Optimisation of stir bar sorptive extraction and liquid desorption combined with large volume injection-gas chromatography–quadrupole mass spectrometry for the determination of volatile compounds in wines

Stir bar sorptive extraction and liquid desorption followed by large volume injection coupled to gas chromatography–quadrupole mass spectrometry (SBSE–LD/LVI-GC–qMS) had been applied for the determination of volatiles in wines. The methodology was optimised in terms of extraction time and influence of ethanol in the matrix; LD conditions, and instrumental settings. The optimisation was carried out by using 10 standards representative of the main chemical families of wine, i.e. guaiazulene, E,E-farnesol, β-ionone, geranylacetone, ethyl decanoate, β-citronellol, 2-phenylethanol, linalool, hexyl acetate and hexanol. The methodology shows good linearity over the concentration range tested, with correlation coefficients higher than 0.9821, a good reproducibility was attained (8.9–17.8%), and low detection limits were achieved for nine volatile compounds (0.05–9.09 μg L−1), with the exception of 2-phenylethanol due to low recovery by SBSE. The analytical ability of the SBSE–LD/LVI-GC–qMS methodology was tested in real matrices, such as sparkling and table wines using analytical curves prepared by using the 10 standards where each one was applied to quantify the structurally related compounds. This methodology allowed, in a single run, the quantification of 67 wine volatiles at levels lower than their respective olfactory thresholds. The proposed methodology demonstrated to be easy to work-up, reliable, sensitive and with low sample requirement to monitor the volatile fraction of wine.

Optimisation of solid-phase microextraction combined with gas chromatography–mass spectrometry based methodology to establish the global volatile signature in pulp and skin of Vitis vinifera L. grape varieties

The volatiles (VOCs) and semi-volatile organic compounds (SVOCs) responsible for aroma are mainly present in skin of grape varieties. Thus, the present investigation is directed towards the optimisation of a solvent free methodology based on headspace-solid-phase microextraction (HS-SPME) combined with gas chromatography–quadrupole mass spectrometry (GC–qMS) in order to establish the global volatile composition in pulp and skin of Bual and Bastardo Vitis vinifera L. varieties. A deep study on the extraction-influencing parameters was performed, and the best results, expressed as GC peak area, number of identified compounds and reproducibility, were obtained using 4 g of sample homogenised in 5 mL of ultra-pure Milli-Q water in a 20 mL glass vial with addition of 2 g of sodium chloride (NaCl). A divinylbenzene/carboxen/polydimethylsiloxane fibre was selected for extraction at 60 °C for 45 min under continuous stirring at 800 rpm. More than 100 VOCs and SVOCs, including 27 monoterpenoids, 27 sesquiterpenoids, 21 carbonyl compounds, 17 alcohols (from which 2 aromatics), 10 C13 norisoprenoids and 5 acids were identified. The results showed that, for both grape varieties, the levels and number of volatiles in skin were considerably higher than those observed in pulp. According to the data obtained by principal component analysis (PCA), the establishment of the global volatile signature of grape and the relationship between different part of grapes—pulp and skin, may be an useful tool to winemaker decision to define the vinification procedures that improves the organoleptic characteristics of the corresponding wines and consequently contributed to an economic valorization and consumer acceptance.

Nanosistemas de penicilina G benzatina para tratamento profilático da febre reumática: estudo analítico

Investigations in the field of pharmaceutical analysis and quality control of medicines require analytical procedures with good perfomance characteristics. Calibration is one of the most important steps in chemical analysis, presenting direct relation to parameters such as linearity. This work consisted in the development of a new methodology to obtain calibration curves for drug analysis: the stationary cuvette one. It was compared to the currently used methodology, and possible sources of variation between them were evaluated. The results demonstrated that the proposed technique presented similar reproducibility compared to the traditional methodology. In addition to that, some advantages were observed, such as user-friendliness, cost-effectiveness, accuracy, precision and robustness. Therefore, the stationary cuvette methodology may be considered the best choice to obtain calibration curves for drug analyis by spectrophotometry

Validação interlaboratorial do teste de polarização fluorescente para o diagnóstico sorológico da brucelose bovina

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

Development of Y-chromosome-Specific SCAR Markers Conserved in Taurine, Zebu and Bubaline Cattle

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

Utilização de marcador molecular SCAR na identificação de Fusarium subglutinans, agente causal da malformação da mangueira

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

Análise tribológica das malhas multifuncionais obtidas por multicamadas

The present work consists in the analysis of tribologycal properties of basic and multifunctional knitted fabrics. This knowledge has fundamental importance for the textile industry since it can quantify, in an objective way, the tactil. The fabrics used were characterized by friction and mechanical tests for determining the viscoelastic region, wear resistance and friction coefficient of the fabrics used. The stress-strain curve was obtained by the method Kawabata, KES-FB1. Wear tests performed with the aid of equipment Martindale. The measurement of friction coefficient, two methods were used and analyzed comparatively. The first was a method already established worldwide known as KES-FB4 and the second was an innovative method called FRICTORQ, developed by the University of Minho. These two methods were compared taking into account the relative motion between the tribologycal pairs are different from each method. While the first motion is translational, the second is rotational. It was formal that the knitted had a multifunctional fabrics tribologycal performance which was better than the basic knitted fabrics, as the viscoelastic region, was laager highlighting a multifunctional structure, with greater wear resistance mainly on the back side of the knitted fabrics and lower friction coefficient. Performing a comparative analysis between two methods used to measure the friction coefficient, it was formal that both methods were consistent in terms of results. In operational terms, the FRICTORQ showed ease of operation and increased reproducibility of results

Síntese de pigmentos cerâmicos inorgânicos nanométricos pela rota dos precursores poliméricos

Considering the constant evolution of technology in growth and the need for production techniques in the ceramics area to move forward together, we sought in this study, the research and development of polymeric precursor method to obtain inorganic ceramic pigments. Method that provides quality to obtain the precursor powders of oxides and pigments at the same time, offers time and cost advantages, such as reproducibility, purity and low temperature heat treatment, control of stoichiometry. This work used chromium nitrate and iron nitrate as precursors. The synthesis is based on the dissolution of citric acid as a complexing agent, addition of metal oxides, such as ion chromophores; polymerization with ethylene glycol and doping with titanium oxide. Passing through precalcination, breakdown, thermal treatments at different temperatures of calcination (700 to 1100 oC), resulting in pigments: green for chromium oxide deposited on TiO2 (CrTiO3) and orange for iron oxide deposited on TiO2 ( FeTiO3). Noticing an increase of opacity with increasing temperature. Were performed thermal analysis (TG and ATD) in order to evaluate its thermodecomposition. The powders were also characterized by techniques such as XRD, revealing the formation of crystalline phases such as iron titanate (FeTiO3) and chrome titanate (CrTiO3), SEM, demonstrating formation of rounded particles for both oxides and Spectroscopy in the UV-Visible Region, verifying the potential variation and chromaticity os pigments. Thus, the synthesized oxides were within the requirements to be applied as pigments and shown to be possible to propose its use in ceramic materials

Relação entre a tensão aplicada e a sensação de desconforto nos músculos isquiotibiais durante o alongamento

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

Biomimetic biosensor based on lipidic layers containing tyrosinase and lutetium bisphthalocyanine for the detection of antioxidants

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

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.

ANÁLISE DESCRITIVA QUANTITATIVA da AGUARDENTE DE CANA DURANTE O ENVELHECIMENTO em TONEL DE CARVALHO (Quercus alba L.)

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

Validação de método analítico por espectrofotometria UV para sistema emulsionado lipídico contendo benznidazol

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Consistência interna e reprodutibilidade da versão em português do critério de diagnóstico na pesquisa para desordens temporomandibulares (RDC/TMD - Eixo II)

OBJETIVO: Estudar a confiabilidade, da versão em português, do questionário para o diagnóstico psicológico e psicossocial dos indivíduos com desordens temporomandibulares (RDC/TMD). MÉTODOS: Foram entrevistados 109 indivíduos, de ambos sexos, que demandaram atendimento junto à Clínica de Fisioterapia do Centro Universitário de Araraquara, de janeiro a julho de 2006. Os questionários foram aplicados por um único examinador. Após duas semanas, o mesmo foi reaplicado em 36 indivíduos. Para avaliação da consistência interna do método, utilizou-se o Coeficiente Alfa de Cronbach; para análise da reprodutibilidade intra-examinador, o Coeficiente de Correlação Intraclasse (ro) e a estatística Kappa (kapa), respectivamente às variáveis de natureza quantitativa e qualitativa. RESULTADOS: A consistência interna para as dimensões intensidade da dor crônica e incapacidade; limitação da função mandibular; sintomas físicos não-específicos, incluindo os itens de dor; sintomas físicos não-específicos, excluindo os itens de dor e depressão foi de 0,8479, 0,8971, 0,8673, 0,8080 e 0,9270 respectivamente, atestando ao método excelente validade interna. Obteve-se excelente concordância intra-examinador para as questões referentes ao tempo de presença da dor e sua gradação, e boa para a questão referente à dor presente. Os menores valores de kapa relacionaram-se aos itens de sintomas físicos e depressão. A percepção de estalos ou rangidos pelos indivíduos apresentou concordância regular bem como a questão referente à procura de profissional para tratamento da dor. As demais questões apresentaram reprodutibilidade boa e ótima, sendo que a maioria dessas apresentou nível máximo de concordância. CONCLUSÃO: A versão adaptada para o português mostrou-se confiável para detecção das alterações psicológicas e psicossociais associadas às desordens temporomandibulares.

Validade e reprodutibilidade do Wii Balance Board para avaliação do equilíbrio vertical estático: um novo método de avaliação.

The Wii Balance Board (WBB) began to be investigated as a low-cost alternative for assessing static balance in vertical posture. However, studies employed methodological procedures that did not eliminate result variability between the tests and equipment used. Objective: Determine the validity and reproducibility of the WBB as an instrument for assessing static balance in the vertical position, using simultaneous data analysis and superimposed equipment. Methods: This is an accuracy study of 29 healthy young individuals of both sexes aged 18 to 30 years. Subjects were assessed 24h apart (test-retest), using unipodal and bipodal support tests, with eyes closed and open. To that end the WBB was placed on top of a force platform (FP) and data (postural sway) were collected simultaneously on both devices. Validity and reproducibility were analyzed using the interclass correlation coefficient (ICC). Finally, Bland-Altman analysis was applied to assess agreement. Results: The sample was composed of 23 women and 6 men, with mean age of 24.2±6.3 years, 60.7±6.3 kg and 1.64±4.2 m. The validity of the WBB compared to the FP was excellent for all 4 tasks proposed (ICC = 0.93 0.98). The reproducibility analyzed by test-retest was excellent for the bipodal support tasks (ICC = 0.93-0.98) and only moderate for the unipodal support tests (ICC = 0.46 0.70). Graphic analysis exhibited good agreement between the devices, since most of the measures were within the limits of agreement. Conclusion: this study proved the validity and reproducibility of the Wii Balance Board as an instrument for assessing static balance in vertical posture, using simultaneous analysis with superimposed equipment. Thus, the WBB has been increasingly used by physical therapists and other health professionals in their clinical practice, as both a rehabilitation and assessment tool