献   

17.
《Analytical letters》2012,45(9):1750-1762
Abstract

The interaction between clozapine (CLZ) as an orally administrated antipsychotic drug with double stranded calf thymus DNA (dsDNA) was investigated at electrode surface using differential pulse voltammetry (DPV). Activated carbon paste electrode (CPE) was modified with dsDNA and used for monitoring the changes of the characteristics peak of CLZ in 0.05 M acetate buffer (pH 4.3). The adsorptive stripping voltammetry on dsDNA‐modified carbon paste electrode (dsDNA‐CPE) was used for determination of very low concentration of CLZ. Under optimal conditions, the oxidation peak current is proportional to CLZ concentration in the range of 7×10?9?1.2×10?6 mol l?1 with a detection limit of 1.5×10?9 mol l?1 for 180 s accumulation time by DPV. The proposed dsDNA‐CPE was successfully used for determination of CLZ in human serum samples with recovery of 97.0±2.5%.  相似文献   

18.
《Analytical letters》2012,45(9):763-774
Abstract

The various problems which are associated with the use of carbon paste electrode as thin mercury film electrode (TKFE) for anodic stripping voltammetry (ASV) can be overcame in a very easy and rapid way. The procedure consists to coat the carbon paste surface by spraying a graphite based conductive solution. For example, the dispersion of colloidal graphite in a mixture of methyl polymethacrylate with butyl acetate (as solvent) gives interesting results. Such a surface is easily renewable and the electrode does not require any pretreatment procedure like cleaning or polarization cycles…, after coating. The technique offers the advantage to limit the risk of sample contamination and memory effects. After pulverisation, a hard, uniform and compact layer is formed after evaporation of the solvent excess.

The resulting electrode, electrochemically coated with mercury, exhibits a good stability as shown for the differential pulse anodic stripping voltammetry (DPASV) for cadmium ions. Replicate measurements were carried out in two different buffers at pH 8.5 and 5.0. Compared to the originally carbon paste electrode, a marked improvement of the reproducibility of the peak currents is observed. Calibration curves obtained by using the method of standard additions show a good linear relationship between cadmium ions concentration and peak current (down to 4×10?10 M.L?1).

After a deposition time of 10 minutes, the detection limit for cadmium is 1×10?10 M.L?l in both media).  相似文献   

19.
A novel carbon paste electrode modified with ZrO2 nanoparticles and an ionic liquid (n-hexyl-3- methylimidazolium hexafluorophosphate) was fabricated. The electrochemical study of the modified electrode, as well as its efficiency for simultaneous voltammetric oxidation of dopamine and uric acid is described. The electrode was also employed to study the electrochemical oxidation of dopamine and uric acid, using cyclic voltammetry, chronoamperometry and square wave voltammetry as diagnostic techniques. Square wave voltammetry exhibits linear dynamic range from 1.0 × 10?6 to 9.0 × 10?4 M for dopamine. Also, square wave voltammetry exhibits linear dynamic range from 9.0 × 10?6–1.0 × 10?3 M for uric acid. The modified electrode displayed strong function for resolving the overlapping voltammetric responses of dopamine and uric acid into two well-defined voltammetric peaks. In the mixture containing dopamine and uric acid, the two compounds can be well separated from each other with potential difference of 155 mV, which is large enough to determine dopamine and uric acid individually and simultaneously. Finally, the modified electrode was used for determination of dopamine and uric acid in real samples.  相似文献   

20.
Oxine (8-hydroxyquinoline) was used as an efficient and selective ligand for stripping voltammetry trace determination of Mn(II). A validated square-wave adsorptive cathodic stripping voltammetry method has been developed for determination of Mn(II) selectively as oxine complex using both the bare carbon paste electrode (CPE) and the modified CPE with 7 % (w/w) montmorillonite-Na clay. Modification of carbon paste with montmorillonite clay was found to greatly enhance its adsorption capacity. Limits of detection of 45 ng l?1 (8.19?×?10?10 mol L?1) and 1.8 ng l?1 (3.28?×?10?11 mol L?1) Mn(II) were achieved using the bare and modified CP electrodes, respectively. The achieved limits of detection of Mn(II) as oxine complex using the modified CPE are much sensitive than the detection limits obtained by most of the reported electrochemical methods. The developed stripping voltammetry method using both electrodes was successfully applied for trace determination of Mn(II) in various water samples without interferences from various organic and inorganic species.  相似文献   

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