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The present work describes the development and analytical validation of a method involving microextraction packed sorbent and gas chromatography coupled to mass spectrometry (MEPS-GC-MS) for the multi-residue analysis of 22 pesticides (permethrin, fenpropathrin, aldrin, α-hexachlorocyclohexane, β-hexachlorocyclohexane, lindane, vinclozolin, endosulfan, heptaclor, dodecaclor, tetradifon, 1,1-dichloro-2,2-bis (p-chlorophenyl)ethane, 1,1-bis(p-chlorophenyl)-2,2-dichloroethylen, carbofuran, carbaryl, pirimiphos methyl, chlorpyriphos, dimethoate, disulfoton, fenamiphos, terbufos and profenofos) in honey samples. The MEPS variables of sample pH, draw-eject cycles, ionic strength and desorption procedure were optimized to improve the sensitivity of the proposed method. The method was shown to be linear at concentrations ranging from 2, 5 and 10 ng/g (limit of quantification) to 75-100 ng/g. These values are lower than those established as the maximum residue limits for honey samples. The accuracy values (82-114%) were adequate for all the analytes, as were the inter-day precision data, with coefficient of variation lower than 14%. On the basis of analytical validation, the MEPS-GC methodology has been shown to be a promising alternative for the analysis of pesticides in honey samples. The MEPS packed syringe can be reused 40 times for honey samples, whereas the conventional solid-phase extraction (SPE) column can only be used once. Compared with liquid-liquid extraction and SPE, MEPS is able to reduce sample preparation time and organic solvent consumption.

Microextraction in Packed Sorbent for the Determination of Pesticides in Honey Samples by Gas Chromatography Coupled to Mass Spectrometry