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Updated: Jul 7, 2026

Extraction and Analysis of Microbial Phospholipid Fatty Acids in Soils
Published on: August 26, 2016
Sample preparation methods to analyze fipronil in honey by gas chromatography with electron-capture and mass
J J Jiménez1, J L Bernal, Maria J del Nozal
1IU CINQUIMA, Department of Analytical Chemistry, University of Valladolid, Prado de la Magdalena s/n, E-47005 Valladolid, Spain. jjiminez@qua.uva.es
Abstract:
Several sample preparation methods have been assayed to analyze residues of fipronil in honey. After diluting the honey, liquid-liquid extraction (LLE) with organic solvents, and solid-phase extraction (SPE) on commercial cartridges or Florisil-packed column have been tested at three concentration levels: 0.01, 0.1 and 1 mg/kg. LLE with n-hexane or SPE on a Florisil column resulted to be the most suitable procedures to analyze fipronil at trace concentrations. Fipronil was quantified by gas chromatography (GC) with electron-capture detection (ECD) or mass spectrometric (MS) detection after conventional or matrix-matched calibration. The detection limit of fipronil in honey samples was below 1 microg/kg. The degradation of fipronil in honey has also been studied, being identified three minor degradation products in the extracts.
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