RESEARCH ARTICLE Studies on the applicability of HPLC-FLD and HPLC–MS/MS for the determination of ergot alkaloids in rye-containing breads Ba ¨rbel Kniel 1 • Michael Meißner 2 • Peter Koehler 1 • Christine Schwake-Anduschus 3 Received: 29 June 2017 / Accepted: 9 November 2017 Ó Bundesamt fu ¨r Verbraucherschutz und Lebensmittelsicherheit (BVL) 2017 Abstract The aim of this study was to elucidate the applicability of different analytical methods for the quantitation of ergot alkaloids in rye-containing bread by means of a multi-laboratory study, and to clarify how processing of rye flour into bread affects the content of ergot alkaloids at different processing stages. Wholegrain and refined rye flours were spiked to an ergot alkaloid concentration of 500 lg/ kg with ergot powder and then processed into mixed rye/wheat and wholegrain rye breads. Twelve ergot alkaloids were quantitated in flour, dough, and bread by means of liquid chromatography–fluorescence detection and liquid chromatography-tandem mass spectrometry. The effect of sample drying on the ergot alkaloid concentration was also studied. The study was carried out by two laboratories; selected bread samples were additionally analysed by two further laboratories. Both laboratories and analytical methods yielded reliable results with standard deviations of 8–9 % with spiked rye flours. Short-time dough fermentation had no effect on the recoveries. Independent of the analytical method, the bread recoveries were between 42 and 109 %, showing high measurement uncertainty of up to 40 %, which was due to both a non-standardised analytical method and the calculation of the total ergot alkaloid content from 12 individual alkaloid concentrations. Air- or freeze-drying of samples prior to analysis led to partly low recoveries. In conclusion, the study showed that there is an urgent need for a standard- ised analytical method for the quantitation of ergot alkaloids content in baked goods to enable the reli- able control of legal thresholds. Keywords Ergot alkaloids Á Analysis Á Cereals Á Rye Á Bread 1 Introduction In 2012, the European Food Safety Authority (EFSA) published a detailed health assessment of the toxic ergot alkaloids (EA) present in ergots (EFSA 2012). On this basis, a tolerable daily intake (TDI; life-long intake) of 0.6 lg/kg body weight and an acute ref- erence dose (ARfD; one-time dose not eliciting an adverse reaction) of 1 lg/kg body weight were sug- gested. Legal thresholds for EA in foods have not been fixed up to now. A recent study has shown that EA occur frequently in rye- and wheat-containing foods, in particular in northern Europe (Malysheva et al. 2014). In this study, 84 % of rye- and 67 % of wheat-containing foods had EA-contents of up to 1.121 and 591 lg/kg, respectively. Electronic supplementary material The online version of this article (https://doi.org/10.1007/s00003-017-1142-9) contains supplementary material, which is available to authorized users. & Christine Schwake-Anduschus christine.schwake-anduschus@mri.bund.de 1 Biotask AG, Schelztorstraße 54-56, 73728 Esslingen, Germany 2 Detmolder Institut fu ¨r Getreide- und Fettanalytik (DIGeFa) GmbH, Schu ¨tzenberg 10, 32756 Detmold, Germany 3 Max Rubner-Institut (MRI), Bundesforschungsinstitut fu ¨r Erna ¨hrung und Lebensmittel, Institut fu ¨r Sicherheit und Qualita ¨t bei Getreide, Schu ¨tzenberg 12, 32756 Detmold, Germany J Consum Prot Food Saf https://doi.org/10.1007/s00003-017-1142-9 Journal of Consumer Protection and Food Safety Journal fu ¨ r Verbraucherschutz und Lebensmittelsicherheit 123