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1.
A novel poly(p-xylenolsulfonephthalein) modified glassy carbon electrode was prepared for the simultaneous determination of ascorbic acid (AA), epinephrine (EP) and uric acid (UA). Cyclic voltammetric, chronoamperometric, and differential pulse voltammetric methods were used to investigate the modified electrode for the electrocatalytic oxidation of EP, AA, and UA in aqueous solutions. The separation of the oxidation peak potentials for AA–EP and EP–UA was about 200 and 130 mV, respectively. The calibration curves obtained for AA, EP, and UA were in the ranges of 10–1343, 2–390, and 0.1–560 μmol L−1, respectively. The detection limits (S/N = 3) were 4, 0.1, and 0.08 μmol L−1 for AA, EP and UA, respectively. The diffusion coefficient and the catalytic rate constant for the oxidation of EP at the modified electrode were calculated as 1.40(±0.10) × 10−4 cm2 s−1 and 1.06 × 103 mol−1 L s−1, respectively. The present method was applied to the determination of EP in pharmaceutical and urine samples, AA in commercially available vitamin C tablet, and EP plus UA in urine samples.  相似文献   

2.
A simple, rapid and low-cost electroanalytical method is proposed for the determination of acetaminophen (ACP) and codeine (COD) at nanomolar levels in pharmaceutical and biological samples. The analytical procedure is based on a flow injection analysis system coupled to electrochemical detection, which was multiple pulse amperometry (FIA-MPA). Boron-doped diamond was used as the working electrode for electrochemical detection. The electrode was subjected to a cathodic pretreatment and was selected in this work due its good electrochemical performance. By applying the FIA-MPA method, after a number of optimization assays, the analgesics were simultaneously determined at excellent linear concentration ranges. The analytical curves ranged from 80 nmol L−1 to 100 µmol L−1 for ACP and from 50 nmol L−1 to 10 µmol L−1 for COD, and the obtained limits of detection were 30 nmol L−1 and 35 nmol L−1 for ACP and COD, respectively. The practical applicability of the electroanalytical method was evaluated from the ACP and COD determination in two sample matrices: commercial pharmaceutical samples and biological fluids. In the case of pharmaceutical formulation samples, the obtained results were statistically similar to those obtained using a reference chromatographic method. In addition, these drugs were simultaneously quantified in biological fluid samples of urine and human serum with excellent recovery percentages.  相似文献   

3.
A nafion covered carbon nanotubes-paste electrode modified with poly(m-ferrocenylaniline), (Nf/p(FcAni)-CNTsPE), provides a novel voltammetric sensor for the selective determination of dopamine (DA) and uric acid (UA) in the presence of ascorbic acid (AA). We studied the electrochemical activity of Nf/p(FcAni)-CNTsPE toward DA, UA, and AA by differential pulse voltammetry (DPV). DA and UA anodic peaks appear at 0.30 and 0.45 V, respectively while an anodic peak for AA was not observed. DPV oxidation peak values are linearly dependent on DA concentration over the range 1–150 μM (r2 = 0.992), and on UA concentration over the range 5–250 μM (r2 = 0.997). DA and UA detection limits are estimated to be 0.21 and 0.58 μM, respectively. The modified electrode shows both good selectivity and reproducibility for the selective determination of DA and UA in real samples. Finally, the modified electrode was successfully applied for the determination of DA and UA in pharmaceutical or biological sample fluids.  相似文献   

4.
The behavior of a modified carbon platinum electrode (Pt) for lead(II) determination by square wave voltammetry (SWV) was studied. The modified electrode is obtained by electrodeposition of hydroxyapatite (HAP) on the surface of a bare platinum electrode. The new electrode (HAP/Pt) revealed interesting electroanalytical detection of lead(II) based on the adsorption of this metal onto hydroxyapatite under open circuit conditions. After optimization of the experimental and voltammetric conditions, the best voltammetric responses-current intensity and voltammetric profile were obtained in 0.2 mol L?1 KNO3 with: 30 min accumulation time, 5 mV pulse amplitude and 1 mV s?1 scan rate. The observed detection (DL, 3σ) and quantification (DL, 10σ) limits in pure water were 2.01 × 10?8 and 6.7 × 10?7 mol L?1, respectively. The reproducibility of the proposed method was determined from five different measurements in a solution containing 2.2 × 10?6 mol L?1 lead(II) with a coefficients of variation of 2.08%.The electrochemical of hydroxyapatite at platinum surfaces was characterized, after calcinations 900 °C, by X-ray diffraction, infrared spectroscopy, chemical and electrochemical analysis.  相似文献   

5.
A novel carbon-nanofiber-modified carbon-paste electrode (CNF-CPE) was employed for the simultaneous determination of dopamine (DA), ascorbic acid (AA) and uric acid (UA) with good selectivity and high sensitivity. The CNFs were prepared by combination of electrospinning technique with thermal treatment method and were used without any pretreatment. In application to determination of DA, AA and UA in the ternary mixture, the pristine CNF-CPE exhibited well-separated differential pulse voltammetric peaks with high catalytic current. Low detection limits of 0.04 μM, 2 μM and 0.2 μM for DA, AA and UA were obtained, with the linear calibration curves over the concentration range 0.04–5.6 μM, 2–64 μM and 0.8–16.8 μM, respectively.  相似文献   

6.
A new sorbent based on cysteine modified silica gel (SiG-cys) was prepared and studied for preconcentration and separation of noble metals Au(III), Pd(II), Pt(II), Pt(IV). Its extraction efficiency was examined by batch and column solid phase extraction procedures. Laboratory experiments performed showed that sorbent is characterized with high selectivity, permiting quantitative sorption (93–97%) of noble metals Au, Pd and Pt from acidic media 0.1–2 mol L? 1 HCl and unsignificant sorption (less than 2%) for common base metals like Cu, Fe, Mn and Zn. The analytes retained on the sorbent are effectively eluted with 0.1 mol L? 1 thiourea in 0.1 mol L? 1 HCl and measured by ETAAS or ICP OES under optimal instrumental parameters. The sorbent showed high mechanical and chemical stability and extraction efficiency was not changed after 500 cycles of sorption/desorption. The sorbent was successfully applied in analyticals procedures for preconcentration and determination of Au, Pd and Pt in geological and soil samples. Detection limits (3σ criteria) achieved, depending on the instrumental methods used are: ETAAS (0.005 μg L? 1 for Au in river and sea water, 0.002 μg g? 1 for Au in copper ore and copper concentrate); ICP OES (0.03 μg L? 1 for Pd and 0.06 μg L? 1 for Pt in river and sea water, 0.006 μg g? 1 for Pd in copper ore and copper concentrate and 0.002 μg g? 1 for soluble Pt in soil). The accuracy of the procedures developed was confirmed by added/found method for sea and river water; by the analysis of national certified materials (copper ore and copper concentrate for Au and Pd) and by determination of the sum of soluble Pt(II) + Pt(IV) in spiked soil samples.  相似文献   

7.
《Comptes Rendus Chimie》2014,17(5):465-476
A novel modified multiwall carbon nanotubes paste electrode with sodium dodecyl sulfate as a surfactant (SDS) has been fabricated through an electrochemical oxidation procedure and was used to electrochemically detect dopamine (DA), ascorbic acid (AA), uric acid (UA), and their mixture by cyclic voltammetry (CV) and differential voltammetry (DPV) methods. Several factors affecting the electrocatalytic activity of the hybrid material, such as the effect of pH, of the scan rate and of the concentration were studied. The bare carbon nanotubes paste electrode (BCNTPE) and SDS-modified carbon nanotubes paste electrode (SDSMCNTPE) were characterized using Field Emission Scanning Electron Microscopy (FESEM) and Energy-Dispersive X-ray spectroscopy (EDX). Using the CV procedure, a linear analytical curve was observed in the 1 × 10−6–2.8 × 10−5 M range with a detection limit at 3.3 × 10−7 M in pH 6.5, 0.2 M phosphate buffer solutions (PBS).  相似文献   

8.
This paper presents the optimization of instrumental and solution parameters for determination of tamoxifen in urine and plasma and formulation by fast Fourier transform square wave voltammetry (SWV) using a gold microelectrode in flow-injection system. The samples are subjected by the same buffer solution and are injected in the flow-injection apparatus. By applying a novel square wave voltammetry method to perform as a sensitive method the voltamograms are recorded. The method used for determination of tamoxifen by measuring the changes in admittance voltammogram of a gold ultramicroelectrode (in 0.05 mol L?1 H3PO4 solution) caused by adsorption of the tamoxifen on the electrode surface. The best sensitivity was achieved using a frequency of 600 Hz and a medium composed of 0.05 mol L?1 phosphate buffers at pH 2.0. The best performance was obtained with the pH value of 2, pulse amplitude 25 mV, frequency 600 Hz, accumulation potential of ?100 mV and accumulation time of 0.5 s. Furthermore, signal-to-noise ratio has significantly increased by application of discrete fast Fourier transform (FFT) method, background subtraction and two-dimensional integration of the electrode response over a selected potential range and time window. Calibration plots are given for solutions containing 1.0 × 10?11 to 3.0 × 10?6 mol L?1 of tamoxifen. The detection limit is calculated to be 3.0 × 10?12 mol L?1 (~2 pg mL?1). The relative standard deviation at concentration 2.0 × 10?8 M is 6.1% for five reported measurements.  相似文献   

9.
The potentiometric response characteristics of zinc ion selective PVC-based membrane electrode employing 1,12,14-triaza-5,8-dioxo-3(4),9(10)-dibenzoyl-1,12,14-triene as an inophore was investigated. The proposed electrode exhibits a Nernstian behavior with a slope of 29.2 ± 0.4 mV per decade with a working concentration range of 1.3 × 10?7–1.0 × 10?1 mol L?1 and a detection limit of 1.0 × 10?8 mol L?1. The membrane having the composition as TDODBCPT:O-NPOE:PVC:OA; 7:57:30:6 wt.% exhibits the best results. It has a fast response time of 7 s and can be used for at least 100 days without any considerable divergence in potential. The proposed electrode show good discrimination of Zn2+ ion from diverse ions. The potential response remains constant over a pH range of 3.5–9.2. The electrode found well work under laboratory conditions. The proposed sensor directly used for determination of zinc ions in human hair sample, wastewater and an indicator electrode with EDTA titration.  相似文献   

10.
《Comptes Rendus Chimie》2015,18(4):438-448
A highly sensitive method was investigated for the simultaneous determination of acetaminophen (AC), dopamine (DA), and ascorbic acid (AA) using a PbS nanoparticles Schiff base-modified carbon paste electrode (PSNSB/CPE). Differential pulse voltammetry peak currents of AC, DA and AA increased linearly with their concentrations within the ranges of 3.30 × 10−8–1.58 × 10−4 M, 5.0 × 10−8–1.2 × 10−4 M and 2.50 × 10−6–1.05 × 10−3 M, respectively, and the detection limits for AC, DA and AA were 5.36 × 10−9, 2.45 × 10−9 and 1.86 × 10−8 M, respectively. The peak potentials recorded in a phosphate buffer solution (PBS) of pH 4.6 were 0.672, 0.390, and 0.168 V (vs Ag/AgCl) for AC, DA and AA, respectively. The modified electrode was used for the determination of AC, DA, and AA simultaneously in real and synthetic samples.  相似文献   

11.
A novel electrochemical platform was designed and prepared for simultaneous determination of p-acetaminophen (AMP) and p-aminophenol (AP) by combining the excellent conductivity and electrocatalytic activities of tetraaminophenyl porphyrin functionalized multi-walled carbon nanotubes (CNTs-CONH-TAPP) and gold nanoparticles (AuNPs). The as-synthesized CNTs-CONH-TAPP composites were characterized by Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy and scanning electron microscope. The incisive oxidation current responses of AMP and AP at the modified electrode promised a sensitive and selective simultaneous determination of AMP and AP. Under optimized conditions, the peak currents were directly proportional to the concentrations of AMP and AP over the ranges of 4.5–500 μmol L−1 and 0.08–60 μmol L−1, respectively, and the limits of detection were 0.44 μmol L−1 for AMP and 0.025 μmol L−1 for AP(S/N = 3) respectively. The proposed modified electrode showed excellent selectivity, reproducibility and long-term stability and could be applied in simultaneous determination of p-acetaminophen and p-aminophenol in real samples.  相似文献   

12.
A novel method for the determination of berberine has been developed based on quenching of the fluorescence of thioglycolic acid-capped CdTe quantum dots (TGA-CdTe QDs) by berberine in aqueous solutions. Under optimum conditions, the relative fluorescence intensity was linearly proportional to the concentration of berberine between 2.5 × 10?8 and 8.0 × 10?6 mol L?1 with a detection limit of 6.0 × 10?9 mol L?1. The method has been applied to the determination of berberine in real samples, and satisfactory results were obtained. The mechanism of the proposed reaction was also discussed.  相似文献   

13.
A simple and rapid method for morphine detection is described based on PEDOT electrode in the presence of SDS. The electrochemistry of morphine is investigated by CV, LSV and SWV. The effect of common interferences on the current response of morphine namely AA and UA is studied. The electrode is applied to the selective determination of morphine in urine samples in the linear ranges 0.3–8 µmol L?1 and 10–60 µmol L?1, with low detection limits of 50 and 68 nmol L?1, respectively and recovery of 96.4 %. The application of PEDOT is realized in determination of morphine in tablets successfully.  相似文献   

14.
A novel sensor based on a screen-printed electrode (SPE) modified with a stable dispersion of commercially available carbon black (CB) N220 was developed. This probe showed significantly enhanced electrochemical activity relative to a bare SPE when tested with ferricyanide, epinephrine, norepinephrine, benzoquinone and NADH. When challenged in amperometric batch mode with NADH, the response was stable and revealed a linear dependence up to 2·10?4 mol L?1 with a detection limit of 3·10?7 mol L?1. The analytical performance, coupled with the low cost of the CB nanomaterial, suggests that this sensor holds promise for electrochemical applications.  相似文献   

15.
Human serum albumin (HSA) was the most abundant protein in human plasma and has significant physiological function. In Tris–HCl buffer solution (pH 7.4), water-soluble semiconductor CdSe quantum dots (QDs) reacted with HSA and the products resulted in a great enhancement of the intensity of resonance Rayleigh scattering (RRS) and second-order scattering (SOS). Based on this, a new method was developed to investigate the interactions between QDs and HSA. The parameters with regard to determination were optimized, and the reaction mechanism was discussed. Under optimal conditions, the increments of scattering intensity (ΔI) were directly proportional to the concentrations of HSA in the range of 0.4–48.0 μmol L?1. The detection limits were 0.10 μmol L?1 for RRS method and 0.25 μmol L?1 for SOS method. The proposed method was sensitive, simple and rapid. It has been successfully applied to the determination of HSA in human urine samples. Analytical results obtained with this novel assay were satisfactory.  相似文献   

16.
朱小红  林祥钦 《中国化学》2009,27(6):1103-1109
用循环伏安法(CV)选择不同电位区间来电聚合烟酰胺(NA)得到了两种聚合物膜修饰电极:poly-niacinamide/GCE (poly-NA/GCE)和poly- nicotinic acid /GCE (poly-NC/GCE)。这两电极都具有显著电化学催化作用,能明显地降低多巴胺(DA)、尿酸(UA)和抗坏血酸(AA)的氧化过电位,并在混合溶液中使这些物质的氧化峰电位距离足够大,可进行三物质的同时测定。poly-NC/GCE的电催化性能更好一些,用差分脉冲伏安法(DPV)测定抗坏血酸,线性范围为75–3000 µmol L-1,电流灵敏度为5.6 mA•L•mol-1;测定多巴胺,线性范围为0.37 – 16 µmol L-1,电流灵敏度为1140 mA•L•mol-1; 测定尿酸,线性范围为0.74 – 230 µmol L-1,电流灵敏度为102 mA•L•mol-1。该电极具有很高的灵敏度、选择性和抗污染能力。  相似文献   

17.
A novel biosensor by electrochemically codeposited Pt nanoclusters and DNA film was constructed and applied to detection of dopamine (DA) and uric acid (UA) in the presence of high concentration ascorbic acid (AA). Scanning electron microscopy and X‐ray photoelectron spectroscopy were used for characterization. This electrode was successfully used to resolve the overlapping voltammetric response of DA, UA and AA into three well‐defined peaks with a large anodic peak difference (ΔEpa) of about 184 mV for DA and 324 mV for UA. The catalytic peak current obtained from differential pulse voltammetry was linearly dependent on the DA concentration from 1.1× 10?7 to 3.8×10?5 mol·L?1 with a detection limit of 3.6×10?8 mol·L?1 (S/N=3) and on the UA concentration from 3.0×10?7 to 5.7×10?5 mol·L?1 with a detection limit of 1.0×10?7 mol·L?1 with coexistence of 1.0×10?3 mol·L?1 AA. The modified electrode shows good sensitivity and selectivity.  相似文献   

18.
The electrochemical reduction of secnidazole was carried out in BR buffer solutions in the pH range 2.0–11.8 by dc polarography. The polarograms exhibited two irreversible reduction waves in acidic media and one wave in alkaline media, corresponding to the reduction of nitro group in the drug. The cathodic adsorptive voltammetric behavior was studied on glassy carbon electrode to optimize an analytical method for determination of secnidazole. The drug was determined in the range between 4.0 × 10?6 and 1.2 × 10?4 mol L?1. The proposed method was successfully applied to the determination of the drug content in tablets with mean recovery and relative standard deviation of 100.91% and 1.82%, respectively. It was also applied to human serum with a good precision and accuracy.  相似文献   

19.
New biocomposite materials, based on the incorporation of DNA doped p-aminobenzensulfonic acid, was fabricated by electrochemical method. A carbon fiber microelectrode modified by this thin film was fabricated for selective determination of uric acid (UA) in the presence of a larger amount of ascorbic acid (AA). It was found that the voltammetric oxidation peak separation between UA and AA is about 260 mV at the modified electrode. A linear response of the peak current versus the concentration was found in the range of 8 × 10−7–6 × 10−4 M with correlation coefficient of 0.9991 and the detection limit was 5 × 10−7 M (s/n = 3) at the 5 × 10−4 M AA. The presence of high concentration AA did not interference the determination. The electropolymerized film was characterized by SEM techniques. The modified electrode shows good sensitivity, selectivity and stability.  相似文献   

20.
A simple and sensitive method for simultaneously measuring dopamine (DA), ascorbic acid (AA), and uric acid (UA) using a poly(1‐aminoanthracene) and carbon nanotubes nanocomposite electrode is presented. The experimental parameters for composite film synthesis as well as the variables related to simultaneous determination of DA, AA, and UA were optimized at the same time using fractional factorial and Doehlert designs. The use of carbon nanotubes and poly(1‐aminoanthracene) in association with a cathodic pretreatment led to three well‐defined oxidation peaks at potentials around ?0.039, 0.180 and 0.351 V (vs. Ag/AgCl) for AA, DA, and UA, respectively. Using differential pulse voltammetry, calibration curves for AA, DA, and UA were obtained over the range of 0.16–3.12×10?3 mol L?1, 3.54–136×10?6 mol L?1, and 0.76–2.92×10?3 mol L?1, with detection limits of 3.95×10?5 mol L?1, 2.90×10?7 mol L?1, and 4.22×10?5 mol L?1, respectively. The proposed method was successfully applied to determine DA, AA, and UA in biological samples with good results.  相似文献   

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