HPLC-DAD methodology for the quantification of organic acids, furans and polyphenols by direct injection of wine samples

This article proposes a simple and sensitive HPLC method with photo-diode array detection for the analysis of organic acids, monomeric polyphenols and furanic compounds in wine samples by direct injection. The chromatographic separation of 8 organic acids, 2 furans and 22 phenolic compounds was carried out with a buffered solution (pH 2.70) and acetonitrile as mobile phases and a difunctionally bonded C18 stationary phase, Atlantis dC18 (250 4.6 mm, 5mm) column. The elution was performed in 12 min for the organic acids and in 60 min for the phenolic compounds, including phenolic acids, stilbenes and flavonoids. Target compounds were detected at 210 nm (organic acids, flavan-3-ols and benzoic acids), 254 nm (ellagic acid), 280 nm (furans and cinnamic acid), 315 nm (hydroxycinnamic acids and trans-resveratrol) and 360 nm (flavonoids). The RSD for the repeatability test (n55) of peak area and retention times were below 3.1 and 0.3%, respectively, for phenolics and below 1.0 and 0.2% for organic acids. The RSDs expressing the reproducibility of the method were higher than for the repeatability results but all below 9.0%. Method accuracy was evaluated by the recovery results, with averaged values between 80 and 104% for polyphenols and 97–105% for organic acids. The calibration curves, obtained by triplicate injection of standard solutions, showed good linearity with regression coefficients higher than 0.9982 for polyphenols and 0.9997 for organic acids. The LOD was in the range of 0.07–0.49 mg/L for polyphenols (cinnamic and gallic acids, respectively) and 0.001–0.046 g/L for organic acids (oxalic and lactic acids, respectively). The method was successfully used to measure and assess the polyphenolic fingerprint and organic acids profile of red, white, rose ´ and fortified wines.

Análise da reprodutibilidade de parâmetros no domínio da frequência do sinal EMG utilizados na caracterização da fadiga muscular localizada

The aim of this study was to analyze the reproducibility of the electromyography signal's parameters (EMG) in the frequency domain used in the characterization of localized muscle fatigue. Fifteen male subjects underwent a fatigue test based on isometric knee extension, being held at three different times at intervals of seven days. To assess the reproducibility of data between the tests we calculated the correlation coefficient (ICC) for the median frequency (MF) in total exercise time (MFT), MF obtained for every 10% of exercise time (MF10%) and the powers of the frequency bands obtained by dividing the power spectrum at windows of 20 Hz. The results showed: (1) excellent reproducibility for MFT, (2) good reproducibility for MF10%, and (3) greater variation in the signal EMG bands from 20 to 120 Hz, especially at the bands of 20-40 Hz and 40-60 Hz, which showed greater sensitivity to the process of muscle fatigue. We conclude that the MF is a variable that shows good reproducibility and that the fragmented analysis of the power spectrum, by means of frequency bands, showed that significant variations occur in the EMG signal during the installation of the fatigue process, having potential to become a new method for the characterization of localized muscle fatigue.

Vortex dynamics in mesoscopic superconducting square of variable surface

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

Off line extraction of phenol from human urine sample with isoamyl alcohol and determination by HPLC

This method has been developed for extraction and determination of phenol in a urine sample by high performance liquid chromatography.After acid hydrolysis, the free phenol was extracted with isoamyl alcohol solvent, followed by back extraction with 0.5 mol.L-1 sodium hydroxide solution and analyzed by an isocratic HPLC Varian System, equipped with reverse-phase column (MicroPak-C-18). The mobile phase was acetonitrile in 0.01 mol.L-1 hydrochloric acid solution, (20:80 v/v), and at a now-rate of 1.0 mL.min-1. The chromatogram was monitored at 220 nm in room temperature. The identification was based on retention time and the quantification was performed by automatic peak-area determination, corrected for the external standards method.The recovery was higher than 99.5 % for phenol and reproducibility of method was shown to be 2.3% standard deviation and 5.6% coefficient of variance (n=20). The limit detection was 0.05 mgL(-1) and a range of 0.05 to 20.0 mgL(-1) of phenol for linearity.

Determination of the numerical parameters of a continuous damage model for the structural analysis of clay brick masonry

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

Boundary identification criteria and geometry analysis of Al 7050 stretch zone from elevation profiles

This article describes the development of a method for analysis of the shape of the stretch zone surface based on parallax measurement theory and using digital image processing techniques. Accurate criteria for the definition of the boundaries of the stretch zone are established from profiles of fracture surfaces obtained from crack tip opening displacement tests on Al-7050 alloy samples. The elevation profiles behavior analysis is based on stretch zone width and height parameters. It is concluded that the geometry of the stretch zone profiles under plane strain conditions can be described by a semi-parabolic relationship. (C) Elsevier B.V., 1999. All rights reserved.

Digital Light Microscopy of Macroporous Ceramics Processed by Consolidation Casting with Mixtures of Native Starches

Porosity in starch consolidation casting technique is rightly related to original size and morphology of starch granules, leaving a pore structure after burning out. This work reports the results for the addition of different native potato and corn starch proportions in suspension,; with TiO(2) (rutile) powder. Gelling temperature have been defined after observation under light microscopy using a heating stage. Analysis of porous network and isolated pores have been clone from images of samples surfaces obtained by depth from focus reconstruction, revealing a qualitative correlation of pores characteristics and starches additions in suspensions, suggesting that the presence of isolated or interconnected pores can be handled by starches selection to control the amylopectin and amylose contents in slurries. Also, the analysis of porous fraction distribution shows no consistent pattern through specimens' volume according to starches in mixtures.

3-D reconstruction by extended depth-of-field in failure analysis - Case study II: Fractal analysis of interlaminar fracture in carbon/epoxy composites

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

Elastic modulus and hardness of CaTiO3, CaCu3Ti4O12 and CaTiO3/CaCu3Ti4O12 mixture

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Surface Corrosion of Ti-16Si-4B Powder Alloy Implanted With Nitrogen by Plasma-Based Technique

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

Photopyroelectric response of PTCa/PEEK composite

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

Stability of cp-Ti and Ti-6Al-4V alloy for dental implants as a function of saliva pH - an electrochemical study

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Comparison of space analysis performed on plaster vs. digital dental casts applying Tanaka and Johnston's equation

OBJETIVO: comparar medidas de tamanhos dentários, suas reprodutibilidades e a aplicação da equação de regressão de Tanaka e Johnston na predição do tamanho dos caninos e pré-molares em modelos de gesso e digital. MÉTODOS: trinta modelos de gesso foram escaneados para obtenção dos modelos digitais. As medidas do comprimento mesiodistal dos dentes foram obtidas com paquímetro digital nos modelos de gesso e nos modelos digitais utilizando o software O3d (Widialabs). A somatória do tamanho dos incisivos inferiores foi utilizada para obter os valores de predição do tamanho dos pré-molares e caninos utilizando equação de regressão, e esses valores foram comparados ao tamanho real dos dentes. Os dados foram analisados estatisticamente, aplicando-se aos resultados o teste de correlação de Pearson, a fórmula de Dahlberg, o teste t pareado e a análise de variância (p < 0,05). RESULTADOS: excelente concordância intraexaminador foi observada nas medidas realizadas em ambos os modelos. O erro aleatório não esteve presente nas medidas obtidas com paquímetro, e o erro sistemático foi mais frequente no modelo digital. A previsão de espaço obtida pela aplicação da equação de regressão foi maior que a somatória dos pré-molares e caninos presentes nos modelos de gesso e nos modelos digitais. CONCLUSÃO: apesar da boa reprodutibilidade das medidas realizadas em ambos os modelos, a maioria das medidas dos modelos digitais foram superiores às do modelos de gesso. O espaço previsto foi superestimado em ambos os modelos e significativamente maior nos modelos digitais.

Artificial methods of dentine caries induction: A hardness and morphological comparative study

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Detection of the Vandibular Canal and the Mental Foramen in Panoramic Radiographs: Intraexaminer Agreement

The aim of this study was to evaluate the intraexaminer agreement in the detection of the mandibular canal roof (MCR) and mental foramen (MF) in panoramic radiographs. Forty panoramic radiographs of edentulous patients were used. Two calibrated examiners (A and B) read the images 2 times, for both sides independently, under blind conditions. The interval between the readings was 10 days. The intraexaminer agreement in the interpretation of MCR and MF was performed by kappa statistics with linear weighting (x). The intraexaminer agreement for the detection of MCR, in the left side, was good for both examiners (A: kappa = 0.67; B: kappa = 0.71). Related to the right side, it was found to be kappa = 0.47 and kappa = 0.62, respectively to A and B. The intraexaminer agreement for the detection of MF was good for both examiners interpreting the left side (A: kappa = 0.61; B: kappa = 0.63), and in relation to the right side, it was moderate (A: kappa = 0.51) and fair (B: kappa = 0.38). The intraexaminer agreement in the detection of MCR was good and from good to fair in the detection of MF.