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Cyclodextrin modified gold nanoparticles-based open-tubular capillary electrochromatographic separations of polyaromatic hydrocarbons

Řezanka, Pavel and Navrátilová, Klára and Žvátora, Pavel and Sýkora, David and Matějka, Pavel and Mikšík, Ivan and Václav, Kašička and Krá, Vladimír (2011) Cyclodextrin modified gold nanoparticles-based open-tubular capillary electrochromatographic separations of polyaromatic hydrocarbons. Journal of Nanoparticle Research, 13 (11). pp. 5947-5957.

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In this study, spherical gold nanoparticles (GNPs) of 14.7 nm diameter, prepared by citrate reduction of a gold(III) salt and characterized by UV–Vis absorption spectrometry and transmission electron microscopy, were modified by a covalent attachment of 6I-O-(3-mercaptopropyl)β-cyclodextrin (β-CD-SH) or per-6-deoxy-per-6-mercapto-β-cyclodextrin (β-CD-SH7). Subsequently, via three alternative approaches, β-CD-modified GNPs were immobilized onto the inner wall of the fused-silica (FS) capillaries and applied as special stationary phases for open-tubular capillary electrochromatography (OT-CEC). The first immobilization procedure was based on pre-derivatization of a FS capillary with (3-mercaptopropyl)trimethoxysilane (MPTMS) followed by subsequent reactions with GNPs and β-CD-SH or β-CD-SH7. The other two preparation protocols took advantage of sol–gel approach gaining a significant increase in the interaction surface for solutes. In both instances, the sol–gel created 3D structure was further covalently modified with GNPs. Serving that purpose, either β-CD-SH7 modified GNPs were used for the immobilization into the sol–gel matrix ( one-step sol–gel technique ) or native GNPs were immobilized first into the sol–gel matrix and subsequently modified with β-CD-SH7 ( two-step sol–gel technique ). The separation performance of CD-GNPs modified FS capillaries was tested by OT-CEC in reversed-phase mode applied to separation of a model mixture of five polyaromatic hydrocarbons. The highest separation efficiencies were obtained with the capillaries prepared by two-step sol–gel technique. However, with respect to the relatively low reproducibility of this method, the first of the above preparation procedures, i.e., a simple pre-derivatization of the FS capillary with MPTMS ensued with β-CD-SH7-GNPs immobilization seems to be more feasible approach providing decent separation efficiency.

Item Type:Article
ID Code:11513
Deposited By:Prof. Alexey Ivanov
Deposited On:05 Jan 2012 09:30
Last Modified:05 Jan 2012 09:42

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