Analysis of ergot alkaloids in cereal-based food products from the US market using LC-MS/MS

Cereal grains such as rye, wheat, oat, and barley are susceptible to ergot fungus such as Claviceps spp. that produce toxins known as ergot alkaloids (EAs), posing potential health risks to consumers. Despite growing global concern, occurrence data on EA contamination in cereal-based food products within the US market remains scarce. To address this data gap, a targeted LC-MS/MS method was developed and validated to quantify six predominant EAs and their corresponding epimers across a variety of cereal-based food matrices. Samples were prepared by extraction using a mixture of acetonitrile and water under alkaline conditions and clean-up using a MycoSep 150 Ergot SPE column. This method was single laboratory validated, demonstrating reliable performance with limits of quantification (LOQs) of 1.0 µg/kg for all analytes. The validated method was then applied to the analysis of sixty commercially available cereal-based products collected as a convenience sampling from the US market, revealing that 42% of food products (25 out of 60) analysed contained at least one detectable EA and seven products contained all 12 targeted EAs. Concentrations of individual EAs ranged between <1.0 and 231 μg/kg, while total EA concentrations ranged from <1.0 to 755 µg/kg in tested products. Among the product categories analysed, flour and rye-based products showed the highest incidence and concentrations of total EAs.