Mycotoxins – Determination of deoxynivalenol and deepoxydeoxynivalenol in urine by LC-MS/MS
Biomonitoring Method – Translation of the German version from 2025
Marion Berger1 (Method development)Lennart Marske1 (Method development)
Bernhard Monien2 (External verification)
Solveigh Siodlaczek2 (External verification)
Thomas Göen3 (Head of the working group “Analyses in Biological Materials” of the Permanent Senate Commission for the Investigation of Health Hazards of Chemical Compounds in the Work Area, Deutsche Forschungsgemeinschaft)
Andrea Hartwig4 (Chair of the Permanent Senate Commission for the Investigation of Health Hazards of Chemical Compounds in the Work Area, Deutsche Forschungsgemeinschaft)
MAK Commission5
1 Federal Institute for Occupational Safety and Health (BAuA), Division 4 – Hazardous Substances and Biological Agents, Unit 4.2 – Health Surveillance, Biological Monitoring, Nöldnerstraße 40/42, 10317 Berlin, Germany
2 German Federal Institute for Risk Assessment, Unit 54 – Food Safety Department, Max-Dohrn-Straße 8–10, 10589 Berlin, Germany
3 Friedrich-Alexander-Universität Erlangen-Nürnberg, Institute and Outpatient Clinic of Occupational, Social, and Environmental Medicine, Henkestraße 9–11, 91054 Erlangen, Germany
4 Institute of Applied Biosciences, Department of Food Chemistry and Toxicology, Karlsruhe Institute of Technology (KIT), Adenauerring 20a, Building 50.41, 76131 Karlsruhe, Germany
5 Permanent Senate Commission for the Investigation of Health Hazards of Chemical Compounds in the Work Area, Deutsche Forschungsgemeinschaft, Kennedyallee 40, 53175 Bonn, Germany
Abstract
The working group “Analyses in Biological Materials” of the German Senate Commission for the Investigation of Health Hazards of Chemical Compounds in the Work Area (MAK Commission) developed and verified the presented biomonitoring method. The aim of this method is the selective and sensitive quantitation of deoxynivalenol (DON; free DON plus glucuronides not otherwise specified) and its metabolite deepoxydeoxynivalenol (DOM-1) in urine. After enzymatic hydrolysis of the urine sample and purification of the analytes on an immunoaffinity column, followed by preconcentration of the eluates under a stream of nitrogen, determination is carried out by high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). Calibration is performed with comparative standards prepared in urine and treated analogously to the samples to be analysed. DON is quantified using an internal standard (ISTD; 13C15-DON), whereas DOM-1 is quantified without the use of an ISTD. Good precision data with standard deviations below 9% for DON and below 6% for DOM-1, as well as good accuracy data with mean relative recoveries in the range of 93–114% for DON and 97–103% for DOM-1, show that the method provides reliable and accurate analytical results. The method is both selective and sensitive, and has a limit of quantitation of 0.179 μg/l for DON and of 0.26 μg/l for DOM-1. Due to rapid renal excretion, the method is primarily suitable for analysing acute exposure which occurred only hours prior to sampling.
