Determination of pesticides in vegetables using large-volume injection column liquid chromatography-electrospray tandem mass spectrometry

Direct injection of a large volume (900 μl) of a sample extract onto a liquid chromatographic (LC) column, LC separation and electrospray tandem mass spectrometric detection were used for the quantitative analysis of a wide polarity range of pesticides in carrots and potatoes. Rapid sample preparation involved extraction of a small amount of sample (2 g) with a small volume of organic solvent (3 ml), clean-up over a filter and dilution of the organic extract with the aqueous LC eluent. The extraction efficiency for the selected pesticides was studied using methanol, acetone and acetonitrile as solvents. Evaluation of the performance of the overall method, using extraction with acetonitrile and detection in the selected-reaction-monitoring mode, showed excellent linearity in the range of 2-100 μg/kg with limits of detection of 0.5-2 μg/kg for both types of vegetable. With relative standard deviations of the MS peak area measurements of less than 6.5% (n = 8) the repeatability of the method was fully satisfactory. (C) 2000 Elsevier Science B.V.