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A method was developed for determination of residues of 446 pesticides in fruits and vegetables through the use of cleanup by a 3-cartridge solid-phase extractiongas chromatography/ mass spectrometry (GC/MS) and liquid chromatography/tandem mass spectrometry (LC/MS/MS). Fruit and vegetable samples (20 g) were extracted with 40 mL acetonitrile, salted out, and centrifuged. Half of the supernatant was passed into an Envi-18 cartridge, eluted with acetonitrile, and cleaned up with Envi-Carb and aminopropyl Sep-Pak cartridges in series after concentration of the eluates. Pesticides were eluted with acetonitriletoluene (3 + 1, v/v), and eluates were concentrated to 0.5 mL and then added into internal standards after solvent exchange with 2 mL hexane and used for determination of 383 pesticides by GC/MS. The other half of the supernatant was concentrated to 1 mL and cleaned up with Envi-Carb and aminopropyl Sep-Pak cartridges in series. Pesticides were eluted with acetonitriletoluene (3 + 1, v/v), and the eluates were concentrated to 0.5 mL, dried with nitrogen gas, diluted to 1.0 mL with acetonitrilewater (3 + 2, v/v), and used for determination of 63 pesticides by LC/MS/MS. The limit of detection for the method was 0.2600 ng/g depending on the individual pesticide. In the method, fortification recovery tests at high, medium, and low levels were conducted on 6 varieties of fruits and vegetables, i.e., apples, oranges, grapes, cabbage, tomatoes, and celery, with average recoveries falling within the range of 55.0-133.8% for 446 pesticides, among which average recoveries between 60.0-120.0% accounted for 99% of the results. The relative standard deviation was between 2.1-39.1%, of which a relative standard deviation of 2.1-25.0% made up 96% of the results. Experiments proved that the method was applicable for determination of residues of 446 pesticides in fruit and vegetables.

journal of aoac international

Determination of Residues of 446 Pesticides in Fruits and Vegetables by Three-Cartridge Solid-Phase ExtractionGas Chromatography-Mass Spectrometry and Liquid Chromatography-Tandem Mass Spectrometry