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1.
Anal Bioanal Chem ; 410(25): 6573-6583, 2018 Oct.
Artículo en Inglés | MEDLINE | ID: mdl-30030578

RESUMEN

The toxicity of nitrofuran drugs has attracted great attention, and the reported electroanalytical methods suffered limited sensitivity. In this work, a sensitive electrochemical assay in the cathodic region is developed to determine four nitrofuran derivatives, including nitrofurantoin (NFT), nitrofurazone (NFZ), furaltadone (FTD), and furazolidone (FZD). The screen-printed carbon electrode (SPCE) was used as the electrode substrate, and the sensing surface was composed of multi-walled carbon nanotube (MWCNT) and conducting poly(melamine) (PME). The overoxidation-pretreated MWCNTs affect the surface morphology of the electrodeposited PME and, thus, the interaction with nitrofuran drugs. The characteristics of the nanocomposite-modified electrode surfaces were well characterized by field emission scanning electron microscopy (FE-SEM), X-ray photoelectron spectroscopy (XPS), and surface water contact angle experiments. The nanocomposite-modified electrodes exhibited excellent adsorption and electrochemical reduction of nitrofurans by cyclic voltammetry. The proposed assay exhibited a linear range of sub-micro to micro molar concentrations for the four drugs under the optimized differential pulse voltammetric (DPV) technique. The detection limits were found to be in the nanomolar ranges. The developed assay was applied to detect NFT in two real samples, and the results showed good recoveries that ranged from 99.0 to 104.8% and 98.0 to 103.2% for milk and lake water samples, respectively. Graphical abstract ᅟ.


Asunto(s)
Nanopartículas/química , Nanotubos de Carbono/química , Nitrofuranos/química , Polímeros/química , Triazinas/química , Animales , Técnicas Electroquímicas , Electrodos , Agua Dulce/química , Límite de Detección , Leche/química , Estructura Molecular , Factores de Tiempo
2.
Anal Chim Acta ; 1123: 44-55, 2020 Aug 01.
Artículo en Inglés | MEDLINE | ID: mdl-32507239

RESUMEN

The triclosan contamination in daily life has attracted great attention, and there is rare electroanalytical assay based on π-system dyes. In this work, a facile preparation and electroanalytical application of an organic dispersion containing bacteriochlorin dyes (LS11) and gold nanoparticles (AuNPs) was proposed. The organic-inorganic hybrid nanocomposites were characterized by transmission electron microscope (TEM) showing a core-shell structure with a uniform layer of dye molecules. The as-prepared nanocomposites were successfully coated onto glassy carbon electrodes, and the surface characteristics of the top most layer of the modified electrodes were examined by atomic force microscopy (AFM), field emission scanning electron microscopy (FE-SEM) and water contact angle experiments. The nanocomposite film-modified electrodes exhibited good electrochemical activity towards oxidation of triclosan. The oxidation of adsorbed triclosan occurred at a reduced overpotential, and the anodic current responses under a pre-concentration step prior to the potential scan were used for quantitative analysis. A good linear relationship from 0.01 µM to 0.5 µM was obtained using differential pulse voltammetry. The sensitivity and detection limit (S/N = 3) were 23.69 µA µM-1 and 0.03 µM, respectively. The proposed assay was applied to detect triclosan in two personal hygiene products using standard addition method, and the results showed good recoveries that ranged from 96.6% to 101.5% and from 99.3% to 103.8% for a toothpaste sample and a hand wash sample, respectively. A reference HPLC-UV method was used to evaluate the proposed electroanalytical method, and a good agreement was achieved.


Asunto(s)
Técnicas Biosensibles , Técnicas Electroquímicas , Oro/química , Nanopartículas del Metal/química , Porfirinas/química , Triclosán/análisis , Carbono/química , Electrodos , Desinfección de las Manos , Estructura Molecular , Pastas de Dientes/química
3.
Talanta ; 180: 81-89, 2018 Apr 01.
Artículo en Inglés | MEDLINE | ID: mdl-29332837

RESUMEN

The toxicity of sulfa drugs has attracted great attention, and the reported electrochemical methods for sulfa drugs usually employ a high oxidation potential. In this work, a one-pot synthesized conducting polymer nanocomposite containing poly(3,4-ethylenedioxythiophene) (PEDOT) and MnO2 was cast on a screen-printed carbon electrode (SPCE), and the modified electrode showed superior electrochemical activity over a bare electrode for sulfamethazine (SMZ) determination. The SMZ detection was based on the electrochemical oxidation product, which showed an adsorptive property and exhibited a redox couple at 0.39V in pH 3 phosphate buffer solutions (PBS). The electrode surfaces were well characterized by the water contact angle technique, Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM) and cyclic voltammetry. By the use of square wave voltammetry (SWV), a wide linear response to SMZ, from 1.0µM to 500µM, was obtained. The sensitivity and detection limits (S/N = 3) were 0.115µAµM-1 and 0.16µM, respectively. The proposed method and a reference high-performance liquid chromatographic method (HPLC) were applied for the determination of SMZ in two real samples using the standard addition method, and satisfactory recoveries and good agreement were obtained.


Asunto(s)
Antiinfecciosos/análisis , Compuestos Bicíclicos Heterocíclicos con Puentes/química , Análisis de los Alimentos/métodos , Miel/análisis , Leche/química , Nanocompuestos/química , Polímeros/química , Sulfametazina/análisis , Animales , Técnicas Electroquímicas/métodos , Electrodos , Límite de Detección , Compuestos de Manganeso/química , Nanocompuestos/ultraestructura , Óxidos/química
4.
Anal Chim Acta ; 901: 41-50, 2015 Dec 11.
Artículo en Inglés | MEDLINE | ID: mdl-26614056

RESUMEN

In this work, an electrochemical sensor coupled with an effective flow-injection amperometry (FIA) system is developed, targeting the determination of gallic acid (GA) in a mild neutral condition, in contrast to the existing electrochemical methods. The sensor is based on a thin electroactive poly(melamine) film immobilized on a pre-anodized screen-printed carbon electrode (SPCE*/PME). The characteristics of the sensing surface are well-characterized by field emission scanning electron microscopy (FE-SEM), X-ray photoelectron spectroscopy (XPS) and surface water contact angle experiments. The proposed assay exhibits a wide linear response to GA in both pH 3 and pH 7.0 phosphate buffer solutions (PBS) under the optimized flow-injection amperometry. The detection limit (S/N = 3) is 0.076 µM and 0.21 µM in the pH 3 and pH 7 solutions, respectively. A relative standard deviation (RSD) of 3.9% is obtained for 57 successive measurements of 50 µM GA in pH 7 solutions. Interference studies indicate that some inorganic salts, catechol, caffeine and ascorbic acid do not interfere with the GA assay. The interference effects from some orthodiphenolic compounds are also investigated. The proposed method and a conventional Folin-Ciocalteu method are applied to detect GA in green tea samples using the standard addition method, and satisfactory spiked recoveries are obtained.


Asunto(s)
Técnicas Electroquímicas/métodos , Ácido Gálico/análisis , Polímeros/química , Té/química , Triazinas/química , Límite de Detección , Oxidación-Reducción
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