Miniaturizované ampérometrické detektory pro HPLC a kapilární zónovou elektroforézu

Translated title of the contribution: Miniaturized amperometric detectors for HPLC and capillary zone electrophoresis

Karolina Pecková, Veronika Mocko, Frantlšek Opekar, Greg M. Swain, Jiří Zima, Jiří Barek

Research output: Contribution to journalReview article

27 Citations (Scopus)

Abstract

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.

Original languageCzech
Pages (from-to)124-132
Number of pages9
JournalChemicke Listy
Volume100
Issue number2
Publication statusPublished - 1 Feb 2006
Externally publishedYes

Fingerprint

Electrophoresis
Detectors
Diamond
Electrodes
2-Naphthylamine
Boron
Microelectrodes
Amino Acids
Capillary electrophoresis
Polytetrafluoroethylene
Tubing
Platinum
Complexation
Histidine
Tryptophan
Wire
Derivatives
Thin films
Coatings
Electrons

ASJC Scopus subject areas

  • Chemistry(all)

Cite this

Pecková, K., Mocko, V., Opekar, F., Swain, G. M., Zima, J., & Barek, J. (2006). Miniaturizované ampérometrické detektory pro HPLC a kapilární zónovou elektroforézu. Chemicke Listy, 100(2), 124-132.

Miniaturizované ampérometrické detektory pro HPLC a kapilární zónovou elektroforézu. / Pecková, Karolina; Mocko, Veronika; Opekar, Frantlšek; Swain, Greg M.; Zima, Jiří; Barek, Jiří.

In: Chemicke Listy, Vol. 100, No. 2, 01.02.2006, p. 124-132.

Research output: Contribution to journalReview article

Pecková, K, Mocko, V, Opekar, F, Swain, GM, Zima, J & Barek, J 2006, 'Miniaturizované ampérometrické detektory pro HPLC a kapilární zónovou elektroforézu', Chemicke Listy, vol. 100, no. 2, pp. 124-132.
Pecková K, Mocko V, Opekar F, Swain GM, Zima J, Barek J. Miniaturizované ampérometrické detektory pro HPLC a kapilární zónovou elektroforézu. Chemicke Listy. 2006 Feb 1;100(2):124-132.
Pecková, Karolina ; Mocko, Veronika ; Opekar, Frantlšek ; Swain, Greg M. ; Zima, Jiří ; Barek, Jiří. / Miniaturizované ampérometrické detektory pro HPLC a kapilární zónovou elektroforézu. In: Chemicke Listy. 2006 ; Vol. 100, No. 2. pp. 124-132.
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AU - Pecková, Karolina

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AU - Swain, Greg M.

AU - Zima, Jiří

AU - Barek, Jiří

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N2 - 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.

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