QuEChERS method combined to liquid chromatography high-resolution mass spectrometry for the accurate and sensitive simultaneous determination of pyrrolizidine and tropane alkaloids in cereals and spices

Within the last decades, in the EU, there has been an increasing interest in toxic plant alkaloids as food contaminants, especially after the continuous and growing consumption of plant-based foods compared with food of animal origin. In this regard, the once neglected presence of these tropane alkaloids (TAs) and pyrrolizidine alkaloids (PAs) has recently been reconsidered by the European Food Safety Authority, highlighting the lack of data and the need to develop risk assessment strategies. For this reason, the emphasis has been placed on detecting their occurrence in food through the development of accurate and sensitive analytical methods to achieve the determination of these compounds. The present study aims to elaborate and validate an analytical method based on QuEChERS sample preparation approach, exploiting the UHPLC coupled to the HRMS to simultaneously identify and quantify 21 PAs and two TAs in cereals and spices. For TAs, the obtained limit of detection (LOD) is 0.1 μg·kg−1 and the limit of quantification (LOQ) is 0.4 μg·kg−1, while for PAs, the LODs values ranging between 0.2 to 0.3 μg·kg−1 and the LOQ, between 0.4 and 0.8 μg·kg−1, ensuring compliance with the recently established European Regulations. Several commercial samples were analysed to further verify the applicability of this comprehensive analytical approach.