Study of mycotoxin calibration approaches on the example of trichothecenes analysis from flour

The aim of this study was to evaluate the applicability of different calibration approaches in trichothecenes analysis from wheat flour. Concretely eight trichothecenes (five type B trichothecenes and three type A trichothecenes) were analyzed by matrix solid-phase dispersion (MSPD) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). In the first set of experiments the presence of matrix effects was evaluated; values ranged between 59% and 79%. In the second set of experiments, solutions to compensate these signal suppressions were examined. Different calibration methods showed to tackle matrix effects obtaining values between 69% and 85% for external matrix matched calibration and values from 76% to 111% and from 78% to 108% by analog and deuterated internal standard calibrations, respectively. Trueness of the method was studied using quality control material and certificated reference material (DON 1062 ± 110 μg kg−1). The values were compared by matrix-matched, analog internal standard (deepoxydeoxynivalenol (DOM-1)) and deuterated internal standard (DON-d1).

► First comparison between external and internal addition calibration for trichothecenes analysis. ► Analogs and deutered internal standards were successful for trichothecenes analysis in wheat flour. ► Matrix-matched calibration demonstrated to be useful for trichothecenes analysis in wheat flour. ► The trueness of the method was demonstrated by recoveries, quality control samples and certified reference material. ► Since it is not legislated, the analyst can decide the calibration method according to its possibilities.