Validation of Two Variations of the QuEChERS Method for the Determination of Multiclass Pesticide Residues in Cereal-Bas

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Validation of Two Variations of the QuEChERS Method for the Determination of Multiclass Pesticide Residues in Cereal-Based Infant Foods by LC–MS/MS Chris J. Anagnostopoulos & Pipina Aplada Sarli & Konstantinos Liapis & Serko A. Haroutounian & George E. Miliadis

Received: 15 May 2011 / Accepted: 31 August 2011 / Published online: 15 September 2011 # Springer Science+Business Media, LLC 2011

Abstract Over the past years to ensure food safety and particular for food that intend to be consumed by infants and young children, the European Union has adopted specific legislation concerning the control of pesticide residue levels in that kind of food. In this paper, a liquid chromatography tandem quadrupole mass spectrometry (LC–MS/MS) multiresidue method for the simultaneous analysis of 23 pesticides and metabolites chosen according to the Commission Directives 2006/141/EC, 2006/125/EC, and 96 multiclass pesticides and metabolites chosen according to their physicochemical properties is presented and validated. The extraction procedure is based on three modifications of the quick, easy, cheap, effective, rugged, and safe method according to the analyte. The analytical performance was demonstrated by the analysis of extracts from cereal-based infant foods, spiked at two concentration levels for each pesticide or metabolite. Good sensitivity and selectivity of the method were obtained with limits of quantification at 10 or 3 μg/kg, depending on the analyte. C. J. Anagnostopoulos (*) : P. Aplada Sarli : K. Liapis : G. E. Miliadis Laboratory of Pesticide Residues, Department of Pesticides Control and Phytopharmacy, Benaki Phytopathological Institute, 145 61 Kifissia, Athens, Greece e-mail: [email protected] S. A. Haroutounian Laboratory of General Chemistry, Science Department, Agricultural University of Athens, 118 55 Athens, Greece

All pesticides and metabolites, except six cases, gave recoveries in the range of 60.4–125.4%, with relative standard deviations less than 29.7%, for both validation levels. Keywords QuEChERS . LC–MS–MS . Cereal-based infant foods . Validation . Pesticide residues

Introduction The protection of food crops against pests and diseases by various pesticides is a common approach in conventional farming. Because of the potential health risk for consumers resulting from acute and/or chronic dietary exposure, maximum residue levels for many pesticide/commodity combinations have been established in the European Union (Stepan et al. 2005). Infants and children, comparing to adults, are heavily exposed to pesticides and biologically are more vulnerable to them, due to high food consumption rate per kilogram of body weight. Commission Directive 2006/125/EC codifies and replaces the previous Directive (European Commission 2006a, b) which had been amended a number of times. It sets the rules on the composition and labeling of processed cereal-based foods for particular nutritional use for infants and young children in good health and is intended for use by infants when they are being weaned and as a