Journal
JOURNAL OF CHROMATOGRAPHY A
Volume 1146, Issue 1, Pages 8-16Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2007.01.117
Keywords
gas chromatography; matrix-effect; fipronil; pollen
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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. (c) 2007 Elsevier B.V. All rights reserved.
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