This study was devoted to the characterization and use of two types of laboratory-made miniaturized amperometric detectors. First, an amperometric microcylindrical detector (μCD) for HPLC is described. It is based on a microwire working electrode placed across the flow of mobile phase in Teflon tubing connected directly to the column outlet. The Pt-μCD was employed for the detection of selected hydroxy and amino derivatives of naphthalene. The repeatability of the detector response is satisfactory (< 1 %) in the concentration range 2·10 -7 - 6·10 -5 mol L -1 and detection limits achieved were 7.8·10 -8 mol L -1, 1.1·10 -7 mol L -1, 2.5·10 -7 mol L -1 and 2,8·10 -7 mol L -1 for 1-naph-thylamine, 2-naphthylamine, 1-naphthol, and 2-naphthol, respectively. The Cu-μCD was used as a selective detector for the HPLC analysis of selected amino acids, based on their complexation reaction with Cu 2+ from Cu microwire electrode. Due to a different electron transfer principle, the detector shows a higher background current and noise than Pt-μCD; nevertheless, it enables the detection of amino acids with limits of detection in the range 1.4·10 -6 mol L -1 (histidine) to 1.2·10 -5 mol L -1 (tryptophan). Second, an amperometric detector with boron-doped diamond micro electrode connected to capillary zone electrophoresis was employed for the detection of 2-naphthylamine, 1-naphthol and 2-naphthol in column. The microelectrode was fabricated by coating electrochemically sharpened platinum wires with thin films of polycrystalline boron-doped diamond. The calculated electrode areas were (1.5-4.5)·10 -2 mm 2. The diamond microelectrodes exhibited good electroanalytical performance with a low peak-to-peak noise ∼1 pA, low and stable background current and repeatable responses for studied analytes. Limits of detection for 1-and 2-naphthol were established as 9.5·10 -8 mol L -1 and 9.0·10 -8 mol L -1, respectively. Stable response of all the working electrodes described and their small dimensions are promising for their possible use in micro-HPLC or capillary electrophoresis in microchip format.
|Translated title of the contribution||Miniaturized amperometric detectors for HPLC and capillary zone electrophoresis|
|Number of pages||9|
|Publication status||Published - 1 Feb 2006|
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