Determination of Nitrogen- and Phosphorus-Containing Pesticide Residues in Vegetables by Gas Chromatography with Nitrogen–Phosphorus and Flame Photometric Detection after Gel Permeation Chromatography and a Two-Step Minicolumn Cleanup

An efficient and reliable multiresidue method for determining pesticide residues in a large number of vegetable samples was studied. First, the important target compounds for monitoring, 52 nitrogen-and/or phosphorus-containing pesticides, were selected. The sample was extracted with acetonitrile, and the separated acetonitrile layer was cleaned up by a salting-out step. The acetonitrile extract was purified by gel permeation chromatography that divided the pesticide eluate into 2 fractions; the pesticide fractions were respectively purified by a 2-step minicolumn cleanup in which the second pesticide fraction was loaded on a silica-gel minicolumn. After a Florisil minicolumn was inserted on the silicagel minicolumn, the first pesticide fraction was loaded on the tandem minicolumn, which was eluted with acetone–petroleum ether (3 + 7). The combined eluate was subjected to dual-column gas chromatography (GC) with nitrogen–phosphorus and flame photometric detection. By application of the optimum cleanup conditions to the 52 pesticides selected, good resolution and low breakdown levels of the pesticides during GC were maintained. Recoveries of the 52 pesticides from fortified cabbage, lettuce, spring onion, and spinach ranged from 72 to 108% with relative standard deviations of 2–17%, except for the recoveries of methamidophos and chlorothalonil. The detection limits of the pesticides were satisfactory (0.001–0.009 mg/kg) for monitoring pesticide residues in vegetables.