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A fast and simple LC-ESI-MS/MS method for detecting pyrrolizidine alkaloids in honey with full validation and measurement uncertainty
- Valese, Andressa Camargo, Molognoni, Luciano, de Sá Ploêncio, Leandro Antunes, de Lima, Flávia Gontijo, Gonzaga, Luciano Valdemiro, Górniak, Silvana Lima, Daguer, Heitor, Barreto, Fabiano, Oliveira Costa, Ana Carolina
- Food control 2016 v.67 pp. 183-191
- detection limit, honey, ionization, liquid chromatography, monitoring, monocrotaline, natural toxicants, retrorsine, statistical analysis, tandem mass spectrometry, uncertainty, Brazil
- 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 (<LOD) in only one sample. Because PAs are natural toxins biosynthesized by plants, the importance of monitoring their concentration in honey is evident. For this purpose, a simple, low-cost extraction procedure was performed, and a high-throughput method was developed.