Pressurized Liquid Extraction Coupled with LC–ESI–MS–MS for the Determination of Herbicides Chlormequat and Mepiquat in Flours

摘要

This paper describes a new method for the rapid extraction and unequivocal confirmation of herbicides chlormequat and mepiquat in wheat flours and various flours utilized in infant foods. The highly automated extraction procedure is based on accelerated solvent extraction, followed by liquid chromatography-tandem mass spectrometry as a confirmatory analysis. Typical recoveries from flours and baby food samples ranged from 83 to 99% at a fortification level of 10 ppb, corresponding to the maximum residue limits established by the European Union; while relative standard deviations (RSD) were less than 10% for all samples. The limit of detection (signal-to-noise ratio = 3) of the method for the considered phenols in baby food samples are less than 0.1 μg g−1. Traces of the selected herbicides have been detected in about 50% of baby foods, bought from different Roman supermarkets and butcher shops, applying the described methodology. Keywords Column liquid chromatography–mass spectrometry - Pressurized liquid extraction - Chlormequat and mepiquat