title: Multi-mycotoxin stable isotope dilution LC-MS/MS method for Fusarium toxins in cereals.
abstract: A multi-mycotoxin stable isotope dilution LC-MS/MS method was developed for 14 Fusarium toxins including modified mycotoxins in cereals (deoxynivalenol, 3-acetyldeoxynivalenol, 15-acetyldeoxynivalenol, HT2-toxin, T2-toxin, enniatin B, enniatin B1, enniatin A1, enniatin A, beauvericin, fusarenone X, nivalenol, deoxynivalenol-3-glucoside, and zearalenone). The chromatographic separation of the toxins with particular focus on deoxynivalenol and deoxynivalenol-3-glucoside was achieved using a C18-hydrosphere column. An expedient sample preparation method was developed that uses solid-phase extraction for the purification of trichothecenes combined with zearalenone, enniatins, and beauvericin and provides excellent validation data. Linearity, intra-day precision, inter-day precision, and recoveries were ≥0.9982, 1-6%, 5-12%, and 79-117%, respectively. Method accuracy was verified by analyzing certified reference materials for deoxynivalenol, HT2-toxin, and T2-toxin with deviations below 7%. The results of this method found barley malt samples from 2012, 2013, and 2014 frequently contaminated with high concentrations of enniatin B, deoxynivalenol, and its modified mycotoxin deoxynivalenol-3-glucoside. Samples from 2012 were especially contaminated. Fusarenone X was not detected in any of the analyzed samples.
authors.affiliation: Chair of Analytical Food Chemistry, Technische Universität München, Alte Akademie 10, 85354, Freising, Germany.
authors.forename: Katharina
authors.initials: K
authors.lastname: Habler
authors.affiliation: Chair of Analytical Food Chemistry, Technische Universität München, Alte Akademie 10, 85354, Freising, Germany. michael.rychlik@tum.de.
authors.forename: Michael
authors.initials: M
authors.lastname: Rychlik
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D002523:Edible Grain / Q000737:chemistry* / Q000382:microbiology; D005506:Food Contamination / Q000032:analysis*; D005670:Fusarium / Q000737:chemistry / Q000378:metabolism; D009183:Mycotoxins / Q000737:chemistry* / Q000378:metabolism; D011865:Radioisotope Dilution Technique; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D009183:Mycotoxins
keywords: Barley; Enniatins; LC-MS/MS; Solid-phase extraction; Stable isotope dilution assay; Trichothecenes