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1.
《Analytical letters》2012,45(5-6):449-459
Based on the study of voltammetric behavior of carcinogenic 1-nitropyrene (1-NP), 1-aminopyrene (1-AP), and 1-hydroxypyrene (1-HP), optimum conditions have been found for the determination of these analytes by differential pulse voltammetry (DPV) at a boron-doped diamond film electrode. The optimum medium was methanol-Britton–Robinson buffer (BR buffer) pH 3.0 (70:30) for 1-NP and 1-AP, and methanol-BR buffer pH 5.0 (70:30) for 1-HP. Concentration dependences of the DPV response were measured in the range 1 · 10?6–1 · 10?4 mol dm?3 (R = ?0.9998) with the limit of detection (LOD) 3 · 10?7 mol dm?3 for 1-NP, 1 · 10?7–1 · 10?5 mol dm?3 (R = 0.9971) with LOD 6 · 10?8 mol dm?3 for 1-AP, and 1 · 10?7–1 · 10?5 mol dm?3 (R = 0.9934) with LOD 1 · 10?7 mol dm?3 for 1-HP. Simultaneous determination of 1-NP and 1-AP in a mixture was tested in the methanol-BR buffer pH 3.0 (70:30) medium as well. The content of 1-AP in the concentration range from 1 · 10?6 to 1 · 10?4 mol dm?3 had no effect on the sensitivity of the determination of 1-NP, and vice versa. Due to the close peak potentials of 1-AP and 1-HP, the direct determination of their mixture using voltammetric methods is impossible.  相似文献   

2.
《Analytical letters》2012,45(14):2309-2321
Abstract

A metalloporphyrin incorporated carbon paste sensor has been developed for the determination of metronidazole benzoate (MTZB). Zn(II) complex of 5,10,15,20-tetrakis (3-methoxy-4-hydroxy phenyl) porphyrin (TMHPP) was used as the active material. The MTZB gave a well-defined reduction peak at?0.713 V in 0.1 mol l?1 phosphate buffer solution of pH around 7. Compared with bare carbon paste electrode (CPE), the TMHPP Zn(II) modified electrode significantly enhanced the reduction peak current of MTZB as well as lowered its reduction potential. Under optimum conditions the reduction peak current was proportional to MTZB concentration over the range 1 × 10?3 mol l?1 to 1 × 10?5 mol l?1. The detection limit was found to be 4.36 × 10?6 mol l?1. This sensor has been successfully applied for the determination of MTZB in pharmaceutical formulations and urine samples.  相似文献   

3.
Modified screen printed (SPE) and carbon paste electrodes (CPE) with phenanthroline–tetraphenyl borate ionophore [Phen:TPB] were fabricated for the determination of copper(II). The modified electrodes have linear responses over a wide concentration range (1 × 10?6–1 × 10?2 mol·L?1) of copper(II) ion at 25 °C with divalent cationic slopes of 29.85 ± 0.58 and 29.45 ± 0.81 mV·decade?1 and exhibit a detection limit of 1 × 10?6 mol·L?1 for SPE and CPE. The selectivity coefficient was measured using the match potential method in acetate buffer of pH = 4.2. The modified SPE and CPE sensors show high selectivity and sensitivity for determination of copper(II) and also show stable and reproducible response over a period of five and three months for SPE and CPE sensors, respectively. This method can be used for determination of copper(II) in water, soil, plant and fish tissue samples and the results obtained agreed with those obtained with atomic absorption spectrometer (AAS).  相似文献   

4.
A novel and simple biosensor based on poly(indoleacetic acid) film-modified electrode (PIAA/CPE) was fabricated by electrochemical polymerization of indoleacetic acid on a carbon paste electrode (CPE) through cyclic voltammetry. The resulting electrode was characterized by scanning electron microscopy, and the electrochemical behaviors of dopamine (DA) and epinephrine (EP) at the electrode were studied. It was illustrated that PIAA/CPE had excellent electrochemical catalytic activities toward DA and EP. The anodic peak currents (I pa) were dramatically enhanced by about seven-fold for DA and ten times for EP at PIAA/CPE. Thus, the determinations of DA and EP were carried out using PIAA/CPE successfully. The linear responses were obtained in the range of 3.0?×?10?7~7.0?×?10?4 and 1.0?×?10?6 ~8.0?×?10?4 mol L?1 with the detection limits (3σ) of 1?×?10?7 and 4?×?10?7 mol L?1 corresponding with DA and EP, respectively. Moreover, the cathodic peaks of DA and EP were well-separated with a potential difference about 325 mV in pH 5.3 phosphate-buffered saline, so simultaneous determination of DA and EP was carried out in this paper. Additionally, the interference studies showed that the PIAA/CPE exhibited excellent selectivity in the presence of ascorbic acid (AA). With good selectivity and sensitivity, the present method has been successfully applied to the determination of DA and EP in pharmaceutical samples.  相似文献   

5.
《Analytical letters》2012,45(8):1203-1218
Abstract

Ultraviolet (UV)–derivative spectrophotometry, bivariate calibration algorithm, and Vierodt methods were applied to simultaneous determination of ranitidine (R) and amoxicillin (AMX) in binary mixtures. The first-order derivative allows determination of R in the concentration range 4.0 · 10?6 mol · dm?3 to 6.0 · 10?5 mol · dm?3. Vierordt method enables Ranitidine assaying in the presence of 2.5-fold excess of AMX and 3-fold excess of R. The bivariate calibration method obeys Beer's law in the concentration ranges 4.0 · 10?6 mol · dm?3 to 6.0 · 10?5 mol · dm?3 for R and 2.0 · 10?6 to 2.0 · 10?5 mol · dm?3 for AMX.  相似文献   

6.
《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   

7.
《Electroanalysis》2002,14(23):1668-1673
Voltammetric properties and possibility of the determination of carcinogenic aminoderivatives of polycyclic aromatic hydrocarbons, namely 1‐ and 2‐aminonaphthalene and 2‐aminobiphenyl, have been investigated. Carbon paste electrodes (CPE) modified with monomeric α‐, β‐ or γ‐cyclodextrin and carbon‐based screen‐printed electrodes (SPE) surface‐modified with a thin film of β‐cyclodextrin (β‐CDP) or carboxymethylated β‐cyclodextrin (β‐CDPA) condensation polymer were used for that purpose as simple electrochemical biosensors. Analytical procedure for the DPV determination of tested amines using these biosensors was proposed. Linear calibration plots within the concentration range of 2×10?8 – 2×10?7 mol dm?3 and 2×10?7–1×10?6 mol dm?3 with limits of quantification of the order of 10?9 mol dm?3 were obtained for the modified CPE and modified SPE.  相似文献   

8.
The direct electrochemistry of epinephrine (EP) on a modified carbon paste electrode (CPE) was described. The electrode was modified with Zinc oxide (ZnO) nanoparticles and 1,3-dipropylimidazolium bromide as a binder. The oxidation peak potential of EP at the surface of the ionic liquid ZnO nanoparticle CPE (IL/ZnO/NP/CPE) appeared at 350 mV, which was about 80 mV lower than the oxidation peak potential at the surface of the traditional carbon CPE under a similar condition. On other hand, the oxidation peak current was increased for about three times at the surface of IL/ZnO/NP/CPE compared to CPE. The linear response range and detection limit were found to be 0.09–800 μmol L?1 and 0.06 μmol L?1, respectively. Other physiological species did not interfere in the determination of EP at the surface of the proposed sensor in the optimum condition. The proposed sensor was successfully applied for the determination of EP in real samples.  相似文献   

9.
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   

10.
A mesoporous silica-based hybrid material composed of silica xerogel modified with an ionic silsesquioxane, which contains the 1,4-diazoniabicyclo[2.2.2]octane chloride group, was obtained. The silsesquioxane film is highly dispersed on the surface. This hybrid material was utilized to develop a carbon paste electrode (CPE) for determination of methyl parathion. Transmission FTIR, elemental analysis and N2 adsorption–desorption isotherms were used for characterization of the material. The electrochemical behavior of methyl parathion was evaluated by cyclic voltammetry and differential pulse voltammetry. It was observed a linear response to methyl parathion in the concentration range from 1.25 × 10?7 to 2.56 × 10?6 mol L?1 by employing the carbon paste electrode, in Britton–Robinson buffer solution (pH 6). The achieved detection limit (3 SD of the blank divided by the slope of calibration curve) was 0.013 µmol L?1 and sensitivity was 6.3 µA µmol L?1. This result shows the potentiality of this electrode for application as electrochemical sensor for methyl parathion.  相似文献   

11.
《Analytical letters》2012,45(7):1225-1235
Abstract

A single-sweep voltammetric method was proposed for the determination of tamoxifen. The proposed method took advantage of both the accumulation of carbon paste electrode toward tamoxifen and the rapidity of single-sweep voltammetry. In HAc-NaAc (pH 4.1) buffer/methanol (85:15 v/v) mixed solution, an irreversible oxidation peak of tamoxifen was observed at 1.1 V (versus SCE). The second-order derivative peak current of tamoxifen and its concentration plots were rectilinear over the range of 7.0 × 10?10 ~ 3.0 × 10?8 mol · l?1 with a detection limit of 1.0 × 10?10 mol · l?1 without any preconcentration. The proposed method was evaluated by analyzing tamoxifen citrate tablets, which was characterized by rapidity and higher sensitivity.  相似文献   

12.
《Analytical letters》2012,45(1):141-153
Abstract

In this research, the construction and general performance characteristics of a sunset yellow sensor based on sunset yellow–cetyl pyridinum (SY-CPY) ion pair as an ion exchanger were described. A coated platinum wire electrode (CPE) was prepared and compared with coated graphite (CGE) and membrane electrode (PME). The CPE exhibited a rapid and Nernstian response (?29.77 ± 0.2 mV decade?1) to SY concentration range from 3.16 × 10?7 to 3.16 × 10?3 mol dm?3 within pH 4.5–9.5. Interfering effects of some foreign substances were reported. The optimized matrix was successfully applied to the determination of SY in artificial mixtures and commercial soft drinks. The results showed good agreements with the determination made by use of high-performance liquid chromatography.  相似文献   

13.
《Analytical letters》2012,45(10):1783-1795
The behavior of seven hydroxy anthraquinone derivatives was studied by capillary zone electrophoresis and micellar electrokinetic chromatography. The effects of buffer pH (6.5–10.8) and sodium dodecyl sulfate concentration (10–20 mmol L?1) on the effective mobilities of the analytes and their separation were tested. A comparison of the two optimized separation systems showed that micellar electrokinetic chromatography was superior as it permits separation of all the seven analytes within 15 min, using 15 mmol L?1 sodium dodecyl sulfate in 10 mmol L?1 tetraborate buffer, pH 8.5, at a voltage of 20 kV. The calibration curves were linear in the concentration range from 5.0 · 10?7 to 5.0 · 10?4 mol L?1 for most of the analytes, at a detection wavelength of 254 nm. LOD and LOQ values of the analytes were in the ranges of 2.10 · 10?7–1.28 · 10?6 mol L?1and 6.99 · 10?7–4.25 · 10?6 mol L?1, respectively. The proposed separation conditions were applied to determination of 1,2-dihydroxy anthraquinone (alizarin) and 1,2,4-trihydroxy anthraquinone (purpurin) in Rubia tinctorum aglycone and of the recently described 1-acetyl-2,4,5,7-tetrahydroxy-9,10-anthraquinone and 1-acetyl-2,4,5,7,8-pentahydroxy-9,10-anthraquinone in the mycelium of fungi Geosmithia lavendula.  相似文献   

14.
于浩  郑建斌 《中国化学》2007,25(4):503-509
A copper hexacyanoferrate modified ceramic carbon electrode (CuHCF/CCE) had been prepared by two-step sol-gel technique and characterized using electrochemical methods. The resulting modified electrode showed a pair of well-defined surface waves in the potential range of 0.40 to 1.0 V with the formal potential of 0.682 V (vs. SCE) in 0.050 mol·dm^-3 HOAc-NaOAc buffer containing 0.30 mol·dm^-3 KCl. The charge transfer coefficient (a) and charge transfer rate constant (ks) for the modified electrode were calculated. The electrocatalytic activity of this modified electrode to hydrazine was also investigated, and chronoamperometry was exploited to conveniently determine the diffusion coefficient (D) of hydrazine in solution and the catalytic rate constant (kcat). Finally, hydrazine was determined with amperometry using the resulting modified electrode. The calibration plot for hydrazine determination was linear in 3.0 × 10^-6--7.5 × 10^-4 mol·dm^-3 with the detection limit of 8.0 × 10^-7 molodm^-3. This modified electrode had some advantages over the modified film electrodes constructed by the conventional methods, such as renewable surface, good long-term stability, excellent catalytic activity and short response time to hydrazine.  相似文献   

15.
《Analytical letters》2012,45(12):1976-1988
A sensitive and selective electrochemical method for the simultaneous determination of dopamine (DA) and uric acid (UA) was developed using a pyrogallol red modified carbon paste electrode. Under the optimized conditions, the peak current was linearly dependent on 1.0–700.0 μmol L?1 DA and 50.0–1000.0 μmol L?1 UA. The detection limits for DA and UA were 0.78 μmol L?1 and 35 μmol L?1, respectively. Finally, this method was also examined for the determination of DA and uric acid in real samples such as drugs and urine.  相似文献   

16.
A carbon paste electrode (CPE) modified with Fe3O4 nanoparticles (Fe3O4 NP) and the ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate (IL BMI.PF6) was employed for the electroanalytical determination of estrone (E1) by square-wave voltammetry (SWV). At the modified electrode, cyclic voltammograms of E1 in B–R buffer (pH 12.0) showed an adsorption-controlled irreversible oxidation peak at around +0.365 V. The anodic current increased by a factor of five times and the peak potential shifted 65 mV to less positive values compared with the unmodified CPE. Under optimized conditions, the calibration curve obtained showed two linear ranges: from 4.0 to 9.0 μmol L?1 and from 9.0 to 100.0 μmol L?1. The limits of detection (LOD) and quantification (LOQ) attained were 0.47 and 4.0 μmol L?1, respectively. The proposed modified electrode was applied to the determination of E1 in pork meat samples. Data provided by the proposed modified electrode were compared with data obtained by UV–vis spectroscopy. The outstanding performance of the electrochemical device indicates that Fe3O4 NP and the IL BMI.PF6 are promising materials for the preparation of chemically modified electrodes for the determination of E1.  相似文献   

17.

Electrochemical polymerization of azure B from sulfuric acid solution was carried out by using cyclic voltammetry. The electrolytic solution consisted of 5.0 mmol · dm?3 azure B and 0.3 mol · dm?3 H2SO4. The temperature for polymerization was controlled at 20°C. A blue film, i.e., poly(azure B) was formed on a platinum foil and had a electrochemical reversibility, stability and a fast charge transfer ability in the 0.5 mol · dm?3 Na2SO4 with pH ≤4.0 solution. The currents of both anodic and cathodic peaks are proportional to υ1/2 at the scan rate (υ) region of 25 and 600 mV · s?1 on the cyclic voltammograms. The conductivity of poly(azure B) is 2.8×10?6 S · cm?1 at 20°C. The UV‐visible spectrum and Raman spectrum of the polymer are different from those of the monomer. A possible polymerization mechanism of azure B was also proposed.  相似文献   

18.
儿茶酚胺是一类非常重要的神经递质,在人体的心血管系统、神经系统、内分泌腺、肾脏、平滑肌等组织系统的生理活动中起着广泛的调节作用。肾上腺素为儿茶酚胺的一种,建立灵敏、高效的肾上腺素检测技术具有重要的临床意义。本文将银(Ⅲ)配合物与鲁米诺组成新的流动注射化学发光体系,利用碱性介质中肾上腺素对三价银配合物-鲁米诺化学发光体系有明显的增强效应来测定肾上腺素的含量,并据此建立了高效测定肾上腺素的流动注射化学发光新方法。在优化的条件下,该方法测定肾上腺素的线型范围为1.0×10-9~1.0×10-7 mol L-1,检出限为8.0×10-10 mol L-1,对1.5×10-8 mol L-1肾上腺素11次平行测定,其相对标偏差为2.9%。利用建立的分析方法测定了药物肾上腺素,并对三价银-鲁米诺化学发光新体系测定肾上腺素的反应机理进行了讨论。  相似文献   

19.
《Analytical letters》2012,45(16):2445-2454
A novel voltammetric sensor using multi-wall carbon nanotubes (MWNTs) coupled with Nafion modified glassy carbon electrode (GCE) was developed for the detection of methylparaben (MP). The sensor exhibited good electrocatalytic activity toward the oxidation of MP in the phosphate buffer solution (PBS, pH 6.5). It displayed good sensitivity, repeatability, reproducibility, and long-term stability. Under the optimized conditions, the anodic peak current was linear with the concentration of MP in the range of 3 × 10?6 mol L?1 to 1 × 10?4 mol L?1. The detection limit was 1 × 10?6 mol L?1. The proposed method was successfully applied to determine MP in cosmetics with satisfactory results.  相似文献   

20.
《Analytical letters》2012,45(18):2697-2706
This paper reports a core-shell nanoparticle system coated on the carbon paste electrode (CPE) for determination of hydrogen peroxide. The amino-functionalized shell-magnetic core nanoparticles have been proven to be an effective material for Hb immobilization. The core-shell nanoparticle system was constructed by immobilizing hemoglobin (Hb) on amino-functionalized shell@magnetic core composite nanoparticles (NH2-SiO2-CoFe2O4) with the bridge of gold nanoparticles (AuNPs). Electrochemical impedance spectroscopy, cyclic voltammetry, and chronoamperometry were used to characterize the obtained biosensor. The Hb/AuNPs/NH2-SiO2-CoFe2O4/CPE showed a linear range from 1.9 × 10?6 to 4.6 × 10?3 M, with a detection limit of 6.3 × 10?7 M (S/N = 3) under the optimized experimental conditions. A good affinity was shown due to the small apparent Michaelis–Menten constant of 2.68 mM.  相似文献   

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