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1.
The present study addresses the electrochemical behavior and the analytical applications of six 2-nitrophenylbenzimidazole derivatives with activity against Trypanosoma cruzi. When studied in a wide range of pH, by differential pulse polarography, tast polarography and cyclic voltammetry, these compounds exhibited two irreversible cathodic responses. With analytical purposes, the differential pulse polarography mode was selected, which exhibited adequate analytical parameters of repeatability, reproducibility and selectivity. The percentage of recovery was in all cases over 99%, and the detection and quantitation limits were at the level of 1 × 10−7 mol L−1 and 1 × 10−6 mol L−1, respectively. In addition, the differential pulse polarography method was successfully applied to study the hydrolytic degradation kinetic of one of the tested compounds. Activation energy, kinetic rate constants at different temperatures and half-life values of such application are reported.  相似文献   

2.
Mehretie S  Admassie S  Hunde T  Tessema M  Solomon T 《Talanta》2011,85(3):1376-1382
A sensitive and selective method was developed for the determination of N-acetyl-p-aminophenol (APAP) and p-aminophenol (PAP) using poly(3,4-ethylenedioxythiophene) (PEDOT)-modified glassy carbon electrode (GCE). Cyclic voltammetry and differential pulse voltammetry were used to investigate the electrochemical reaction of APAP and PAP at the modified electrode. Both APAP and PAP showed quasireversible redox reactions with formal potentials of 367 mV and 101 mV (vs. Ag/AgCl), respectively, in phosphate buffer solution of pH 7.0. The significant peak potential difference (266 mV) between APAP and PAP enabled the simultaneous determination both species based on differential pulse voltammetry. The voltammetric responses gave linear ranges of 1.0 × 10−6-1.0 × 10−4 mol L−1 and 4.0 × 10−6-3.2 × 10−4 mol L−1, with detection limits of 4.0 × 10−7 mol L−1 and 1.2 × 10−6 mol L−1 for APAP and PAP, respectively. The method was successfully applied for the determination of APAP and PAP in pharmaceutical formulations and biological samples.  相似文献   

3.
Hu YF  Zhang ZH  Zhang HB  Luo LJ  Yao SZ 《Talanta》2011,84(2):305-313
A sensitive and selective electrochemical sensor based on a polyaniline modified carbon electrode for the determination of l-phenylalanine has been proposed by utilizing β-cyclodextrin (β-CD) incorporated multi-walled carbon nanotube (MWNT) and imprinted sol-gel film. The electrochemical behavior of the sensor towards l-phenylalanine was investigated by cyclic voltammetry (CV), differential pulse voltammetry (DPV), and amperometric i-t curve. The surface morphologies of layer-by-layer assembly electrodes were displayed by scanning electron microscope (SEM). The response mechanism of the imprinted sensor for l-phenylalanine was based on the inclusion interaction of β-CD and molecular recognition capacity of the imprinted film for l-phenylalanine. A linear calibration plot was obtained covering the concentration range from 5.0 × 10−7 to 1.0 × 10−4 mol L−1 with a detection limit of 1.0 × 10−9 mol L−1. With excellent sensitivity, selectivity, stability, reproducibility and recovery, the electrochemical imprinted sensor was used to detect l-phenylalanine in blood plasma samples successfully.  相似文献   

4.
A carboxyl functionalized graphene oxide (GO-COOH) and electropolymerized ploy-l-lysine (PLLy) modified glassy carbon electrode (GCE) was fabricated and used for the construction of an electrochemical deoxyribonucleic acid (DNA) biosensor. The NH2 modified probe ssDNA sequences were immobilized on the surface of GO-COOH/PLLy/GCE by covalent linking with the formation of amide bonds, which was stable and furthur hybridized with the target ssDNA sequence. Differential pulse voltammetry (DPV) was used to monitor the hybridization events with methylene blue as electrochemical indicator, which gave a sensitive reduction peak at −0.287 V (vs. SCE). Under the optimal conditions the reduction peak current was proportional to the concentration of tlh gene sequence in the range from 1.0 × 10−12 to 1.0 × 10−6 mol L−1 with a detection limit as 1.69 × 10−13 mol L−1 (3σ). The polymerase chain reaction products of tlh gene from oyster samples were detected with satisfactory results, indicating the potential application of this electrochemical DNA sensor.  相似文献   

5.
M. Pérez-Ortiz 《Talanta》2010,82(1):398-630
In this work, the electrochemical behavior and the analytical application of atomoxetine, a selective noradrenaline reuptake inhibitor, are studied. Atomoxetine, studied by differential pulse voltammetry and cyclic voltammetry on a glassy carbon electrode, exhibited an anodic response in aqueous media with pH between 1.5 and 7. In non-aqueous medium (acetonitrile), the drug exhibited two irreversible oxidation peaks that are diffusion controlled. From chronocoulometric studies in acetonitrile, it was determined that each oxidation signal involves two and four electrons, respectively. For analytical purposes, a differential pulse voltammetry technique in 0.1 mol L−1 perchloric acid was selected, which exhibited adequate figures of merit. The percent recovery was 96.6 ± 1.2 and the detection and quantitation limits were 6.9 × 10−5 and 1.0 × 10−4 mol L−1, respectively. Also, results indicate that excipients do not interfere with the oxidation signal of atomoxetine, which leads to the conclusion that the developed method is satisfactorily selective for atomoxetine quantification in pharmaceuticals with no prior separation or extraction necessary. Finally, the proposed voltammetric method was successfully applied to both the assay and the uniformity content of atomoxetine in capsules. For comparison, high-performance liquid chromatography analysis was also performed.  相似文献   

6.
Yang Wang  Guojun Yao  Peihua Zhu  Xiaoya Hu  Qin Xu 《Talanta》2010,82(4):1500-2527
The analytical performance of lab-on-valve (LOV) system using irreversible biamperometry for the determination of catechol was evaluated. By integrating miniaturized electrochemical flow cell (EFC) designed and processed which is furnished with two identical polarized platinum electrodes, into the LOV unit, the lab-on-valve system combines sampling with analysis, realizing automated on-line analysis for catechol in a closed system. The biamperometric detection system was established to record the relationship between oxidation current and time by coupling the irreversible oxidation of catechol at one pretreated platinum electrode with the irreversible reduction of platinum oxide at the other pretreated platinum electrode. Factors influencing the analytical performance were optimized, including the potential difference (ΔE), buffer solution and pH, and flow variables in the LOV. A linear calibration curve was obtained within the range of 1.0 × 10−6-5.0 × 10−4 mol L−1 of catechol with the detection limit (3σ) of 5.09 × 10−7 mol L−1. The relative standard deviation (R.S.D.) was 2.39% for 11 successive determinations of 1 × 10−5 mol L−1 catechol and the sample throughput was 35 h−1. Moreover, this proposed method was applied to the analysis of catechol in beer sample, which was testified by high-performance liquid chromatography (HPLC).  相似文献   

7.
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   

8.
A simple and highly selective electrochemical method was developed for the single or simultaneous determination of paracetamol (N-acetyl-p-aminophenol, acetaminophen) and caffeine (3,7-dihydro-1,3,7-trimethyl-1H-purine-2,6-dione) in aqueous media (acetate buffer, pH 4.5) on a boron-doped diamond (BDD) electrode using square wave voltammetry (SWV) or differential pulse voltammetry (DPV). Using DPV with the cathodically pre-treated BDD electrode, a separation of about 550 mV between the peak oxidation potentials of paracetamol and caffeine present in binary mixtures was obtained. The calibration curves for the simultaneous determination of paracetamol and caffeine showed an excellent linear response, ranging from 5.0 × 10−7 mol L−1 to 8.3 × 10−5 mol L−1 for both compounds. The detection limits for the simultaneous determination of paracetamol and caffeine were 4.9 × 10−7 mol L−1 and 3.5 × 10−8 mol L−1, respectively. The proposed method was successfully applied in the simultaneous determination of paracetamol and caffeine in several pharmaceutical formulations (tablets), with results similar to those obtained using a high-performance liquid chromatography method (at 95% confidence level).  相似文献   

9.
C. Velasco-Aguirre 《Talanta》2010,82(2):796-4507
The electrochemical behavior and the analytical application of the selective serotonin agonist naratriptan (N-methyl-3-(1-methyl-4-piperidyl)indole-5-ethanesulfonamide) are presented herein. Naratriptan exhibits an anodic response in aqueous media over a broad pH range (pH 2-12), as determined by differential pulse voltammetry and cyclic voltammetry using glassy carbon electrodes. This response is irreversible in nature, diffusion-controlled and probably caused by the oxidation of the naratriptan indole moiety. The differential pulse voltammetry technique was performed in 0.1 mol L−1 Britton-Robinson buffer (pH = 3), which elicited the most reproducible results. The percentage of naratriptan recovery was 102.1 ± 1.8%, and the limits of detection and quantitation were 9.5 × 10−6 and 2.0 × 10−5 mol L−1, respectively. Selectivity trials revealed that the oxidation signal of the drug was not disturbed by the presence of excipients or degradation products. Thus, we conclude that the method presented herein is useful for the quantification of naratriptan in pharmaceutical drugs and that this method requires no separations or extractions. Finally, this voltammetric method was successfully applied to determine the quantity and the content uniformity of naratriptan in drug tablets. A comparison of this technique to the standard high-performance liquid chromatography technique was conducted at the end of our study.  相似文献   

10.
Yang Y  Wang Z  Yang M  Li J  Zheng F  Shen G  Yu R 《Analytica chimica acta》2007,584(2):268-274
A novel and sensitive electrochemical DNA biosensor based on nanoparticles ZrO2 and multi-walled carbon nanotubes (MWNTs) for DNA immobilization and enhanced hybridization detection is described. The MWNTs/nano ZrO2/chitosan-modified glassy carbon electrode (GCE) was fabricated and oligonucleotides were immobilized to the GCE. The hybridization reaction on the electrode was monitored by differential pulse voltammetry (DPV) analysis using electroactive daunomycin as an indicator. Compared with previous DNA sensors with oligonucleotides directly incorporated on carbon electrodes, this carbon nanotube-based assay with its large surface area and good charge-transport characteristics increased DNA attachment quantity and complementary DNA detection sensitivity. The response signal increases linearly with the increase of the logarithm of the target DNA concentration in the range of 1.49 × 10−10 to 9.32 × 10−8 mol L−1 with the detection limit of 7.5 × 10−11 mol L−1 (S/N = 3). The linear regression equation is I = 32.62 + 3.037 log CDNA (mol L−1) with a correlation coefficient value of 0.9842. This is the first application of carbon nanotubes combined with nano ZrO2 to the fabrication of an electrochemical DNA biosensor with a favorable performance for the rapid detection of specific hybridization.  相似文献   

11.
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   

12.
Three Mn(III) porphyrins were used for the design of carbon paste and diamond paste based microelectrodes, which were employed for the determination of dopamine in pharmaceutical and biological samples using differential pulse voltammetry (DPV). The limits of detection lie between 1.6 × 10−13 and 2.0 × 10−6 mol L−1 while the sensitivities were between 230 pA μmol L−1 and 3.24 μA mol L−1. Dopamine was recovered reliable from pharmaceutical and biological samples in percentages higher than 91.00% and 92.00%, respectively. The surface of the microelectrodes can easily be renewed by simple polishing, obtaining a fresh surface ready for use in a new assay.  相似文献   

13.
This work reports on the performance of carbon nanotube modified screen-printed electrodes (SPE-MWCNT) for the selective determination of dopamine (DA) in the presence of ascorbic acid (AA) by adsorptive stripping voltammetry (AdSV). Several operating conditions and parameters were examined including the electrochemical pre-treatment and the previous AA interaction and DA accumulation in the presence AA at physiological conditions. Under the chosen conditions, DA peak current of differential pulse voltammograms increases linearly with DA concentration in the range of 5.0 × 10−8 to 1.0 × 10−6 mol L−1 with a limit of detection of 1.5 × 10−8 mol L−1 in connection with 600 s accumulation time. The sensitivity obtained for DA was independent from the presence or absence of AA; therefore, the proposed method can be readily applied to detect DA in real samples. The proposed methodology was successfully used for the quantification of DA in urine samples.  相似文献   

14.
The paper presents the first report on fabrication and application of a user friendly and mercury free electrochemical sensor, with the renewable bismuth bulk annular band working electrode (RBiABE), in stripping voltammetry (SV). The sensor body is partly filled with the internal electrolyte solution, in which the RBiABE is cleaned and activated before each measurement. Time of the RBiABE contact with the sample solution is precisely controlled. The usefulness of this sensor was tested by Ni(II) and Co(II) traces determination by means of differential pulse adsorptive stripping voltammetry (DP AdSV), after complexation with dimethylglyoxime (DMG) in ammonia buffer (pH 8.2). The experimental variables (composition of the supporting electrolyte, pre-concentration potential and time, potential of the RBiABE activation, and DP parameters), as well as possible interferences, were investigated. The linear calibration graphs for Ni(II) and Co(II), determined individually and together, in the range from 1 × 10−8 to 70 × 10−8 mol L−1 and from 1 × 10−9 to 70 × 10−9 mol L−1 respectively, were obtained. The calculated limit of detection (LOD), for 30 s of the accumulation time, was 3 × 10−9 mol L−1 for Ni(II) in case of a single element’s analysis, whereas the LOD was 5 × 10−9 mol L−1 for Ni(II) and 3 × 10−10 mol L−1 for Co(II), when both metal ions were measured together. The repeatability of the Ni(II) and Co(II) adsorptive stripping voltammetric signals obtained at the RBiABE were equal to 5.4% and 2.5%, respectively (n = 5). Finally, the proposed method was validated by determining Ni(II) and Co(II) in the certified reference waters (SPS-SW1 and SPS-SW2) with satisfactory results.  相似文献   

15.
A novel method to improve the sensitivity of molecularly imprinted polymer sensors was developed. Oxytetracycline (OTC), which was selected as the template molecule, was first rebound to the imprinted cavities. Gold nanoparticles were then labeled with the amino groups of OTC molecules via electrostatic adsorption and non-covalent interactions. Copper ions were catalytically reduced by the gold nanoparticles, and copper was deposited onto the electrode. The deposited copper was electrochemically dissolved, and its oxidative currents were recorded by differential pulse voltammetry (DPV). OTC could be determined indirectly within the concentration range of 3.0 × 10−10 to 1.5 × 10−7 mol L−1 with a detection limit of 6.8 × 10−11 mol L−1.  相似文献   

16.
We proposed a green and facile approach for the synthesis of β-cyclodextrin-coated poly(diallyldimethylammonium chloride)-functionalized graphene composite film (β-CD-PDDA-Gr) by using l-ascorbic acid (l-AA) as the reducing agent at room temperature. The β-CD-PDDA-Gr composite film modified glassy carbon-rotating disk electrode (GC-RDE) was then developed for the sensitive simultaneous determination of two synthetic food colorants: sunset yellow (SY) and tartrazine (TT). By cyclic voltammetry (CV), the peak currents of SY and TT increased obviously on the developed electrochemical sensor. The kinetic parameters, such as diffusion coefficient D and standard heterogeneous rate constant kb, were estimated by linear sweep voltammetry (LSV). Under the optimal conditions, the differential pulse voltammetry (DPV) signals of SY and TT on the β-CD-PDDA-Gr modified GC-RDE were significantly enhanced. The enhanced anodic peak currents represented the excellent analytical performance of simultaneous detection of SY and TT in the range of 5.0 × 10−8 to 2.0 × 10−5 mol L−1, with a low limit of detection (LOD) of 1.25 × 10−8 mol L−1 for SY and 1.43 × 10−8 mol L−1 for TT (S N−1 = 3). This proposed method displayed outstanding selectivity, good stability and acceptable repeatability and reproducibility, and also has been used to simultaneously determine SY and TT in some commercial soft drinks with satisfactory results. The obtained results were compared to HPLC of analysis for those two colorants and no significant differences were found. By the treatment of the experimental data, the electrochemical reaction mechanisms of SY and TT both involved a one-electron-one-proton-transfer process.  相似文献   

17.
A solid paraffin-based carbon paste electrode modified with 2-aminothiazole organofunctionalized silica (SiAt-SPCPE) was applied to Ni2+ determination in commercial ethanol fuel samples. The proposed method comprised four steps: (1) Ni2+ preconcentration at open circuit potential directly in the ethanol fuel sample, (2) transference of the electrode to an electrochemical cell containing DMG, (3) differential pulse voltammogram registering and (4) surface regeneration by polishing the electrode. The proposed method combines the high Ni2+ adsorption capacity presented by 2-aminothiazole organofunctionalized silica with the electrochemical properties of the Ni(DMG)2 complex, whose electrochemical reduction provides the analytical signal.All experimental parameters involved in the proposed method were optimized. Using a preconcentration time of 20 min, it was obtained a linear range from 7.5 × 10−9 to 1.0 × 10−6 mol L−1 with detection limit of 2.0 × 10−9 mol L−1. Recovery values between 96.5 and 102.4% were obtained for commercial samples spiked with 1.0 μmol L−1 Ni2+ and the developed electrode was totally stable in ethanolic solutions. The contents of Ni2+ found in the commercial samples using the proposed method were compared to those obtained by graphite furnace atomic absorption spectroscopy by using the F- and t-test. Neither the F- nor t-values exceeded the critical values at 95% confidence level, confirming that there are not statistical differences between the results obtained by both methods. These results indicate that the developed electrode can be successfully employed to reliable Ni2+ determination in commercial ethanol fuel samples without any sample pretreatment or dilution step.  相似文献   

18.
We report about the use of carbon paste electrode modified with kaolinite for analytical detection of trace lead(II) in domestic water by differential pulse voltammetry. Kaolinite clay was modified with tripolyphosphate (TPP) by impregnation method. The results show that TPP in kaolinite clay plays an important role in the accumulation process of Pb(II) on the modified electrode surface. The electroanalytical procedure for determination of Pb(II) comprised two steps: chemical accumulation of the analyte under open-circuit conditions, followed by electrochemical detection of the pre-concentrated species using differential pulse voltammetry. The analytical performance of this system has been explored by studying the effects of preconcentration time, carbon paste composition, pH, supporting electrolyte concentration, as well as interferences due to other ions. The calculated detection limit based on the variability of a blank solution (3sb criterion) for 10 measurements was 8.4 × 10−8 mol L−1, and the sensitivity determined from the slope of the calibration graph was 0.910 mol L−1. The reproducibility (RSD) for five replicate measurements at 1.0 mg L−1 lead level was 1.6%. The results indicate that this electrode is sensitive and effective for the determination of Pb2+.  相似文献   

19.
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   

20.
The influence of the boron-doping levels in boron-doped diamond film electrodes on the electrochemical response of nitrofurantoin (NFT) and the development of an electroanalytical procedure for NFT determination were investigated. The investigations were carried out using the techniques of cyclic voltammetry and square wave voltammetry on diamond film electrodes with different boron-doping levels (i.e., 5000, 10,000 and 20,000 mg L−1). The level of boron-doping in the diamond film electrodes influenced the electrochemical reduction of NFT. The appropriate cyclic voltammetric response of NFT was obtained with Britton-Robinson buffer at pH 4 and for diamond films doped with 10,000 and 20,000 mg L−1 of boron. These two films were selected for the development of the electroanalytical procedure. The use of square wave voltammetry with the optimized parameters demonstrated a good linear relationship between the peak current and the NFT concentration for a wide range of concentration. The lower limit of detection for the electrodes doped with 10,000 and 20,000 mg L−1 of boron were 2.69 × 10−8 mol L−1 (6.40 μg L−1) and 8.15 × 10−9 mol L−1 (1.94 μg L−1), respectively, while the lower limits of quantification were 8.96 × 10−8 mol L−1 (21.33 μg L−1) and 2.72 × 10−8 mol L−1 (6.47 μg L−1), respectively. The applicability of the proposed procedure was tested using a commercial pharmaceutical formulation of NFT, and the results were compared with the procedure recommended by the British Pharmacopeia. The proposed procedure was sensitive, accurate and precise for analysis of NFT and did not require complex preparations or renovations of the electrode surface. This presents the advantage of eliminating mercury waste and minimizing the adsorptive problems related to the use of other electrodic solid surfaces.  相似文献   

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