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Comparative study of sample preparation procedures to determine fipronil in pollen by gas chromatography with mass spectrometric and electron-capture detection.

Jiménez JJ, Bernal JL, del Nozal MJ, Martín MT, Mayo R

Department of Analytical Chemistry, Faculty of Sciences, University of Valladolid, Prado de la Magdalena s/n, 47005 Valladolid, Spain. jjimenez@qa.uva.es

Several sample preparation methods have been assayed to analyze residues of fipronil in pollen at trace concentrations. Extraction with organic solvents, solid-phase extraction on either commercial cartridges or a Florisil-packed column and a matrix solid-phase dispersion, also with Florisil as a dispersing agent, have been tested. Determination of fipronil in the extracts has been carried out by GC with electron-capture and mass spectrometric detection. An extraction with acetonitrile followed by a clean-up on ODS or polymeric cartridges was the most suitable procedure to obtain acceptable recoveries and relatively simple chromatograms. The matrix-effects observed in the quantification can be corrected with a matrix-matched calibration.

Published 12 March 2007 in J Chromatogr A, 1146(1): 8-16.
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