A solid-phase microextraction method for the chromatographic determination of organophosphorus pesticides in fish, water, potatoes, guava and coffee

Abstract

This paper describes a Solid Phase Microextraction method (SPME-CG) to the determination of organophosphorus pesticides in samples of fresh-water fish, water, potatoes, guava and coffee by capillary gas chromatography with nitrogen phosphorus detector. The samples were collected from October 2002 to April 2003 in the tributaries and sub-tributaries of the Paranaiba River, which supplies the city of Patos de Minas, Minas Gerais, Brazil. The determination of the pesticides: co-ral (O,O-diethyl O-(3-chloro-4-methyl-2-oxo-2H-1-benzopyran-7-yl) phosphorothioate), DDVP (2,2-dichloroethenyl dimethylphosphate), disyston (O,O-diethyl S-[2-(ethylthio) ethyl] phosphorodithioate), ethion (O,O,O’,O’-tetraethyl S,S’-methylene bis(phosphorodithioate)), phorate (O,O-diethyl S-ethylthiomethyl phosphorodithioate), phosdrin (2-methoxycarbonyl-1-methylvinyl dimethyl phosphate), guthion (O,Odimethyl-S-[(4-oxo-1,2,3-benzotriazin-3(4H)-yl)methyl] phosphorodithioate)), malathion (diethyl (dimethoxy thiophosphorylthio succinate) and methyl-parathion (O,O-dimethyl O-4-nitrophenyl phosphorothioate) in samples of fish, water and others foods with a manual SPME-CG holder using a 100 μm PDMS microfiber, is simple, easy to handle and solvent-free. The optimised conditions for pesticides extraction by SPME-CG method were: sample agitation, absorption at room temperature for 40 min, desorption at 220°C for 10 min, and sample volume in the vial of 16.0 mL. Under these conditions, the analytical curves were linear in different ranges (depend of each pesticide) with correlation coefficients from 0.997 to 0.999 and the precision was good (RSD from 4.40 to 15.13%). The detection limit was 0.05 μg L-1 to 8.37 μg L-1 and the quantitation limit was 0.09 μg L-1 to 8.70 μg L-1. The method was employed to detect and quantify pesticides in 24 fish of three different species and also in water, potatoes, guava and coffee. The samples analyzed showed residues of six different organophosphorus pesticides.