Method development towards qualitative and semi-quantitative analysis of multiple pesticides from food surfaces and extracts by desorption electrospray ionization mass spectrometry as a preselective tool for food control.

Abstract

Direct analysis of fruit and vegetable surfaces is an important tool for in situ detection of food contaminants such as pesticides. We tested three different ways to prepare samples for the qualitative desorption electrospray ionization mass spectrometry (DESI-MS) analysis of 32 pesticides found on nine authentic fruits collected from food control. Best recovery rates for topically applied pesticides (88%) were found by analyzing the surface of a glass slide which had been rubbed against the surface of the food. Pesticide concentration in all samples was at or below the maximum residue level allowed. In addition to the high sensitivity of the method for qualitative analysis, quantitative or, at least, semi-quantitative information is needed in food control. We developed a DESI-MS method for the simultaneous determination of linear calibration curves of multiple pesticides of the same chemical class using normalization to one internal standard (ISTD). The method was first optimized for food extracts and subsequently evaluated for the quantification of pesticides in three authentic food extracts. Next, pesticides and the ISTD were applied directly onto food surfaces, and the corresponding calibration curves were obtained. The determination of linear calibration curves was still feasible, as demonstrated for three different food surfaces. This proof-of-principle method was used to simultaneously quantify two pesticides on an authentic sample, showing that the method developed could serve as a fast and simple preselective tool for disclosure of pesticide regulation violations. Graphical Abstract Multiple pesticide residues were detected and quantified in-situ from an authentic set of food items and extracts in a proof of principle study.