A simple and accurate method has been developed for the simultaneous determination of four pyrrolizidine alkaloids (PAs) including echimidine, senecionine, jacobine and intermidine in food supplements of plant origin. The instrumental conditions including the use of TSK-Gel column for the separation and an MS/MS detector in positive ESI source, multi-reactive monitoring (MRM) mode for quantitation were optimized. The method has fully validated and meets the performance requirement of AOAC with good specificity. The linearity varies from 1.0 µg/kg to 40 µg/kg, the LOD was of 0.3 µg/kg; the repeatability and recovery range from 3.6% to 7.5% and 88.7% to 117%, respectively. The method was applied to determine PAs in 90 food supplement samples, of which 26 samples (28.8%) contain PAs.
LC-MS/MS, pyrrolizidine alkaloids, senecionine, jacobine, intermidine, echimidine
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