A fast and simple LC-ESI-MS/MS method for detecting pyrrolizidine alkaloids in honey with full validation and measurement uncertainty

•A full-validated LC-MS method for detecting eight PAs in honey was developed.•A simple, environmentally friendly extraction was performed.•Despite their potential health consequences, no regulatory levels were settled.•At least three PAs were detected in 99.07% of the 92 samples.•Several analysed samples exceeded the suggested tolerable daily doses for PAs.

A fast and simple method was developed to determine pyrrolizidine alkaloids (PAs) in honey using liquid chromatography tandem mass spectrometry (LC- MS/MS) with electrospray ionization (ESI). An efficient extraction procedure was carried out by simply diluting with water, without the need of any additional clean-up steps. A full validation of the method was performed according to Commission Decision 2002/657/EC. The method was linear in the 050 μg kg−1 range and presented satisfactory intra-day and inter-day precision with relative standard deviations of 1.45-10.2% and 1.60-1-0.2%, respectively. The measurement uncertainty, limit of detection (LOD) (0.1-1.0 μg kg−1) and limit of quantification (LOQ) (0.2-1.5 μg kg−1) were also calculated. The proposed method was applied to analyse eight PAs, namely, senecionine, senecionine-N-oxide, echimidine, intermedine, lycopsamine, retrorsine, monocrotaline and retrorsine-N-oxide, in 92 commercial honey samples from Brazil. At least three PAs were detected in 99.1% of the samples. PAs were not detectable (

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