Direct detection of underivatized chitooligosaccharides produced through chitinase action using capillary zone electrophoresis

Capillary electrophoresis with capacitively coupled contactless conductivity detection was successfully used to quantify N-acetylglucosamine and five N-acetyl-chitooligosaccharides (C2-C6) produced after reaction with a purified chitinase (TmChi) from Tenebrio molitor (Coleoptera). No derivatization process was necessary. The separation was developed using 10 mM NaOH with 10% (v/v) acetonitrile as background electrolyte and homemade equipment with a system that avoids the harmful effect of electrolysis. The limit of detection for all oligosaccharides was ca. 3 mu M, and the results indicated that the larger the oligosaccharide, the higher the sensitivity. Analysis of the chitooligosaccharides produced revealed that TmChi has an endolytic cleavage pattern with C5 as the best substrate (higher catalytic efficiency k(cat)/K-M) releasing C2 and C3. (c) 2007 Elsevier Inc. All rights reserved.

A simple and sensitive detection of diquat herbicide using a dental amalgam electrode A comparison using the chromatographic technique

This paper describes the use of a dental amalgam electrode (DAE) to evaluate the electrochemical behaviour and to develop an electroanalytical procedure for determination of diquat herbicide in natural water and potato samples. The work was based on the square wave voltammetry responses of diquat, which presented two well-defined and reversible reduction peaks, at -0.56 V (peak 1) and -1.00V (peak 2). The experimental and voltammetric parameters were optimised, and the analytical curves were constructed and compared to similar curves performed by high performance liquid chromatography coupled to ultraviolet-visible spectrophotometric detector (HPLC/UV-vis). The responses were directly proportional to diquat concentration in a large interval of concentration, and the calculated detection limits were very similar, around 10 mu g L(-1) (10 ppb) for voltammetric and chromatographic experiments. These values were lower than the maximum residue limit established for natural water by the Brazilian Environmental Agency. The recovery percentages in pure electrolyte, natural water and potato samples showed values from 70% to 130%, demonstrating that the voltammetric methodology proposed is suitable for determining any contamination by diquat in different samples, minimising the toxic residues due to the use of liquid mercury or the adsorptive process relative to use of other solid surfaces. (C) 2009 Published by Elsevier B.V.

Development and Application of a Highly Selective Biomimetic Sensor for Detection of Captopril, an Important Ally in Hypertension Control

A biomimetic sensor is proposed as a promising new analytical method for determination of captopril in different classes of samples. The sensor was prepared by modifying a carbon paste electrode with iron (II) phthalocyanine bis(pyridine) [FePe(dipy)] complex. Amperometric measurements in a batch analytical mode were first carried out in order to optimize the sensor response. An applied potential lower than 0.2 V vs Ag vertical bar AgCl in 0.1 mol L(-1) of TRIS buffer at pH 8.0 provided the best response, with a linear range of 2.5 x 10(-5) to 1.7 x 10(-4) mol L(-1). A detailed investigation of the selectivity of the sensor, employing seventeen other drugs, was also performed. Recovery studies were carried out using biological and environment samples in order to evaluate the sensor`s potential for use with these sample classes. Finally, the performance of the biomimetic sensor was optimized in a flow injection (FIA) system using a wall jet electrochemical cell. Under optimized flow conditions, a broad linear response range, from 5.0 x 10(-4) to 2.5 x 10(-2) mol L(-1), was obtained for captopril, with a sensitivity of 210 +/- 1 mu A L mol(-1).