Optimization of a matrix solid-phase dispersion method for the analysis of pesticide residues in vegetables

A multiresidue method based on matrix solid-phase dispersion (MSPD) is studied to determine chlorfenvinfos, chlorpyrifos, fenarimol, iprodione, procimydone, propiconazole, tetradifon, triadimefon and vinclozolin in artichokes, green beans, lettuces and tomatoes. Alumina, silica and Florisil were assessed as extracting phases, and the extracts from Florisil were the cleanest. To facilitate manual extraction, sand was added to the sample together with the dispersing phase. Three eluting systems were then studied, and dichloromethane proved to be the best. Further purification can be performed using solid-phase cleanup after diluting extracts with aqueous solutions. Octyl- and octadecyl-silica, modifications of the aqueous diluted extracts and several eluting solvents were studied. Determination was done by capillary gas chromatography (GC) with electron-capture detection, and confirmed by GC-MS using the electron impact mode and the selected ion monitoring. The proposed MSPD method was used to analyze 48 samples taken in the course of a year. Procymidone, vinclozolin, chlorpyrifos and chlorfenvinfos were identified in 10 samples at levels below the maximum residue levels allowed by the Spanish Government.