Mykotoxine – Bestimmung von Deoxynivalenol und Deepoxydeoxynivalenol in Urin mittels LC-MS/MS

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.