The application of salting out assisted liquid-liquid extraction for the rapid and simple simultaneous determination of pyrrolizidine alkaloids and related N-oxide in honey and pollen was evaluated. The determination of PAs and PANOs was obtained by ultra high performance liquid chromatography coupled with tandem mass spectrometry. The critical parameters (pH of the aqueous solution, extraction solvent, type and amount of salting-out agents) affecting SALLE performance were carefully studied and optimized using a chemometric approach. Under the optimal experimental conditions, the developed procedure showed excellent extraction efficiency (82-104%) and recoveries (82-113%) for all target analytes, except for Intermedine N-oxide, at three concentration levels (0.25, 2.5 and 25 μg kg-1 and 2.5, 25 and 250 μg kg-1 for honey and pollen samples, respectively), and satisfactory intra-day (<10) and inter-day (<13) precisions. The proposed method showed negligible matrix effect for both studied matrices and method quantification limits at very low levels...

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