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1.
《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   

2.
A sensitive adsorptive stripping voltammetric method for the determination of dinitrophenolic herbicides, dinoseb (DSB) and dinoterb (DTB) at a bare carbon paste electrode (CPE) and a clay modified carbon paste electrode (CMCPE) was developed. A systematic study of various experimental conditions, such as the pH, accumulation variables and composition of a modifier on the adsorptive stripping response, were examined by using differential pulse voltammetry. A significant improvement was observed in the sensitivity by using the present method with CMCPE. When CMCPE was used, a linear response was obtained over the concentration range 2 x 10(-10) to 3 x 10(-7) M and 6 x 10(-10) to 6 x 10(-7) M with lower detection limits of 1 x 10(-10) M and 5.4 x 10(-10) M for dinoseb and dinoterb, respectively, at an accumulation time of 100 s. The interference from other herbicides and ions on the stripping signals of both compounds was also evaluated. The described method was applied to estimate of the dinoseb and dinoterb in environmental samples.  相似文献   

3.
《Analytical letters》2012,45(13):2402-2411
Abstract

Porous pseudo-carbon paste electrode (PPCPE) as a novel high-sensitive electrochemical biosensor was fabricated by mixing polymethyl methacrylate (PMMA) microspheres for use as the template, graphite powders for the filler, and pyrrole as the precursor of the polymer which acted as the paste. After the polymerization of pyrrole catalyzed by Fe3+, the PMMA microspheres were removed to form PPCPE. The pore size was determined by SEM observations, with diameters ranging from 2 to 5 µm. The anodic stripping voltammetry response of DNA indicated that the adsorption of oligonucleotide on PPCPE was enhanced. The PPCPE was easy to preserve and had a good reusability in comparison with that of a pure carbon paste electrode (CPE) and a carbon nanotube-modified carbon paste electrode (CNTPE). The detection limits of guanine and adenine were 20 nM and 8 nM, respectively.  相似文献   

4.
《Analytical letters》2012,45(5):763-777
A multiwall carbon nanotube titanium dioxide nanoparticle modified carbon paste electrode was used for direct determination of methimazole. The nanoparticles in the carbon paste increased the surface area of the electrode and improved the sensitivity by enhancing the peak current. The electrochemical behavior of methimazole on the modified electrode was investigated. Experimental variables such as pH and electrode composition were optimized. At the optimum pH 7.0 (universal buffer), the modified electrode had a linear dynamic range of 0.5 to 100.0 μmol L? 1 (0.1–11.4 ppm) with a limit of detection of 0.17 μmol L? 1 . The application of the electrode for the determination of methimazole in pharmaceuticals and blood serum was investigated.  相似文献   

5.
《Analytical letters》2012,45(5-6):436-448
This work reports the determination of bisphenol A (BPA) released from baby feeding bottles by adsorptive stripping voltammetry on a diphenylether carbon paste electrode (DPE-CPE). BPA was as accumulated on the surface of the DPE-CPE by an adsorptive/extractive mechanism at ?0.20 V in B-R buffer at pH 7.0. Following pre-concentration, an anodic scan was applied in the range ?0.20 V to +1.00 V during which BPA was oxidized and the oxidation peak current was related to the BPA concentration in the sample. The parameters related to both the preconcentration and stripping step were investigated. Using the selected conditions, the limit of detection for BPA was 7.8 × 10?9 mol L?1 at a preconcentration time of 240 s and the % relative standard deviation was 4.2% for 6.7 × 10?7 mol L?1 of BPA (n = 8). The proposed method was applied to the determination of BPA leaching from polycarbonate baby feeding bottles under simulated conditions of typical use. The results compared well with those obtained with liquid chromatography-tandem mass spectrometry (LC-MS/MS).  相似文献   

6.
《Analytical letters》2012,45(16):3119-3128
Abstract

This paper describes the preparation and electrochemical application of a modified carbon paste electrode with chitosan for the determination of Hg(II) ions in water using anodic stripping voltammetry. Experimental parameters, including the pH of the supporting electrolyte, time and potential of accumulation and scan rate were investigated. The best voltammetric response was observed for a paste composition of 60% (m/m) of graphite powder, 20% (m/m) of chitosan and 20% (m/m) of mineral oil, with 0.1 mol/l NaNO3 solution at pH 6.3 as supporting electrolyte, a preconcentration potential of ?0.2 V, preconcentration time of 270 s and a scan rate of 25 mV/s. Under these optimal experimental conditions, the voltammetric signals were linearly dependent on the Hg(II) concentration in the range of 9.99×10?7 to 3.85×10?5 mol/l with a detection limit of 6.28×10?7 mol/l. Three “spiked” samples of water were evaluated using the proposed sensor, and results agreed with those obtained by a reference method at the 95% confidence level.  相似文献   

7.
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   

8.
The aim of this work was to obtain an adsorptive stripping voltammetric method for the Ce(III) determination at a carbon paste electrode, chemically modified with N'‐[(2‐hydroxyphenyl)methylidene]‐2‐furohydrazide (NHMF). The electroanalytical procedure comprised two steps: the Ce(III) chemical accumulation at ?200 mV followed by the electrochemical detection of the Ce(III)/NHMF 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 (5.0–90 nmol dm?3). The detection limit was found to be 0.8 nmol dm?3 on the basis of a signal to noise ratio of 3. The precision for six determinations of 10 and 55 nmol dm?3 Ce(III) was 5.6% and 2.1% (relative standard deviation), respectively. Application of the procedure to the determination of cerium in phosphate rock and wastewater samples gave good results.  相似文献   

9.
《Analytical letters》2012,45(14):2643-2655
Abstract

A carbon paste electrode modified with organically functionalized silica was used for the determination of lead. The measurements were carried out in three steps including an open circuit accumulation followed by electrolysis of accumulated lead at the carbon paste electrode and differential pulse voltammetric determination. The effects of several experimental variables such as carbon paste composition, pH and concentration of supporting electrolyte, electrolysis potential, and electrolysis time were studied. The resulting electrode demonstrates linear response over a wide range of Pb(II) concentration (5–1000 ng mL?1) with an accumulation time of 60 sec. The effects of potential interfering ions were studied, and it was found that the proposed procedure is free from most interferences. Long lifetime and rapid and convenient renewal of electrode surface allows the use of a single modified electrode surface in multiple analytical determinations over at least 4 months. The prepared electrode was used for determination of lead spiked in a hair sample, and very good recovery results were obtained over a wide concentration range of lead.  相似文献   

10.
《Analytical letters》2012,45(13):2247-2258
Abstract

The electrochemical behavior of the quercetin (Q) at a carbon paste electrode (CPE) containing 15% paraffin oil is investigated. Square wave anodic stripping voltammetric (SWASV) was used to determine quercetin in the presence of 0.04 M phosphate buffer (pH ~4) containing 0.1 M KCl with 15 s accumulation time at 25±1°C. Under the optimal experimental conditions, the adsorbed form is oxidized irreversibly. The linear concentration ranged from 67.66 to 338.3 ppb quercetin. The detection limit of 6.77 ppb Q (r=0.9997), with 15 s accumulation time and the relative standard deviation of 0.45 (n=5) was calculated. The interferences of some metal ions and some amino acids were studied. The method was applied to the analysis of spiked urine, with recovery of 99.9±0.5, and the relative standard deviation of 3.2%. Results were compared with the reported methods.  相似文献   

11.
《Electroanalysis》2006,18(5):507-512
A coumestan derivative modified carbon paste electrode (CMCPE) was used as a sensitive electrochemical sensor for determination of electrocatalytic of hydrazine and hydroxylamine. The mechanism of electrocatalytic oxidation of both hydrazine and hydroxylamine using CMCPE was investigated by cyclic voltammetry and polarization studies. The kinetic parameters such as the electron transfer coefficient, α, heterogeneous rate constant, k′, and exchange current density, j0, for oxidation of hydrazine and hydroxylamine at the CMCPE surface were determined using cyclic voltammetry. Further more, the linear dynamic range, sensitivity and limit of detection for hydrazine and hydroxylamine detections were evaluated using differential pulse voltammetry.  相似文献   

12.
A. Radi 《Mikrochimica acta》1999,132(1):49-53
 The electrochemical oxidation of nicergoline is investigated using cyclic and differential pulse voltammetry at a carbon paste electrode. For the determination of nicergoline an adsorptive stripping procedure is proposed. The response is characterized with respect to pH, ionic strength, preconcentration time, accumulation potential, nicergoline concentration, reproducibility and other variables. By differential pulse voltammetry at a carbon paste electrode and pH 8.0, a linear calibration in the range 5×10−8 M to 1×10−7 M and a detection limit of 1×10−8 M are obtained. The preconcentration medium-exchange approach was used for a selective determination of nicergoline in urine. For dilute urine samples a detection limit of 5×10−8 M is obtained after 3 min of accumulation and medium-exchange. The procedure also is applied for the determination of nicergoline in dosage form. Received August 24, 1998. Revision April 8, 1999.  相似文献   

13.
This environmentally benign work describes a simple electrochemical sensor constructed with a chemically modified carbon paste electrode (CMCPE) using aloe vera xanthate nanoparticles to detect mercury ions. The characterization and morphology of nanoparticles were thoroughly investigated using modern techniques. The CMCPE efficiently senses the mercury ions. The limit of detection of mercury ions wasexcellent to the order of 0.231 μg mL−1. Real-time sample analysis showed promising results. The recovery range was between 99.4 % and 101.7 %. The activity of CMCPE was commendable even after fifty days.  相似文献   

14.
The electrooxidation of the antitumour drug 2-methyl-9-hydroxyellipticinium (Celiptium) was investigated by cyclic, differential-pulse and adsorptive voltammetry at carbon paste (CPE) and lipid-modified carbon paste electrodes (LM-CPE). The influence of the paste composition, i.e., the ratio of graphite to binder, was studied in order to elucidate the nature of the accumulation process at the surface of the CPE. The electrode surface coverage at saturation was calculated. A.c. measurements at the CPE and at the LM-CPE during the accumulation of Celiptium demonstrated an increased differential double layer capacity of the LM-CPE. The influence of several parameters that affect the adsorptive step at the CPE was investigated, such as pH, ionic strength and interfering ions. Improved signals were obtained at the CPE and the detection limit in 0.1 M sodium perchlorate (tacc.=3 min) was found to be 2 × 10?10 M. Measurements of the drug in dilute standard serum samples were done using the medium-exchange technique.  相似文献   

15.
A lead film plated in situ at a carbon paste support was tested as a novel, potential electrode for adsorptive stripping voltammetric determination of cobalt traces in an ammonia buffer solution. To show the practical applicability of the new electrode, a catalytic adsorptive Co system in a supporting electrolyte containing 0.1 M ammonia buffer, 5×10?4 M nioxime and 0.25 M nitrite was selected and investigated as a model solution. Pb and Co ions were simultaneously accumulated in situ on the electrode surface: Pb ions electrochemically at ?1.3 V) and then at ?0.75 V, at which potential the Co(II)‐nioximate complex was also pre‐concentrated via adsorption. Instrumental parameters, such as the time of nucleation and formation of Pb film deposits, the time of accumulation of the Co‐nioxime complex at the PbF/CPE, and the procedures of electrode regeneration, were optimized to obtain good reproducibility and sensitivity of the Co response. The optimized procedure yields favorable and highly stable stripping responses with good precision (RSD=3% for a 5×10?8 M Co) and good linearity (up to 5×10?7 M, coefficient of determination, R=0.996). The detection limit was 4×10?10 M Co (0.023 μg L?1) for an accumulation time of 120 s. The method enables the determination of Co in the presence of high excesses of Ni or Zn. The voltammetric data were correlated with the structural characterization by scanning electron microscopy (SEM) and X‐ray fluorescence spectroscopy (XRF).  相似文献   

16.
《Analytical letters》2012,45(10):2032-2044
Abstract

A stripping method for the determination of cysteine in the presence of copper at the submicromolar concentration levels is described. The method is based on controlled adsorptive accumulation of cysteine at mercury film electrode followed by linear cyclic voltammetry scan measurement of the surface species. Optimum experimental conditions were found to be the use of a 1×10?3 M NaOH solution, an accumulation potential of ?0.50 V and a scan rate of 200 mV. s?1. The response of cysteine is linear over the concentration range 0.04–0.20 ppm. For an accumulation time of 15 minutes, the detection limit was found to be 0.9 ppb (7.4×10?9 M). The more convenient relation to measuring the cysteine in presence of metals, and others amino acids were also investigated. The utility of the method is demonstrated by presence of casein and ATP.  相似文献   

17.
《Analytical letters》2012,45(16):2665-2682
Abstract

The oxidation of theophylline was studied at a carbon paste electrode in the presence of cetyltrimethyl ammonium bromide by cyclic and differential pulse voltammetry. The results indicated that the electrochemical responses of theophylline are apparently improved by cetyltrimethyl ammonium bromide, due to the enhanced accumulation of theophylline at carbon paste electrode surface. Under optimal conditions the peak current was proportional to theophylline concentration in the range of 8.0 × 10?7 to 2.0 × 10?4 M with a detection limit of 1.85 × 10?7 M by differential pulse voltammetry. The proposed method was applied to the determination of theophylline in tablet and urine samples.  相似文献   

18.
碳糊电极阳极吸附伏安法测定环丙沙星   总被引:6,自引:0,他引:6  
易兰花  王俊芬  黎拒难  高朋 《化学研究》2005,16(1):59-61,75
报道了用碳糊电极阳极吸附伏安法测定环丙沙星的新方法.在 0. 40mol/L的NH4Ac HAc(pH4. 30)缓冲液中,使用JP 303极谱分析仪,环丙沙星在碳糊电极 (CPE)上有一灵敏的吸附伏安氧化峰,峰电位为1. 12V(vs.SCE).该氧化峰的二阶导数峰电流与环丙沙星的浓度在 8. 0×10-9 ~8. 0×10-7 mol/L(富集 90s)范围内成良好的线性关系,相关系数为 0. 998 8,检出限为 4. 0×10-9 mol/L(S/N=3,富集 110s).探讨了环丙沙星在碳糊电极上的伏安性质和电极反应机理,并且成功应用于人体尿样中环丙沙星含量的测定.加入回收实验,回收率在95. 5%至 103. 9%之间.  相似文献   

19.
ABSTRACT

A modified carbon paste electrode has been developed for the determination of Pb(ΙΙ) ions based on Fe3O4/eggshell magnetic nanocomposite. The structure and morphology of Fe3O4/eggshell were analysed by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The prepared nanocomposite was also characterized by Fourier transform infrared spectroscopy (FT-IR) and vibrating sample magnetometer (VSM). The electrochemical procedure was based on the accumulation and determination of Pb(ΙΙ) ions at the surface of the modified carbon paste electrode with Fe3O4/eggshell nanocomposites and carbon nanotubes by differential pulse anodic stripping voltammetry (DPASV). Various experimental parameters involved in the preconcentration of Pb(ΙΙ) ions and voltammetric stripping step were studied. Under the optimum conditions, the voltammetric peak current of Pb(ΙΙ) occurs at a potential about ?0.5 V. Also, the voltammetric peak current increased linearly with Pb(ΙΙ) concentration in the range of 0.5–200 ng mL?1 and a detection limit of 0.15 ng mL?1 was obtained for Pb(ΙΙ). The selectivity of the proposed electrode for Pb(ΙΙ) ions in the presence of some cations was also examined. The practical application of the proposed modified electrode was evaluated by the determination of Pb(ΙΙ) ions in human hair and water samples. The results were satisfactory for the spiked samples.  相似文献   

20.
A new method for the determination of trace copper was described. A multiwalled carbon nanotube modified carbon paste electrode was prepared and the adsorptive voltammetric behavior of copper‐alizarin red S (ARS) complex at the modified electrode was investigated. By use of the second‐order derivative linear sweep voltammetry, it was found that in 0.04 mol/L acetate buffer solution (pH 4.2) containing 4×10?6 mol/L ARS, when accumulation potential is 0 mV, accumulation time is 60 s and scan rate is 100 mV/s, the complex can be adsorbed on the surface of the electrode, yielding one sensitive reduction peak at ?172 mV (vs. SCE). The peak current of the complex is proportional to the concentration of Cu(II) in the range of 2.0×10?11–4.0×10?7 mol L?1 with a detection limit (S/N=3) of 8.0×10?12 mol/L (4 min accumulation). The proposed method was successfully applied to the determination of copper in biological samples with satisfactory results, the recoveries were found to be 96%–102%.  相似文献   

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