Voltammetric Studies of Cobalt Hexacyanoferrate Formed on the Titanium (IV) Phosphate Surface and its Application to the Determination of Sulfite

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Preparation and Voltammetric Studies of Titanium (IV) Phosphate Modified with Silver Hexacyanoferrate to a Voltammetric Determination of L-Cysteine

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Aplicabilidade da voltametria de pulso diferencial na quantificação de ácido fólico e ácido oxálico: um método comparativo

The development of more selective and sensitive analytical methods is of great importance in different areas of knowledge, covering, for example, food, biotechnological, environmental and pharmaceutical sectors. The study aimed to employ the technique electroanalytical differential pulse voltammetry (DPV) as an innovative and promising alternative for identification and quantification of organic compounds. The organic compounds were investigated in this study oxalic acid (OA) and folic acid (FA). The electrochemical oxidation of oxalic acid has been extensively studied as a model reaction in the boundary between the organic and inorganic electrochemistry. Since the AF, an essential vitamin for cell multiplication in all tissues, which is essential for DNA synthesis. The AF has been investigated using analytical techniques, liquid chromatography and molecular absorption spectrophotometry. The results obtained during the experimental procedure indicated that the process of electrochemical oxidation of oxalic acid is strongly dependent on the nature of the anode material and the oxidation mechanism, which affects their detection. Efficient removal was observed in Ti/PbO2 anodes, graphite, BDD and Pt 90, 85, 80 and 78% respectively. It was also shown that the DPV employing glassy carbon electrode offers a fast, simple, reliable and economical way to determine the AO during the process of electrochemical oxidation. Furthermore, electroanalytical methods are more expensive than commonly used chromatographic analysis and other instrumental methods involving toxic reagents and higher cost. Compared with the classical method of titration and DPV could be a good fit, confidence intervals and detection limits confirming the applicability of electroanalytical technique for monitoring the degradation of oxalic acid. For the study of AF was investigated the electrocatalytic activity of the carbon paste electrode for identification and quantification in pharmaceutical formulations by applying the DPV. The results obtained during the experimental procedure showed an irreversible oxidation peak at 9.1 V characteristic of FA. The carbon paste sensor showed low detection limit of 5.683×10−8 mol L-1 reducing matrix effects. The spectrophotometric analysis showed lower concentrations of HF compared with those obtained by HPLC and DPV. The levels of AF were obtained according to the methodology proposed by the Brazilian Pharmacopoeia. The electroanalytical method (DPV) proposed is cheaper than GC analysis commonly used by the pharmaceutical industry. The results demonstrated the potential of these electroanalytical techniques for future applications in environmental, chemical and biological sensors

Determination of selenium by GFAAS in slurries of fish feces to estimate the bioavailability of this micronutrient in feed used in pisciculture

This paper presents a simple, fast and sensitive method to determine selenium in samples of feces and of fish feed by graphite furnace atomic absorption spectrometry (GFAAS) through the direct introduction of slurries of the samples into the spectrometer's graphite tube. The limits of detection (LOD) and quantification (LOQ calculated for 20 readings of the blank of the standard slurries (0.50% m/v of feces or feed devoid of selenium) were 0.31 mu g 1(-1) and 1.03 mu g 1(-1), respectively, for the standard feces slurries and 0.35 mu g 1(-1) and 1.16 mu g 1(-1), respectively, for the standard feed slurries. The proposed method was applied in studies of bioavailability of selenium in different fish feeds and the results proved consistent with that obtained from samples mineralized by acid digestion using the microwave oven. (C) 2007 Elsevier Ltd. All rights reserved.

Determination of chromium by GFAAS in slurries of fish feces to estimate the apparent digestibility of nutrients in feed used in pisciculture

This paper presents a simple, fast and sensitive method to determine chromic oxide (used as a biological marker of fish feed) in samples of fish feces by GFAAS through the direct introduction of slurries of the samples into the spectrometer's graphite tube. The standard samples of feces and of fish feed containing 0.10-1.00 mg kg(-1) of Cr2O3 were pre-frozen for I min in liquid nitrogen and then ground a cryogenic mill for 2 min, which reduced the samples' grain size to less than 60 mu m. The standard slurries were prepared by mixing 20 mg of standard samples of fish feed or feces with I mL of a solution containing 0.05% (v/v) of Triton X-100 and 0.50% (v/v) of suprapure HNO3 directly in the spectrometer's automatic sampling glass. The final concentrations of Cr2O3 present in the standard slurries were 2, 4, 8, 16 and 20 mu g L-1. After sonicating the mixture for 20s, 10 mu L of standard slurries were injected into the graphite tube, whose internal wall was lined with a metallic palladium film that acted as a permanent chemical modifier. The limits of detection (LOD) and quantification (LOQ) calculated for 20 readings of the blank of the standard slurries (2%, m/v of feces or feed devoid of minerals) were 0.81 and 2.70 mu g L-1 of Cr2O3 for the standard feces slurries, 0.84 and 2.83 mu g L-1 of Cr2O3 for the standard feed slurries. The proposed method was applied in studies of nutrient digestibility of different fish feeds and its results proved compatible with the results obtained from samples pre-mineralized by acid digestion. (c) 2005 Elsevier B.V. All rights reserved.

Gold (198Au) foils brachytherapy use on canine skin tumor

Este trabalho relata um caso clínico de carcinoma escamo celular cutâneo em um cão da raça Weimaraner, fêmea, 8 anos de idade tratado utilizando-se braquiterapia com folhas de Ouro-198. Os objetivos deste relato foram: avaliar o uso de um molde radioativo confeccionado para uso veterinário e sua eficácia no tratamento de um tumor de pele em cão. O método demonstrou ser eficaz no tratamento do tumor, mostrou ser uma prática segura para a equipe profissional envolvida, com baixos custos e resultado radiobiológico superior quando comparado com o tratamento padrão utilizado com outros elementos radioativos.

Efeito do cobre na atividade da enzima pirogalol peroxidase em plantas de Myriophyllum aquaticum cultivadas em solução nutritiva

Myriophyllum aquaticum é uma planta perene, herbácea, que pode se desenvolver totalmente submersa ou com a porção terminal dos ramos acima da superfície da água. É também considerada uma planta daninha que possui elevado potencial de colonização, o qual, dependendo da densidade populacional, pode causar aumento no teor de matéria orgânica e redução de oxigênio na água, comprometendo a qualidade da água e seus usos múltiplos. O objetivo do presente trabalho foi verificar a influência do cobre na atividade da pirogalol peroxidase de plantas de M. aquaticum submetidas à solução nutritiva contendo concentrações de cobre de 1,2; 11,2; 21,2; 31,2; e 41,2 µg L-1. O experimento foi conduzido em um delineamento experimental inteiramente casualizado, com quatro repetições e cinco tratamentos, aos quais as plantas foram submetidas durante 21 dias. Aos 81 dias após a instalação das mudas em solução nutritiva contendo os diferentes níveis de cobre, as folhas foram colhidas a partir do ápice da planta até o final do ramo, que não estavam em contato com a solução. Esse material fresco foi envolvido por plástico transparente e papel-alumínio e, a seguir, congelado em nitrogênio líquido, sendo armazenado em freezer a -20 ºC até o momento da determinação da atividade da enzima pirogalol peroxidase. A atividade da enzima foi progressiva com o aumento das doses de cobre. As plantas cultivadas com 40 µg L-1 de Cu2+ após três semanas, com base em avaliação visual, apresentaram redução no desenvolvimento.

Evaluation of Cu, Mn, and Se in Vegetables Using Ultrasonic Extraction and GFAAS Quantification

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

A solid paraffin-based carbon paste electrode modified with 2-aminothiazole organofunctionalized silica for differential pulse adsorptive stripping analysis of nickel in ethanol fuel

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 x 10(-9) to 1.0 x 10(-6) mol L-1 with detection limit of 2.0 x 10(-9) mol L-1. Recovery values between 96.5 and 102.4% were obtained for commercial samples spiked with 1.0 mu mol 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. (c) 2006 Elsevier B.V. All rights reserved.

Metallomic study on plasma samples from Nile tilapia using SR-XRF and GFAAS after separation by 2D PAGE: initial results

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Levels of copper in Nile tilapia from Brazil

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

In situ evaluation of anticancer drug methotrexate-DNA interaction using a DNA-electrochemical biosensor and AFM characterization

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

GFAAS Determination of Zinc in Fish Feed and Feces Using Slurry Sampling

This paper presents a simple, fast, and sensitive method to determine zinc in samples of feces and fish feed by electrothermal atomic absorption spectrometry through the direct introduction of slurries of the samples into the spectrometer's graphite tube. The procedure is based on the injection of 10 mu L of an acidified aqueous solution containing 0.50% w/v of feces or feed and 0.50% v/v HNO(3) into graphite tube. The limits of detection and quantification calculated for 20 readings of the blank of the standard slurries (0.50% w/v of feces or feed devoid of zinc) were 0.04 and 0.13 mu g L(-1) for the standard feces slurries and 0.05 and 0.17 mu g L(-1) for the standard feed slurries. The proposed method was applied in studies of digestibility of zinc in different fish feeds, and their results proved compatible with that obtained from samples mineralized by acid digestion using microwave oven.

Initiating structural studies of Lys49-PLA2 homologues complexed with an anionic detergent, a fatty acid and a natural lipid

Lys49-Phospholipase A(2) (Lys49-PLA(2) - EC 3.1.1.4) homologues damage membranes by a Ca2+-independent mechanism which does not involve catalytic activity. Both MjTX-II from Bothrops moojeni and BthTX-I from Bothrops jararacussu are dimeric in solution and in the crystalline states, and a model for the Ca2+-independent membrane damaging mechanism has been suggested in which flexibility at the dimer interface region pert-nits quaternary structural transitions between open and closed membrane bound dimer conformations which results in the perturbation of membrane phospholipids and disruption of the bilayer structure [1]. With the aim of gaining insights into the structural determinants involved in protein/lipid association, we report here the crystallization and preliminary X-ray analysis of the (i) MjTX-II/SDS complex at a resolution of 2.78Angstrom, (ii) MjTX-II/STE complex at a resolution of 1.8 Angstrom and (W) BthTX-I/DMPC complex at 2.72Angstrom. These complexes were crystallized by the hanging drop vapour-diffusion technique in (i) HEPES buffer (pH 7.5) 1.8M ammonium sulfate with 2% (w/v) polyethyleneglycol 400, in (ii) 0.6-0.8 M sodium citrate as the precipitant (pH 6.0-6.5) and in (iii) sodium citrate buffer (pH 5.8) and PEG 4000 and 20% isopropanol, respectively. Single crystals of these complexes have been obtained and X-ray diffraction data have been collected at room temperature using a R-AXIS IV imaging plate system and graphite monochromated Cu Kalpha X-ray radiation generated by a Rigaku RU300 rotating anode generator for (i) and (W) and using using a Synchrotron Radiation Source (Laboratorio Nacional de Luz Sincrotron, LNLS, Campinas, Brazil) for (ii).

Metal fluxes at the sediment-water interface in rivers in the Turvo/Grande drainage basin, So Paulo State, Brazil

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)