Determination of fipronil residues in honey and pollen by gas chromatography

C Sánchez Brunete,J.L Tadeo,E Miguel,B Albero

doi:10.5424/sjar/200806s1-368

Abstract

This work describes the development of the analytical methodology for determining fipronil residues in honey and pollen samples by gas chromatography with two detecting systems: electron-capture detection (GC-ECD) and mass spectrometry (GC-MS). Fipronil was extracted from honey samples by solid-phase extraction, using alumina as adsorbent and hexane-ethyl acetate (1:1, v/v) as eluting solvent, and from pollen samples by matrix solid-phase dispersion with C18 and acetonitrile, assisted by sonication. The developed methods gave recovery results >90% with relative standard deviations

Highlights

This work describes the development of the analytical methodology for determining fipronil residues in honey and pollen samples by gas chromatography with two detecting systems: electron-capture detection (GC-electron-capture detectors (ECD)) and mass spectrometry (GC-MS)
Los límites de detección obtenidos con GC-ECD fueron 1 μg kg-1 para el polen y 0,5 μg kg-1 para la miel y los valores correspondientes para GC-MS fueron 0,2 y 0,1 μg kg-1, respectivamente
The aim of this study was to develop the analytical methodology for the determination of fipronil in honey and pollen samples, based on solid-phase extraction (SPE) and Matrix solid-phase dispersion (MSPD), respectively

Summary

Introduction

This work describes the development of the analytical methodology for determining fipronil residues in honey and pollen samples by gas chromatography with two detecting systems: electron-capture detection (GC-ECD) and mass spectrometry (GC-MS). The limits of detection obtained with GC-ECD were 1 μg kg-1 for pollen and 0.5 μg kg-1 for honey and the corresponding values for GC-MS were 0.2 and 0.1 μg kg-1, respectively These methods were applied to the determination of fipronil levels in various samples of honey and pollen commercialised in Spain and no residues of this compound were detected. Matrix solid-phase dispersion (MSPD) is an extraction technique that has been used in the determination of fipronil in honeybees (Morzycka, 2002) These techniques, SPE and MSPD, were firstly applied by our laboratory for the extraction of fipronil from honey and pollen samples, respectively (Sánchez-Brunete et al, 2005a)

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