Multiresidue analysis of pesticides in vegetables and fruits by gas chromatography/mass spectrometry after gel permeation chromatography and graphitized carbon column cleanup

A multiresidue method for pesticides that enables quantitative, sequential analysis of a large number of vegetable and fruit samples by gas chromatography/mass spectrometry has been developed. First, 89 important target compounds were selected for monitoring, and then the appropriate internal standards for these pesticides, 14 stable isotopically labeled pesticides (surrogates), were used. The sample was extracted with acetonitrile, and the extract was cleaned up by a salting-out step followed by redissolution in ethyl acetate. Coextractives were removed automatically by gel permeation chromatography with a graphitized carbon column, and then by use of a tandem silica-gel/PSA cartridge column. Recoveries of 82 of the 89 pesticides from fortified spinach, tomato, apple, and strawberry were within a range from 70 to 120%, and the relative standard deviation values of 80 of the 89 pesticides were <5%. The method was applied to 188 commercial vegetable and fruit samples to demonstrate its use in routine analysis.