Quantification of N-acetylcysteine in pharmaceuticals using cobalt phthalocyanine modified graphite electrodes

Flow injection analysis (FIA) with amperometric detection was employed for the quantification of N-acetylcysteine (NAC) in pharmaceutical formulations, utilizing an ordinary pyrolytic graphite (OPG) electrode modified with cobalt phthalocyanine (CoPc). Cyclic voltammetry was used in preliminary studies to establish the best conditions for NAC analysis. In FIA-amperometric experiments the OPG-CoPc electrode exhibited sharp and reproducible current peaks over a wide linear working range (5.0 x 10(-5)-1.0 x 10(-3) mol L(-1)) in 0.1 mol L(-1) NaOH solution. High sensitivity (130 mA mol(-1) cm(2)) and a low detection limit (9.0 x 10(-7) mol L(-1)) were achieved using the sensor. The repeatability (R.S.D.%) for 13 successive flow injections of a solution containing 5.0 x 10(-4) mol L(-1) NAC was 1.1%. The new procedure was applied in analyses of commercial pharmaceutical products and the results were in excellent agreement with those obtained using the official titrimetric method. The proposed amperometric method is highly suitable for quality control analyses of NAC in pharmaceuticals since it is rapid, precise and requires much less work than the recommended titrimetric method. (C) 2010 Elsevier B.V. All rights reserved.

Dynamic Solid Phase DNA Extraction and PCR Amplification in Polyester-Toner Based Microchip

A variety of substrates have been used for fabrication of microchips for DNA extraction, PCR amplification, and DNA fragment separation, including the more conventional glass and silicon as well as alternative polymer-based materials. Polyester represents one such polymer, and the laser-printing of toner onto polyester films has been shown to be effective for generating polyester-toner (PeT) microfluidic devices with channel depths on the order of tens of micrometers. Here, we describe a novel and simple process that allows for the production of multilayer, high aspect-ratio PeT microdevices with substantially larger channel depths. This innovative process utilizes a CO(2) laser to create the microchannel in polyester sheets containing a uniform layer of printed toner, and multilayer devices can easily be constructed by sandwiching the channel layer between uncoated cover sheets of polyester containing precut access holes. The process allows the fabrication of deep channels, with similar to 270 mu m, and we demonstrate the effectiveness of multilayer PeT microchips for dynamic solid phase extraction (dSPE) and PCR amplification. With the former, we found that (i) more than 65% of DNA from 0.6 mu L of blood was recovered, (ii) the resultant DNA was concentrated to greater than 3 ng/mu L., (which was better than other chip-based extraction methods), and (iii) the DNA recovered was compatible with downstream microchip-based PCR amplification. Illustrative of the compatibility of PeT microchips with the PCR process, the successful amplification of a 520 bp fragment of lambda-phage DNA in a conventional thermocycler is shown. The ability to handle the diverse chemistries associated with DNA purification and extraction is a testimony to the potential utility of PeT microchips beyond separations and presents a promising new disposable platform for genetic analysis that is low cost and easy to fabricate.

Electrochemical sensor for sulfite determination based on a nanostructured copper-salen film modified electrode

The electrochemical preparation described herein involved the electrocatalytic oxidation of sulfite on a platinum electrode modified with nanostructured copper salen (salen=N,N'-ethylenebis(salicylideneiminato)) polymer films. The complex was prepared and electropolymerized at a platinum electrode in a 0.1 mol L-1 solution of tetrabutylammonium perchlorate in acetonitrile by cyclic voltammetry between 0 and 1.4V vs. SCE. After cycling the modified electrode in a 0.50 mol L-1 KCI solution, the estimated surface concentration was found to be equal to 2.2 x 10(-9) Mol cm(-2). This is a typical behavior of an electrode surface immobilized with a redox couple that can usually be considered as a reversible single-electron reduction/oxidation of the copper(II)/copper(III) couple. The potential peaks of the modified electrode in the electrolyte solution (aqueous) containing the different anions increase with the decrease of the ionic radius, demonstrating that the counter-ions influence the voltammetric behavior of the sensor. The potential peak was found to be linearly dependent upon the ratio [ionic charge]/[ionic radius]. The oxidation of the sulfite anion was performed at the platinum electrode at +0.9V vs. SCE. However, a significant decrease in the overpotential (+0.45V) was obtained while using the sensor, which minimized the effect of oxidizable interferences. A plot of the anodic current vs. the sulfite concentration for chronoamperometry (potential fixed = +0.45V) at the sensor was linear in the 4.0 x 10(-6) to 6.9 x 10(-5) mol L-1 concentration range and the concentration limit was 1.2 x 10(-6) mol L-1. The reaction order with respect to sulfite was determined by the slope of the logarithm of the current vs. the logarithm of the sulfite concentration. (C) 2009 Elsevier Ltd. All rights reserved.

An electrochemical sensor for dipyrone determination based on nickel-salen film modified electrode

An amperometric dipyrone sensor based on a polymeric nickel-salen (salen = N,N'-ethylenebis(salicydeneiminato)) film coated platinum electrode was developed. The sensor was constructed by electropolymerization of nickel-salen complex at a platinum electrode in acetonitrile/tetrabuthylamonium perchlorate by cyclic voltammetry. After cycling the modified electrode in a 0.50 mol L-1 KCl solution, the estimated surface concentration was found to be equal to 1.29 x 10(-9) mol cm(-2). This is a typical behavior of an electrode surface immobilized with a redox couple that can usually be considered as a reversible single-electron reduction/oxidation of the nickel(II)/nickel(III) couple. A plot of the anodic current versus the dipyrone concentration for chronoamperometry (potential fixed = +0.50 V) at the sensor was linear in the 4.7 x 10(-6) to 1.1 x 10(-4) mol L-1 concentration range and the concentration limit was 1.2 x 10(-6) mol L-1. The proposed electrode is useful for the quality control and routine analysis of dipyrone in pharmaceutical formulations.

Development of biosensors based on hexacyanoferrates

Ferric and copper hexacyanoferrates (PB and CuHCF, respectively) were electrodeposited on glassy carbon electrodes providing a suitable catalytic surface for the amperometric detection of hydrogen peroxide. Additionally glucose oxidase was immobilized on top of these electrodes to form glucose biosensors. The biosensors were made by casting glucose oxidase-Nafion layers onto the surface of the modified electrodes. The operational stability of the films and the biosensors were evaluated by injecting a standard solution (5 mu M H2O2 for PB, 5 mM H2O2 for CuHCF and 1.5 mM glucose for both) over 5-10 h in a now-injection system with the electrodes polarized at - 50 (PB) and -200 mV (CuHCF) versus Ag/AgCl, respectively. The glucose biosensors demonstrated suitability for glucose determination: 0.0-2.5 mM (R-2 = 0.9977) for PB and 0.0-10 mM (R-2 = 0.9927) for CuHCF, respectively. The visualization of the redox catalyst modifiers (PB and CuHCF films) was presented by scanning electron micrographs. (C) 2000 Elsevier B.V. B.V. All rights reserved.

Flow-through cell based on an array of gold microelectrodes obtained from modified integrated circuit chips

The construction of a flow-through cell incorporating an array of gold microelectrodes is described and its application to flow injection analysis with amperometric detection is presented, Simple modification of almost any conventional integrated circuit chip, used as an inexpensive source of pre-assembled gold micro-wires, leads to the rapid and successful preparation of arrays of 8-48 elements, the polymeric encapsulation material from the top face of the chip is removed by abrasion until the gold micro-mires (used to interconnect the silicon circuit to the external contact pins of the chip) are disrupted and their transversal (elliptical) sections become exposed. Once polished, the flat and smooth top surface of the gold microelectrode-array chip (MEAC) is provided with a spacer and fitted under pressure against an acrylic block with the reference and auxiliary electrodes, to form the electrochemical (thin-layer) flow cell, while the contact pins are plugged into a standard IC socket, This design ensures autonomous electric contact with each electrode and allows fast dismantling for polishing or substitution, the performance of flow cells with MEACs was investigated utilizing the technique of reverse pulse amperometry without oxygen removal, A method was established for the determination of the copper concentration in sugar cane spirit, regulated by law for beverages, Samples from industrial producers and small-scale (alembic) brewers were compared, With a 24 MEAC, a detection limit of 30 mu g I-l of copper (4.7 x 10(-7) mol l(-1) of Cu-II for 100 mu l injections) was calculated, Routine operation was established at a frequency of 60-90 determinations per hour, Intercomparison with atomic absorption spectrometric determinations resulted in excellent agreement.

Escurecimento enzimático em frutos: polifenoloxidase de atemóia (Annona cherimola Mill. X Annona squamosa L.)

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Estudo de filmes poliméricos de complexos a base de tiofeno8Schiff na construção de sensores eletroquímicos

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

Detecção eletroquímica de furfural e hidroximetilfurfural em bagaço de cana-de-açúcar utilizando cromatografia líquida de alta eficiência

Pós-graduação em Química - IQ

Detecção eletroquímica de ácidos urônicos presentes no bagaço de cana-de-açúcar utilizando eletrodo modificado com nanopartículas de cobre em técnica de HPLC

Pós-graduação em Química - IQ

Glucose biosensor based on multisegment nanowires exhibiting reversible magnetic control

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

Preparação e Modificação Química de Nanoestruturas de Octa(aminopropil) silsesquioxano para Aplicações Analíticas

Pós-graduação em Ciência dos Materiais - FEIS

Determination of uronic acids in sugarcane bagasse by anion-exchange chromatography using an electrode modified with copper nanoparticles

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

Desenvolvimento de detector eletroquímico para cromatografia líquida de alta eficiência baseado em um eletrodo modificado com nanopartículas metálicas para determinação de ácidos carboxílicos em vinhaça de cana-de-açúcar

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

Determination of Tetracycline in Environmental Water Samples at a Graphite-Polyurethane Composite Electrode

A bare graphite-polyurethane composite was evaluated in the tetracycline (TC) determination in natural water samples. Using differential pulse voltammetry (DPV), a linear response was observed in the range of 4.00-40.0 mu mol L-1 with limit of detection of 2.80 mu mol L-1, without the need of surface renewing between successive runs. During the tetracycline determination in water samples, recoveries between 92.6 and 100% were found. The results for TC determination in water samples after a pre-concentration stage agreed with spiked value at a 95% confidence level according to student t-test.