Emprego de sílica gel organicamente modificada e impressa ionicamente para pré-concentração seletiva on-line de íons cobre

The present work purposes the preparation of a silica gel sorbent organically modified with 2-aminoethyl-3-aminobutylmethyldimethoxysilane (AAMDMS) and imprinted with Cu2+ ions by means surface imprinting technique and its use for selective on-line sorbent preconcentration of Cu2+ ions with further UV-VIS spectrophotometric determination by flow injection analysis. The Cu2+-imprinted silica gel, when compared with non imprinted silica gel and silica gel, showed from the binary mixture of Cu2+/Ni2+ relative selectivity coefficient (k') of 6.84 and 5.43 and 6.64 and 19.83 for the mixture Cu2+/Pb2+, thus demonstrating higher selectivity of Cu2+-imprinted silica gel towards Cu2+ ions. Under optimized condition, the on-line preconcentration method provided detection limit of 3.4 μg L-1 and linear range ranging from 30.0 up to 300.0 μg L-1 (r = 0.995). The accuracy of method was successfully assessed by analyzing different kind of spiked water samples with recovery values ranging from 92.2 up to 103.0%.

Otimização e validação de método para determinação de ácidos orgânicos em vinhos por cromatografia líquida de alta eficiência

The organic acids (tartaric, malic, citric, lactic and succinic) are de main components responsible for the acidity in the wine. This method for simultaneous determination of organic acids and interfering peaks in wines can be achieved in 16 min. The sample preceded by a dilution and filtration step. The chromatographic separation required one reversed phase column, isocratic mobile phase (acetonitrila, formic acid in water) and detection wavelength was set at 212 nm. The validation confirmed good repeatability, recovery and application in red and white wines.

Terbinafine: optimization of a LC method for quantitative analysis in pharmaceutical formulations and its application for a tablet dissolution test

A simple liquid chromatographic method was optimized for the quantitative determination of terbinafine in pharmaceutical hydroalcoholic solutions and tablets, and was also employed for a tablet dissolution test. The analysis was carried out using a RP-C18 (250 mm × 4.6 mm, 5 μm) Vertical® column, UV-Vis detection at 254 nm, and a methanol-water (95:5, v/v) mobile phase at a flow-rate of 1.2 mL min-1. Method validation investigated parameters such as linearity, precision, accuracy, robustness and specificity, which gave results within the acceptable range. The tablets dissolution was quite fast: 80% of the drug was dissolved within 15 min.

Spectroscopic characterization of schiff base-copper complexes immobilized in smectite clays

Herein, the immobilization of some Schiff base-copper(II) complexes in smectite clays is described as a strategy for the heterogenization of homogeneous catalysts. The obtained materials were characterized by spectroscopic techniques, mostly UV/Vis, EPR, XANES and luminescence spectroscopy. SWy-2 and synthetic Laponite clays were used for the immobilization of two different complexes that have previously shown catalytic activity in the dismutation of superoxide radicals, and disproportionation of hydrogen peroxide. The obtained results indicated the occurrence of an intriguing intramolecular redox process involving copper and the imine ligand at the surface of the clays. These studies are supported by computational calculations.

Biodegradação de uma mistura de corantes têxteis usando o fungo Ganoderma sp: um estudo cinético

The kinetics of biodegradation by the fungus Ganoderma sp of textile dyes Yellow, Blue and Red Procion were studied in effluents using UV-Vis spectroscopy, Partial Least Squares Regression (PLS) and univariate analysis. The kinetic of the reactions were founded intermediate between first and second orders and the rate constants were calculated. The biodegradation after 72 h at 28 ºC were 33.6, 43.5 and 57.7% for the dyes Yellow, Blue and Red Procion, respectively. The quantitative analysis of the effluent by HPLC method can not be used without previous separation.

Adsorção do corante azul de metileno em partículas de argilominerais: análise dos tamanhos das partículas

Interactions of cationic dye methylene blue (MB) with clay particles in aqueous suspension have been extensively studied. As already known, the number of natural negative charges on the clay modifies significantly the particle sizes dispersed in water and therefore the nature of the interaction with the dye. This work evaluated with UV-Vis spectroscopy method how the clay particle sizes weighted on the adsorption and rearrangement of the dye molecules in aqueous system. The results obtained from light-scattering measurements confirmed that larger particles are found in suspensions containing the high-charged clays as the visible absorption band related to the MB aggregates (570 nm) on these suspensions prevailed.

Método para determinação de carboidratos empregado na triagem de adulterações em café

The objective in this work was to validate a chromatography method for the determination of total carbohydrates in soluble coffee, using a HPLC-UV-VIS with postcolumn derivatization system, in order to verify adulterant additions. The validated method was accurate and robust. Adulteration could be observed by increasing xylose and glucose levels in samples with addition of coffee husks and starchy products while decreasing of galactose and mannose characteristic carbohydrates presenting in high concentration in soluble coffees produced by arabica and robusta coffee beans.

Materiais híbridos orgânico-inorgânicos (ormosil) obtidos por sol-gel com potencial uso como filtro solar

This work aimed at the synthesis and characterization of particles of modified silica containing the organic filter dibenzoylmethane (DBM) by the hydrolytic sol-gel method, with modifications to the Stöber route. The structures of the resulting Xerogels were characterized by diffuse reflectance UV-VIS spectroscopy in the solid state, infrared absorption spectroscopy, Scanning Electron Microscopy (SEM) and 29Si Nuclear Magnetic Resonance (29Si NRM). The results showed favorable formation of hybrid organic-inorganic nanoparticles with efficient absorption/reflectance of radiation in the UV / VIS range, which enables their potential use as sunscreen.

Influência do tipo de ácido e tempo de envelhecimento na atividade fotocatalítica de filmes finos de TiO2

TiO2 thin films were prepared by the sol-gel method using different acids (HCl and HAc), with a parallel evaluation of the gel ageing effects on the film properties. After the thermal treatments, the resulting materials were characterized through gravimetric analysis, UV-VIS spectrophotometry (from which optical parameters such as band gap was derived), XRD, morphological surface analysis (AFM) and photocatalytic activity. The majority of the obtained thin films parameters were similar independent of the acid type and the ageing time of the gel. Nevertheless, a visible effect of the surface morphology properties on the films and their photocatalytic activity was observed.

Degradação fotoeletroquímica do herbicida bentazona sobre eletrodos de carbono modificados por TiO2

This work involved the study of degradation of the herbicide bentazone in aqueous solution by different routes, in order to search a method that generates safe products to the environment. It was tested electrochemical polarization methods involving positive and negative potential, irradiation with UV light and deposition of TiO2 on the electrode surface, seeking a catalytic effect. After different times of degradation, aliquots were removed and the scan of molecular absorption spectrum of UV-Vis was performed. From the spectra decay of bentazone, the kinetics of different processes was accompanied and the rate constants were determined.

Efeito da adição de lantânio em catalisadores de Ni/ZrO2 aplicados na reação de reforma a vapor de etanol

The catalytic performance of Ni/ZrO2 catalysts loaded with different lanthanum content for steam reforming of ethanol was investigated. Catalysts were characterized by BET surface area, X-ray diffraction, UV-vis spectroscopy, temperature programmed reduction, and X-ray absorption fine structure techniques. Results showed that lanthanum addition led to an increase in the degree of reduction of both NiO and nickel surface species interacting with the support, due to the higher dispersion effect. The best catalytic performance at 450 ºC was found for the Ni/12LZ catalyst, which exhibited an effluent gaseous mixture with the highest H2 yield.

Avaliação de procedimentos para quantificação espectrofotométrica de flavonoides totais em folhas de Bauhinia forficata Link

Interest in analytical methods for quality control of herbal drugs has grown sharply due to the scarcity of monographs in official manuals. Thus, the aim of the present study was to evaluate analytical procedures for quantitative determination of flavonoids from leaves of Bauhinia forficata Link (pata-de-vaca). Two procedures for quantification of total flavonoids (with and without acid hydrolysis) by spectrophotometry were tested. The proposed methods proved to be specific, sensitive, precise, accurate and robust, being suitable for routine laboratory use.

Desenvolvimento e validação de método analítico para a determinação de sulfassalazina em suspensão oral: comparação do método espectrofotométrico e de cromatografia líquida de alta eficiência (CLAE)

Sulfasalazine is a prodrug used in the treatment of the Chron's disease and rheumatoid arthritis. Two analytical methods for analysis of sulfasalazine in oral suspension were validated using Spectrophotometric and HPLC. There is not any pharmacopoeic method to assay sulfasalazine in oral suspension. The methods are insurance and fast execution for the quality control. Both, suspension and tablets 500 mg (Azulfin®) had been analyzed by methods using UV/VIS and HPLC and the results were satisfactory.

Sorção de Diuron em minerais da fração argila

The objective of the present study was to evaluate the adsorption of the herbicide Diuron onto smectite and Fe oxides minerals. Ninety mg of each mineral, 1 mL of 0.15 mol L-1 CaCl2 and 8 mL of Diuron (0.25-10.00 mg L-1) were used in triplicates. These materials were shaken, ultra centrifuged and the supernatant collected and analysed on a UV-Vis spectrophotometer. The Diuron presented low adsorption onto clay mineral fractions. Adsorption was greater onto Fe oxides at pH 7.0, possibly due to proximity to the point of zero charge of these minerals.

Ácidos fenólicos, flavonoides e atividade antioxidante em méis de Melipona fasciculata, M. flavolineata (Apidae, Meliponini) e Apis mellifera (Apidae, Apini) da Amazônia

Honey produced by three stingless bee species (Melipona flavolineata, M. fasciculata and Apis mellifera) from different regions of the Amazon was analyzed by separating phenolic acids and flavonoids using the HPLC technique. Data were subjected to multivariate statistical analysis (PCA, HCA and DA). Results showed the three species of honey samples could be distinguished by phenolic composition. Antioxidant activity of the honeys was determined by studying the capacity of inhibiting radicals using DPPH assay. Honeys with higher phenolic compound contents had greater antioxidant capacity and darker color.