Development and validation of an easy multiresidue method for the determination of multiclass pesticide residues using GC-MS/MS and LC-MS/MS in olive oil and olives

Abstract

Olives and olive oil are two of the most important commodities produced in the Mediterranean region. Due to their significant economical importance, the usage of pesticides in their production is systematic, by using a wide range of plant protection products with a variety of modes of action. As a consequence, monitoring of their residue levels in this products is a necessity. In the present study a gas and liquid chromatography-tandem mass spectrometry multiresidue method, with a short sample preparation step, based on acetonitrile extraction is developed and validated according to the European Union guidelines (SANCO Doc. No. 12495/2011) in olives and olive oil, with a large scope that includes pesticides of different chemical classes. Good sensitivity and selectivity of the method were obtained with limits of quantification at 10 μg/kg. All pesticides had recoveries in the range of 70-120%, with relative standard deviation values less than 20-25%, at both validation levels. Excellent linearity was achieved with r≥0,99 for both matrices. The method is easy, with low consumption of reagents, is characterized by reliability, sensitivity and therefore is suitable for the monitoring the levels of multiclass pesticides residues in olives and olive oil. The method was applied to 262 samples of the Greek market, of which 7% were found positive for the present of pesticides. In some of the samples 2-8 different analytes were detected.