Molecularly imprinted polymer solid-phase extraction coupled to square wave voltammetry at carbon fibre microelectrodes for the determination of fenbendazole in beef liver |
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Authors: | A Guzmán-Vázquez de Prada Oscar A Loaiza B Serra D Morales P Martínez-Ruiz A J Reviejo J M Pingarrón |
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Institution: | (1) Department of Analytical Chemistry, Faculty of Chemistry, Complutense University of Madrid, 28040 Madrid, Spain;(2) Department of Organic Chemistry, Faculty of Chemistry, Complutense University of Madrid, 28040 Madrid, Spain |
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Abstract: | A molecularly imprinted polymer was developed and used for solid-phase extraction (MISPE) of the antihelmintic fenbendazole
in beef liver samples. Detection of the analyte was accomplished using square wave voltammetry (SWV) at a cylindrical carbon
fibre microelectrode (CFME). A mixture of MeOH/HAc (9:1) was employed both as eluent in the MISPE system and as working medium
for electrochemical detection of fenbendazole. The limit of detection was 1.9 × 10−7 mol L−1 (57 μg L−1), which was appropriate for the determination of fenbendazole at the maximum residue level permitted by the European Commission
(500 μg kg−1 in liver). Given that the SW voltammetric analysis could not be directly performed in the sample extract as a consequence
of interference from some sample components, a sample clean-up with a MIP for selectively retaining fenbendazole was performed.
The MIP was synthesized using a 1:8:22 template/methacrylic acid/ethylene glycol dimethacrylate ratio. A Britton–Robinson
Buffer of pH 9.0 was selected for retaining fenbendazole in the MIP cartridges, and an eluent volume of 5.0 mL at a flow rate
of 2.0 mL min−1 was chosen in the elution step. Cross-reactivity with the MIP was observed for other benzimidazoles. The synthesized MIP
exhibited a good selectivity for benzimidazoles with respect to other veterinary drugs. The applicability of the MISPE-SWV
method was tested with beef liver samples, spiked with fenbendazole at 5,000 and 500 μg kg−1. Results obtained for ten different liver samples yielded mean recoveries of (95 ± 12)% and (96 ± 11)% for the upper and
lower concentration level, respectively. |
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Keywords: | Benzimidazoles Fenbendazole Molecularly imprinted polymer Square wave voltammetry Beef liver |
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