RESUMO
A beta-cyclodextrin (CD) modified copolymer membrane of sulfanilic acid (p-ASA) and N-acetylaniline (SPNAANI) on glassy carbon electrode (GCE) was prepared and used to determine uric acid (UA) in the presence of a large excess of ascorbic acid (AA) by differential pulse voltammetry (DPV). The properties of the copolymer were characterized by X-ray photoelectron spectra (XPS) and Raman spectroscopy. The oxidation peaks of AA and UA were well separated at the composite membrane modified electrode in phosphate buffer solution (PBS, pH 7.4). A linear relationship between the peak current and the concentration of UA was obtained in the range from 1.0 x 10(-5) to 3.5 x 10(-4)mol L(-1), and the detection limit was 2.7 x 10(-6)mol L(-1) at a signal-to-noise ratio of 3. Two hundred and fifty-fold excess of AA did not interfere with the determination of UA. The application of the prepared electrode was demonstrated by measuring UA in human serum samples without any pretreatment, and the results were comparatively in agreement with the spectrometric clinical assay method.
Assuntos
Alanina/análogos & derivados , Ácido Ascórbico/química , Técnicas Biossensoriais/instrumentação , Eletroquímica/instrumentação , Ácidos Sulfanílicos/química , Ácido Úrico/análise , Ácido Úrico/química , Alanina/química , Misturas Complexas/análise , Misturas Complexas/química , Desenho de Equipamento , Análise de Falha de Equipamento , Concentração de Íons de Hidrogênio , Sensibilidade e EspecificidadeRESUMO
The interactions between plant secondary metabolites (tannic acid, rutin, cinnamic acid and catechin) and glutathione transferase (GST) were investigated by fluorescence and UV-Vis absorption spectroscopy. Intrinsic fluorescence of GST was measured by selectively exciting their tryptophan (Trp) residues and quenching constants were determined using the Stern-Volmer equation. The binding affinity was found to be strongest for tannic acid and ranked in the order tannic acid>rutin>cinnamic acid>catechin. The pH values in the range of 6.7-7.9, except for tannic acid, did not affect significantly the affinity of rutin, cinnamic acid and catechin with GST. Results showed that the fluorescence quenching of GST was a static_quenching. Fluorescence quenching and UV-Vis absorption spectroscopy suggested that only the tannic acid changed the microenvironment of the Trp residues. Furthermore, the number of binding sites and binding constants at different pH values showed that tannic acid had strongest affinity towards GST and hydrogen bonding played an important role in the affinity between GST and the metabolites.
Assuntos
Catequina/química , Cinamatos/química , Glutationa Transferase/química , Plantas/metabolismo , Rutina/química , Taninos/química , Ligação de Hidrogênio , Espectrometria de Fluorescência/métodosRESUMO
For the first time, a novel, simple and reliable method for analysis of pymetrozine residues in flue-cured tobacco leaves has been developed utilizing HPLC-UV with liquid-liquid partition cleanup. Pre-treatment with ultrasonic extraction and liquid-liquid partition procedures gave preferable baseline separation and clean chromatograms by removing water-soluble and fat-soluble components which interfere with pymetrozine in the test. The performance of the method was evaluated and validated: the detection limit (LOD) was 0.005 microg x mL(-1), the relative standard deviation (RSD) was 1.2% (n = 5), and the overall recovery was above 90% at fortification levels of 0.200, 0.500, 1.000, and 5.000 mg x kg(-1). The proposed method was successfully employed for the determination of pymetrozine residues in twelve flue-cured tobacco samples collected from different regions of China.
Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Inseticidas/análise , Nicotiana/química , Triazinas/análise , China , Gorduras/química , Sensibilidade e Especificidade , Solubilidade , Água/químicaRESUMO
Loading an electrocatalyst on poorly conducting substrate can easily lead to undervaluation of its intrinsic property. In this study, the excellent activity of MoS2|NiS|MoO3 nanowires for hydrogen evolution is revealed. The precursor NiMoO4 synthesized on chemically polished Ti foil can be successfully converted to MoS2|NiS|MoO3 catalyst via gas-phase sulfurization. Without deep polish in sulfuric acid for 2 h, the as-synthesized materials do not show competitive results. After sulfurization, the surface morphology of the precursor is transformed into rough features, and the peripheries of these electrocatalysts are coated by multilayered and misaligned MoS2 with a high density of active sites and conductive component NiS. Further analysis shows that defect MoO3 is embedded inside each nanowire, which may facilitate fast electron transfer. Such nanostructured architecture shows promising results for hydrogen evolution reaction in alkaline medium with only 91 mV overpotential for the current density of 10 mA cm-2 and robust long-term stability during more than 20 h of tests.