Renato Camargo Matos

Flow injection analysis-amperometric determination of ascorbic and uric acids in urine using arrays of gold microelectrodes modified by electrodeposition of palladium.

Abstract Uric acid (UA) and ascorbic acid (AA) present in urine were rapidly determined by the amperometric method in association with flow injection analysis. An array of gold microelectrodes modified by electrochemical deposition of palladium was employed as the working electrode. Uric and ascorbic acids were quantified in urine using amperometric differential measurements at +0.75 and +0.55xa0V, respectively. This method is based on three steps involving the flow injection of: (1) the sample spiked with a standard solution, (2) the pure sample, and (3) the enzymatically treated sample. The enzymatic treatment was carried out with ascorbate oxidase, uricase, and peroxidase at pH 7. The calibration curves for freshly prepared ascorbic and uric acid standards were very linear in the concentration ranges of 0.44–2.64xa0mgxa0l −1 (AA) and of 0.34–1.68xa0mgxa0l −1 (UA) with a relative standard deviation (RSD) n xa0=xa09).

Modified microelectrodes and multivariate calibration for flow injection amperometric simultaneous determination of ascorbic acid, dopamine, epinephrine and dipyrone.

Flow injection amperometric quantification of ascorbic acid (AA), dopamine (DA), epinephrine (EP) and dipyrone (DI) in mixtures (in the microgram g-1 range) was successfully performed by using an array of microelectrodes with units modified by the electrodeposition of different noble metals, together with multivariate calibration analysis. The four groups of microelectrodes utilized included a pure gold electrode and electrodes modified by electrodeposition of platinum, palladium or a mixture of platinum + palladium. The array of microelectrodes was inserted in a flow cell and the amperometric data acquisition was performed with a four-channel potentiostat. The analysis of the resulting signals was carried out by a multivariate calibration method, using a group of 16 standard mixtures selected by a two-level factorial design. The analysis of synthetic samples and pharmaceutical compounds containing AA and DI led to very similar values to those obtained by the classical iodimetric analysis. The average absolute errors (in microgram g-1) calculated for each analyte were 0.3, 0.2, 0.4 and 0.4 for AA, DA, EP and DI, respectively.

Flow-injection system with enzyme reactor for differential amperometric determination of hydrogen peroxide in rainwater

Abstract Differential determinations of hydrogen peroxide (H2O2) have been performed by amperometry, combining flow-injection analysis (FIA) and a tubular reactor containing immobilized enzymes. A gold microelectrode modified by electrochemical deposition of platinum was employed as working electrode. Hydrogen peroxide was quantified in rainwater using amperometric differential measurements at +0.60xa0V versus Ag/AgCl(sat). For the enzymatic consumption of H2O2, a tubular reactor containing immobilized catalase was constructed, using a novel way for immobilization of enzymes on Amberlite IRA-743 resin. The linear dynamic range in H2O2 extends from 1 to 100×10−6xa0mol/l, at pH 7.0. At flow rate of 2.0xa0ml/min and injecting 150xa0μl sample volumes, the sampling frequency of the 90 determinations/h is afforded. The reproducibility of the current peaks for hydrogen peroxide in 10−5xa0mol/l range concentration shown a R.S.D. better than 1%. The detection limit of the method is 2.9×10−7xa0mol/l (1.5xa0ng of H2O2 in a 150xa0μl sample). The rainwater samples analyses were compared with the parallel amperometric determinations using static mercury electrode and by spectrophotometry, showing very good correlation between the three methods.

Gold electrodes from compact discs modified with platinum for amperometric determination of ascorbic acid in pharmaceutical formulations

A simple, rapid and precise amperometric method has been developed for quantification of ascorbic acid (AA) in pharmaceutical formulations using flow-injection analysis (FIA). A slice of recordable compact disc (CD) modified by electrodeposition of platinum was employed as the working electrode. The proposed flow system allows determinations in the 1 mumol l(-1) of the analyte and enables 90 determinations per h, employing only 150-mul sample. The method permits the direct quantification of ascorbic acid in many pharmaceutical products, avoiding cumbersome processes as previous separations, solvent extraction or sample filtration. This new procedure was applied to commercial pharmaceutical tablets and the results obtained were identical than the ones obtained by the classical iodometric method. The calibration plots for freshly prepared ascorbic acid standards were highly linear in the concentration range of 1-10 mumol l(-1) with a relative standard deviation (R.S.D.) <1%. For all real samples studied, the deviations were situated between 0.5 and 8.7%.

Amperometric differential determination of ascorbic acid in beverages and vitamin C tablets using a flow cell containing an array of gold microelectrodes modified with palladium

A simple and attractive method for quantification of ascorbic acid (AA) in beers, soda, natural juices and commercial vitamin C tablets was achieved by combining flow injection analysis and amperometric detection. An array of gold microelectrodes electrochemically modified by deposition of palladium was employed as working electrode which was almost unaffected by fouling effects. Ascorbic acid was quantified in beverages and vitamin tablets using amperometric differential measurements. This method is based on three steps involving the flow injection of: (1) the sample plus a standard addition of AA, (2) the pure sample, and (3) the enzymatically-treated sample. The enzymatic treatment was carried out with Cucumis sativus tissue, which is a rich source of ascorbate oxidase, at pH 7. The calibration plots for freshly prepared ascorbic acid standards were very linear in the concentration range of 0.18–1.8 mg L−1 with a relative standard deviation (RSD) < 1%, while for real samples the deviations were between 2.7 % to 8.9 %.

Propulsor pneumático versátil e isento de pulsação para sistemas de análise em fluxo

Aquarium air pumps are proposed and evaluated as pneumatic liquid propulsion devices for flow injection and continuos flow analysis (FIA and CFA) systems. This kind of pump is widely available at a very low cost and it can sustain a pressure around of 4 psi (0.28 bar) indefinitely. By applying this air pressure onto a solution contained in a reservoir flask, it is possible to reach flow rates of up to 12.5 mLxa0min-1 for circuits comprising reactors, made from 0.8 i.d. tubing with a length of 100 cm. The precise adjustment of flow rate below the maximum one can be made with a simplified needle valve or inserting in series a short length of capillary tube. The absence of flow pulsation is a definite advantage in comparison with peristaltic pumps, especially when amperometric detection is elected, as confirmed experimentally in FIA and CF applications.

Development of a Four-Channel Potentiostat for Amperometric Detection in Flow Injection Analysis

Abstract A four-channel multipotentiostat has been developed for simultaneous voltammetric measurements with microelectrode arrays. To reduce the complexity of electrochemical cell, only one reference and one auxiliary electrode are used. The potential ranges of the four working electrodes may be independently controlled, but they are synchronously scanned by only one DAC. This is accomplished through a microcomputer interfaced with a PCL-711B data acquisition board, which allows the continuous monitoring of the currents and actual potentials of the working electrodes. The system has been applied to the simultaneous determination of ascorbic and uric acids in synthetic samples. The measurements were carried out with gold microelectrodes modified by deposition of noble metals, which enhance the electrocatalysis and provide an anticipation and a better definition of the oxidation potentials. Recuperation of 98.2% and 97.8% for ascorbic and uric acids, respectively, was obtained by using amperometry.