Analyses of selected non-authorized insecticides in peppers by gas chromatography/mass spectrometry and gas chromatography/tandem mass spectrometry

Two methods based on gas chromatography coupled with mass spectrometry and tandem mass spectrometry analyzers are described for the identification, confirmation and quantitation of two EU-banned insecticides: isocarbophos and isofenphos-methyl, detected in recent monitoring programmes in pepper samples. The proposed methodologies involved a liquid–liquid extraction with acetonitrile followed by a cleanup step by dispersive solid-phase extraction using primary–secondary amine as sorbent material. Recovery studies performed on peppers spiked at different fortification levels (10 and 50 μg kg−1) yielded average recoveries in the range 85–98% with RSD values below 8%. Identification, confirmation and quantitation were carried out by gas chromatography/mass spectrometry (GC–MS) in selected ion monitoring mode and gas chromatography/tandem mass spectrometry (GC–MS/MS) using an ion trap operating in the multiple reaction monitoring (MRM) mode. The obtained limits of detection (LODs) were in the range 0.1–0.3 μg kg−1, depending on the technique. The proposed methods were successfully applied to the analysis of suspected pepper samples.