Multi-residue pesticide analysis in virgin olive oil by nanoflow liquid chromatography high resolution mass spectrometry

Abstract

In this article, a nanoflow liquid chromatography system coupled to high resolution mass spectrometry (nanoflow LC/ESI Q-Orbitrap-MS) has been applied for the development of a multiresidue pesticide method for the determination of 162 multiclass pesticides in olive oil samples. Due to the relatively high lipid content of the raw QuEChERS acetonitrile extracts obtained from this type of fatty vegetable samples, a dispersive solid phase extraction (dSPE) sorbent proposed to retain both fatty acids and triglycerides, namely Enhanced Matrix Removal-Lipid (EMR-Lipid) has been implemented as additional cleanup step. The analytical performances of the proposed method were evaluated,achieving recoveries in the range 75–119% with relative standard deviations lower than 19% (n = 6). The dSPE sorbent allowed the removal of most coextracted interferences without a significant loss of analytes. Matrix effects were also evaluated, showing a negligible effect for most of the compounds tested, when a dilution factor of 50 was applied. Notably, despite the use of relatively high dilution factors (e.g. 1:50) to minimize matrix effects, the lowest concentration levels detected with this method – in the low μg kg−1 range – are well below the corresponding maximum residue levels established by the current European legislation.