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Desenvolvimento de procedimentos automáticos para determinação de etanol, glicerol e ácido tartárico em vinho empregando multicomutação em fluxo
(Universidade Federal de São Carlos, 2004-08-18) Fernandes, Elizabeth Nunes; Reis, Boaventura Freire dos; https://lattes.cnpq.br/7619359855870896
In the present work, flow systems for the determination of ethanol, glycerol and tartaric acid in wine without previous sample treatment are described. The flow system were based on multicommutation and controlled by microcomputer allowing that the analytic procedures were accomplished automatically without the intervention of the operator. For ethanol determination the proposed procedure employed detection by chemiluminescence using equipment developed in the Centro de Energia Nuclear na Agricultura. The detection device comprised a glass flow cell that was installed between two photodiodes forming a compact unit that was packed into a metallic box. The procedure for ethanol determination was based on the enzymatic reaction using alcohol oxidase producing acetaldehyde and hydrogen peroxide. The hydrogen peroxide reacted with luminol catalyzed by potassium hexacianoferrate (III) producing chemiluminescence. The luminescence intensity presented a direct relationship with ethanol concentration. The system allowed wine sample analysis without any prior treatment, presenting linear response between 2.5 and 25% (v/v) of ethanol characterized by the equation Signal (mV) = (20 ± 1) + (7.8 ± 0.3) % of ethanol (r = 0.997), a coefficient of variation of 1.8% for a typical wine sample presenting 11 % (v/v) of ethanol and a sampling frequency of 28 determinations for hour. For glycerol determination it was based on the reaction with glycerol dehydrogenase in presence the cofactor NAD+, resulting in oxidation of NAD+ to NADH that was monitored at 340 nm. After system optimization, a linear response between 2.0 and 10.0 g l-1 of glycerol characterized by the equation Abs = (0.1320 ± 0.003) + (149x10-4 ± 4x10-4) g l-1 of glycerol (r = 0.998), a coefficient of variation of 1.6% for a typical wine sample presenting 5.3 g L-1 of glycerol and a sampling frequency of 33 determinations for hour were obtained. For tartaric acid determination a single line module of analysis was designed, based on the reaction with vanadate and detection was carried out by spectrophotometry at 490 nm after reaction with sodium vanadate. The procedure presented a linear relationship between 0.50 and 10.0 g l-1 of tartaric acid characterized by the equation Abs = (0.206 ± 0.001) + 0.0404 ± 2.76x10-4 g l-1 of tartaric acid (r = 0.999), a coefficient of variation of 2.1% for a typical wine sample presenting 1.84 g L-1 of tartaric acid and a sampling frequency of 28 determinations for hour. Comparing the reagent consumption with earlier works it was observed that reduction about 65% was obtained. The three systems that comprise this work when applied to analysis wine samples presented results, which compared with results obtained using official methods no significant difference at 90 % confidence level were observed.
Quelato complexos de oxovanádio (IV): potenciais mimetizadores de insulina
(Universidade Federal de São Carlos, 2004-08-18) Barbosa, Andrey Castro; Dockal, Edward Ralph; https://lattes.cnpq.br/6461328124491559
Based on studies of another studies that explored the capacity of oxovanadium(IV) ion to mimic insulin, we had the idea to contribute with this line of research. For this, our choice of ligands was trans - 1,2 diamineciclohexane - N,N,N`,N` - tetraacétic (CDTA) and ethilenediaminetetraacétic (EDTA) acids, to synthesize the [VO(CDTA)], Na2[VO(EDTA)] and [(VO)2(EDTA)].4H2O complexes. These compounds were characterized by Infrared Spectroscopy, Ultraviolet and Visible Spectroscopy, Cyclic Voltammetry and Elemental Analysis. We also used Electronic Paramagnetic Resonance for compounds that contain EDTA ligands and X Ray analysis to analyze the compounds that contains two metallic centers. The last compound was used in biologic tests in Wistar rats.