Um experimento de análise em fluxo envolvendo reações enzimáticas e quimiluminescência

An experiment is proposed to introduce some fundamentals of flow analysis, chemiluminescence and kinetic monitoring of enzymatic reactions in undergraduate courses. Chemiluminescence detection is performed with a simple spectrophotometer equipped with a lab-made spiral flow cell constructed from a polyethylene tube. The hydrogen peroxide produced by the glucose oxidation in the presence of glucose oxidase is continuously monitored by the reaction with luminol in alkaline media in a flow injection system. The exercise allows also the discussion of important analytical features and the comparison with different optical methods of analysis.

Análise de ácidos graxos não-esterificados de plasma humano por cromatografia gasosa capilar com injeção sem divisão de fluxo

The aim of the present work was to test the combination of non-esterified fatty acid (NEFA) isolation using fumed silicon dioxide with capillary gas-chromatography (C-GC) with splitless injection for the analysis of NEFAs in human plasma. Injection volume, solvent re-condensation and split purge flow-rate were the parameters evaluated for the analysis of fatty acid methyl esters by C-GC. The use of a solvent re-condensation technique, associated with 1.0 µL injection and a split purge flow rate of 80 mL/min resulted in satisfactory analysis of NEFAs. Fourteen fatty acids were identified in plasma samples, ranging from 2.03 to 184.0 µmol/L. The combination of both techniques proved useful for routine analyses of plasma NEFAs.

Construção e avaliação de célula de fluxo para estudo da tensão interfacial dinâmica da interface fluxo líquido - sólido por despolarização da fluorescência

A simple low-cost flow cell was developed, built and optimized in order to observe dynamic interfacial tension of continuous flow systems. Distinct materials can be used in one of the cell walls in order to observe the intermolecular forces between the flowing liquid and the chemical constitution of the walls. The fluorescence depolarization was evaluated using Rhodamine B as fluorescent probe seeded in ethylene glycol. The effects of the positioning angles on the data acquired across the cell are reported. The reproducibility of the data was evaluated with a spectrometer assembled in-house and the relative standard deviation was below 3%.

Imobilização de enzimas a partir de "kit" comercial: determinação de parâmetros metabólicos em sangue animal empregando multicomutação em fluxo

Automatic flow procedures based on the multicommutation concept, dedicated to the determination of 3-hydroxybutyrate, glucose and cholesterol are proposed. The enzymes were immobilized on glass beads and packed into mini-columns that were coupled to a flow system. Sampling throughputs of 55, 40 and 40 determinations per hour, linear response from 10 to 150, 50 to 600, 25 to 125 mg L-1, detection limits of 1.5, 14 and 4 mg L-1 and relative standard deviations of 1, 2 and 2% for 3-hydroxybutyrate, glucose and cholesterol, respectively, were achieved.

Informações essenciais para a caracterização de um sistema de análise em fluxo

Essential aspects for characterization of a flow-based analytical procedure or system are discussed in order to permit the composition of a checklist that will lead to a protocol for reporting results and systems in flow analysis. Aspects more related to chromatographic procedures are not considered. The intent is to present normalized proposals in the field of flow analysis for practitioners and developers.

Determinação turbidimétrica de dipirona em fluxo utilizando um reator contendo cloreto de prata imobilizado em resina poliéster

A simple flow injection procedure was developed for determining dipyrone (1-phenyl-2,3-dimethyl-4-methylaminomethano-5-pyrazolone sodium, metamizol, analgin) in pharmaceutical formulations. The determination is based on the reduction of Ag+ ions to Ag0 by dipyrone. A colloidal suspension of Ag0 produced was transported by carrier solution (0.01 mol L-1 NaOH) and turbidimetrically detected at 425 nm. The analytical curve for dipyrone was linear in the range from 5.0 x 10-4 to 2.5 x 10-3 mol L-1 with a correlation coefficient of 0.9990. The detection limit was 1.3 x 10-4 mol L-1 (3sigmaB/slope). The relative standard deviation for ten successive measurements was 1.8% and an analytical frequency of 45 h-1 was obtained. The recovery values from three samples ranged from 96.0 to 102%.

Determinação indireta de N-acetil-L-cisteína por injeção em fluxo empregando Ce(IV) e ferroína

An indirect flow injection spectrophotometric procedure is proposed for the determination of N-acetyl-L-cysteine in pharmaceutical formulations. In this system, ferroin ([Fe(II)-(fen)2]2+) in excess, with a strong absorption at 500 nm, is oxidized by cerium(IV) yielding cerium(III) and [Fe(III)-(fen)2]3+ (colorless), thus producing a baseline. When N-acetyl-L-cysteine solution is introduced into the flow injection system, it reacts with cerium(IV) increasing the analytical signal in proportion to the drug concentration. Under optimal experimental conditions, the linearity of the analytical curve for N-acetyl-L-cysteine ranged from 6.5x10-6 to 1.3x10-4 mol L-1. The detection limit was 5.0x10-6 mol L-1and recoveries between 98.0 and 106% were obtained. The sampling frequency was 60 determinations per hour and the RSD was smaller than 1.4% for 2.2x10-5 mol L-1 N-acetyl-L-cysteine.

Quantificação de fluxos de mercúrio gasoso na interface solo/atmosfera utilizando câmara de fluxo dinâmica: aplicação na bacia do Rio Negro

Gaseous mercury sampling conditions were optimized and a dynamic flux chamber was used to measure the air/surface exchange of mercury in some areas of the Negro river basin with different vegetal coverings. At the two forest sites (flooding and non-flooding), low mercury fluxes were observed: maximum of 3 pmol m-2 h-1 - day and minimum of -1 pmol m-2 h-1 - night. At the deforested site, the mercury fluxes were higher and always positive: maximum of 26 pmol m-2 h-1 - day and 17 pmol m-2 h-1 - night. Our results showed that deforestation could be responsible for significantly increasing soil Hg emissions, mainly because of the high soil temperatures reached at deforested sites.

Estimativa do fluxo de amônia na interface ar-mar na Baía de Guanabara: estudo preliminar

In the begining of April 2004, concentrations of NHx (NH3 + NH4+) were measured in surface waters of the Guanabara Bay. Concentrations varied from 2 to 143 mmol L-1. Ammonia exchange at the air-sea interface was quantified using a numerical model. No measurement of NH3 concentration in air (c air) was performed. Thus, calculations of NH3 flux were based on the assumptions of c air = 1 and 5 µg m-3. Fluxes were predominantly from the water to the atmosphere and varied from -20 to almost 3500 µg N m-2 h-1.

Um novo índice de qualidade das águas para proteção da vida aquática aplicado ao Rio Atibaia, região de Campinas/Paulínia-SP

In this paper a water quality index is developed to subsidize management actions in the Atibaia River for upon protection of aquatic organisms. This index is composed of two measurable environmental parameters normaly, ammonia and dissolved oxygen, the latter representing the contribution of organic matter. Concentrations of these two variables were normalized on a scale from 0 to 100 and translated into statements of quality (excellent, good, regular, bad and very bad). The index was applied to three monitoring points in the Atibaia River and compared to other indices used by the State of São Paulo Environmental Agency (CETESB). The results showed that the degradation in this watershed follows the urban population density. The developed index is more restricted than the other ones routinely used to infer water quality.

Determinação turbidimétrica de metilbrometo de homatropina em formulações farmacêuticas empregando um sistema de análise por injeção em fluxo

A flow injection turbidimetric procedure exploiting merging zones is proposed for determining homatropine methylbromide (HMB) in pharmaceutical preparations. The determination is based on the precipitation reaction of homatropine methylbromide with AgNO3 solution to form a precipitate, which was measured at 410 nm. The analytical curve was linear in the HMB concentration range from 8.0x10-4 to 1.7x10-3 mol L-1, with a detection limit of 9.5x10-5 mol L-1. The recoveries ranged from 94.9 to 104 %, the sampling frequency was 75 h-1 and relative standard deviations were smaller than 2.0 % for solutions containing 1.2x10-3 and 1.5x10-3 mol L-1 HMB (n=10). The results obtained for commercial formulations using the FIA procedure were in good agreement with those obtained by using a comparative method (r= 0.9983).

Controle da biossíntese de poli-hidroxialcanoatos bacterianos através do fluxo de substratos

Manipulation of the flux of substrates was utilized to control the amount of 3-hydroxyvalerate and 3-hydroxy-4-pentenoate produced by Burkohlderia sp. The 3HV production rate was directly proportional to the propionic acid uptake rate with the last one completely directed to 3HV biosynthesis. The 3HPE production rate was inversely proportional to the sucrose uptake rate probably due to operation of the glyoxylate cycle.

Influência do sulfato de condroitina na formação de filmes isolados de polimetacrilato: avaliação do índice de intumescimento e permeabilidade ao vapor d'água

Natural or modified chondroitin sulfate was incorporated in to polymethacrylate to obtain isolated films. The addition of polysaccharide to synthetic polymers occurred at different rates. Isolated films were micro and macroscopically characterized and swelling index and water vapor transmission were determined. Results indicated changed transparency and flexibility, coupled to their dependence on increase in polysaccharide concentration. A similar occurrence was reported in the permeability to water vapor and swelling degree. Films composed of modified chondroitin sulfate, 90:10 concentration, showed hydration levels, permeability and morphological properties which allow them to be applied as excipients in the development of new drug delivery systems.

Adsorção de íons cobre(II) pela quitosana usando coluna em sistema sob fluxo hidrodinâmico

The adsorption of Cu(II) ions from aqueous solution by chitosan using a column in a closed hydrodynamic flow system is described. The adsorption capacities as a function of contact time of copper(II) ions and chitosan were determined by varying the ionic strength, temperature and the flow of the metal solution. The Langmuir model reproduced the adsorption isothermal data better than the Freundlich model. The experimental kinetic data correlate properly with the second-order kinetic reaction for the whole set of experimental adsorption conditions. The rate constants exercise great influence on the time taken for equilibrium to be established by complexation or electrostatic interaction between the amino groups of chitosan and the metal.

Contenido de flavonoides y compuestos fenólicos de mieles chilenas e índice antioxidante

A comparison of the phenolic content of several Chilean honeys showed great variations in flavonoid concentration among the samples analysed. Higher amounts of phenolics are found in honey from dry climates. The antioxidant effect of extracts, using ORAC analysis, did not correlate with the flavonoid content or with the total phenolic concentration.