Screening procedure for organochlorine and organophosphorus pesticide residues in milk using matrix solid phase dispersion (MSPD) extraction and gas chromatographic determination

Abstract

A rapid technique for the extraction and gas chromatographic determination of five organochlorine and five organophosphorus pesticide residues in milk is described. Milk (5.0 ml) is blended with 2.0 g of C18 [octadecylsilyl-derivatized silica] and 1.5 ml acetonitrile in a syringe barrel. After the aqueous phase is removed from the column by vacuum aspiration, the pesticide residues are eluted from the C18/milk matrix with acetonitrile which is then eluted through a Florisil solid phase extraction (SPE) column. The acetonitrile is evaporated under nitrogen and the residue is dissolved in petroleum ether. This extract is directly analysed for organophosphorus pesticides by gas chromatography with flame photometric detection. After further clean-up of the extract on a mini-Florisil column, the organochlorine pesticide residues are determined by gas chromatography with electron capture detection. Grade A homogenized and raw milk samples were fortified with five organochlorine and five organophosphorus pesticide residues. The average recoveries of fortified organochlorine pesticide residues (2.0-20 ppb) ranged from 76.0% to 97.8%. The average recoveries of fortified organophosphorus pesticide residues (10-50 ppb) ranged from 75.0% to 104.5%. The MSPD and the AOAC International multiresidue method for pesticides in milk produced comparable results for milk samples containing incurred organochlorine pesticide residues. The use of the MSPD method results in a 90% reduction in organic solvent consumption and a 95% reduction in the hazardous waste generated when compared with the AOAC method.