Determination of organophosphorus pesticide residues in fruits by gas chromatography with ITD and NPD detection

Summary

Several widely used organophosphorus insecticides, diazinon, methyl-parathion, fenitrothion, malathion, fenthion and methidathion were selected for inclusion in this work. A comparative study of the multiresidue determination of these compounds in citrus fruit and grapes has been carried out by gas chromatography with nitrogen-phosphorus and ion trap detection. Samples were spiked with 0.1, 0.5 and 1 mg kg⁻¹ of each pesticide and blended in a Sorvall homogeniser with ethyl acetate. Column clean-up on Florisil was necessary for citrus peel extracts. The average recoveries varied from 81 to 107% with a relative standard deviation between 0.3 and 9.5% for GC-ITD and from 86 to 104% with a relative standard deviation ranging from 1.4 to 8.0% for GC-NPD. The detection limit of the method was 10 ng g⁻¹ or less for each organophosphorus insecticide, with both detectors. This method was applied to the analysis of treated lemons and 0.25 mg kg⁻¹ of fenitrothion in fruit was detected a week after treatment and identified by its mass spectrum. The results obtained showed that the proposed methods are reproducible and sensitive enough for the simultaneous determination of these insecticides in fruits at residue level.