Ergot alkaloids: comparison of extraction efficiencies for their monitoring in several cereal-solvent combinations by UPLC-MS/MS

To date, there are more than 80 ergot alkaloids identified; their distribution depends on different factors (e.g. geographic regions, host plants). These toxins can cause acute and chronic toxic effects on human health and commonly infect cereal crops such as triticale and rye, wheat, barley and oats. Considering the growing consumption of plant-based foods, the European Food Safety Authority has highlighted the need to develop risk assessment strategies. This work focused on the optimization of extraction efficiency, to quantify the main ergot alkaloids and their epimers, that are available on the market without any legal restriction (ergosine, ergocristine, ergocriptyne, ergocornine, ergosinine, ergocristinine, ergocriptinine and ergocorninine). Considering the quantification of 8 out of 12 regulated compounds by EU (sum of -ine and -inine forms), this approach can be defined as a screening method for a reliable estimation of the risk, specifically devoted to industrial stakeholders that can then possibly outsource to authorized external labs only the samples suspected of significant positivity. The effectiveness of three different extraction conditions (acidic, alkaline and neutral) followed by a rapid clean-up using dispersive solid-phase extraction with C₁₈ sorbent was evaluated by ultra-performance liquid chromatography tandem quadrupole mass spectrometry (UPLC-MS/MS), resulting in a short chromatographic run (16 min). The method was developed and validated in five different cereal production chains (rye, oat, wheat, wheat gluten and baby food). The applicability of the method was examined by analyzing a set of 54 samples, including also other cereals like spelt, tritordeum and triticale, and evaluating also some reference materials.