Analysis of Pesticides in Honey by Solid-Phase Extraction and Gas Chromatography−Mass Spectrometry

Abstract

An analytical method for the simultaneous determination of 51 pesticides in commercial honeys was developed. Honey (10 g) was dissolved in water/methanol (70:30; 10 mL) and transferred to a C(18) column (1 g) preconditioned with acetonitrile and water. Pesticides were subsequently eluted with a hexane/ethyl acetate mixture (50:50) and determined by gas chromatography with electron impact mass spectrometric detection in the selected ion monitoring mode (GC-MS-SIM). Spiked blank samples were used as standards to counteract the matrix effect observed in the chromatographic determination. Pesticides were confirmed by their retention times, their qualifier and target ions, and their qualifier/target abundance ratios. Recovery studies were performed at 0.1, 0.05, and 0.025 microg/g fortification levels for each pesticide, and the recoveries obtained were >86% with relative standard deviations of <10%. Good resolution of the pesticide mixture was achieved in approximately 41 min. The detection limits of the method ranged from 0.1 to 6.1 microg/kg for the different pesticides studied. The developed method is linear over the range assayed, 25-200 microg/L, with determination coefficients of >0.996. The proposed method was applied to the analysis of pesticides in honey samples, and low levels of a few pesticides (dichlofluanid, ethalfluralin, and triallate) were detected in some samples.