A rapid and reliable bonding process for microchip electrophoresis fabricated in glass substrates.

In this report, we describe a rapid and reliable process to bond channels fabricated in glass substrates. Glass channels were fabricated by photolithography and wet chemical etching. The resulting channels were bonded against another glass plate containing a 50-microm thick PDMS layer. This same PDMS layer was also used to provide the electrical insulation of planar electrodes to carry out capacitively coupled contactless conductivity detection. The analytical performance of the proposed device was shown by using both LIF and capacitively coupled contactless conductivity detection systems. Efficiency around 47,000 plates/m was achieved with good chip-to-chip repeatability and satisfactory long-term stability of EOF. The RSD for the EOF measured in three different devices was ca. 7%. For a chip-to-chip comparison, the RSD values for migration time, electrophoretic current and peak area were below 10%. With the proposed approach, a single chip can be fabricated in less than 30 min including patterning, etching and sealing steps. This fabrication process is faster and easier than the thermal bonding process. Besides, the proposed method does not require high temperatures and provides excellent day-to-day and device-to-device repeatability.

Simultaneous voltammetric determination of paracetamol and caffeine in pharmaceutical formulations using a boron-doped diamond electrode.

A simple and highly selective electrochemical method was developed for the single or simultaneous determination of paracetamol (N-acetyl-p-aminophenol, acetaminophen) and caffeine (3,7-dihydro-1,3,7-trimethyl-1H-purine-2,6-dione) in aqueous media (acetate buffer, pH 4.5) on a boron-doped diamond (BDD) electrode using square wave voltammetry (SWV) or differential pulse voltammetry (DPV). Using DPV with the cathodically pre-treated BDD electrode, a separation of about 550 mV between the peak oxidation potentials of paracetamol and caffeine present in binary mixtures was obtained. The calibration curves for the simultaneous determination of paracetamol and caffeine showed an excellent linear response, ranging from 5.0 x 10(-7)mol L(-1) to 8.3 x 10(-5)mol L(-1) for both compounds. The detection limits for the simultaneous determination of paracetamol and caffeine were 4.9 x 10(-7)mol L(-1) and 3.5 x 10(-8)mol L(-1), respectively. The proposed method was successfully applied in the simultaneous determination of paracetamol and caffeine in several pharmaceutical formulations (tablets), with results similar to those obtained using a high-performance liquid chromatography method (at 95% confidence level).

Polyurethane from biosource as a new material for fabrication of microfluidic devices by rapid prototyping.

This paper presents the use of elastomeric polyurethane (PU), derived from castor oil (CO) biosource, as a new material for fabrication of microfluidic devices by rapid prototyping. Including the irreversible sealing step, PU microchips were fabricated in less than 1h by casting PU resin directly on the positive high-relief molds fabricated by standard photolithography and nickel electrodeposition. Physical characterization of microchannels was performed by scanning electron microscopy (SEM) and profilometry. Polymer surface was characterized using contact angle measurements and the results showed that the hydrophilicity of the PU surface increases after oxygen plasma treatment. The polymer surface demonstrated the capability of generating an electroosmotic flow (EOF) of 2.6 x 10(-4)cm(2)V(-1)s(-1) at pH 7 in the cathode direction, which was characterized by current monitoring method at different pH values. The compatibility of PU with a wide range of solvents and electrolytes was tested by determining its degree of swelling over a 24h period of contact. The performance of microfluidic systems fabricated using this new material was evaluated by fabricating miniaturized capillary electrophoresis systems. Epinephrine and l-DOPA, as model analytes, were separated in aqueous solutions and detected with end-channel amperometric detection.

Determination of dipyridamole in pharmaceutical preparations using square wave voltammetry.

An analytical methodology using square wave voltammetry (SWV) at a hanging mercury drop electrode (HMDE) was developed for the quantitative determination of dipyridamole (DIP), a drug used for the treatment of several cardiovascular diseases, in pharmaceutical tablets and injections of Persantin in phosphate buffer (pH 3.0; 0.1M). After optimization of the parameters for SWV, analytical curves were obtained for application in the range of 1.28 x 10(-6)M to 7.02 x 10(-6)M. It was found a detection limit (DL) of 1.88 x 10(-8)M (9.50 ng/ml). The repeatability and the reproducibility of the method were determinated by successive measurements of DIP solutions on the range of the analytical curve with a coefficient variation of 0.97% (n=5) and 1.15%, respectively. The apparent recoveries were obtained by the IUPAC recommended procedure using the second reduction peak. Recoveries obtained by SWV were compared with the UV-vis spectrophotometric method. It was found that the determination of DIP in Persantin tablets gave a mean value of 75.6+/-0.4 mg (100.8%) and 68.9+/-0.3 mg (91.8%) for SWV and UV-vis spectrophotometry, respectively. In the case of injections, it was found 10.4+/-0.1 mg (103.4%) and 9.9+/-0.2 mg (99.9%) for SWV and UV-vis spectrophotometry. Both apparent recoveries for the two types of formulations are in good accordance with the declared value of 75 mg (tablets) and 10 mg (injections).

Determinaçäo de pesticidas por técnicas eletroanalíticas / Pesticides determination by electroanalytical techniques

Apresenta revisao sobre a aplicaçao de técnicas eletroanalíticas na análise e determinaçao de pesticidas em vários meios, como águas naturais, frutas, cereais e solos, entre outros. O baixo custo das análises, a facilidade de manipulaçao das amostras, o curto tempo de realizaçao das medidas e a sensibilidade a interferentes sao as principais vantagens desta aplicaçao. As técnicas eletroanalíticas mais utilizadas sao a polarografia de corrente direta (DC), a polarografia de pulso diferencial e a voltametria adsortiva, em cerca de 60 ingredientes ativos de pesticidas das mais diferentes classes, ou seja, triazinas, organoclorados, organofosforados, carbamatos, compostos nitros e outros.