Multitoxin extraction and detection of trichothecenes in cereals: an improved LC‐MS/MS approach

Abstract

AbstractBACKGROUND: Many multiresidual methods to evaluate natural occurrence of Fusarium toxins are already reported in the scientific literature but a new rapid, reliable, cost‐efficient and high‐sensitivity method for the simultaneous determination of several fusariotoxins is always welcome. Nivalenol (NIV), deoxynivalenol, fusarenon‐X (FUS‐X), 3‐acetyldeoxynivalenol, diacetoxyscirpenol (DAS), HT‐2 toxin, T‐2 toxin, neosolaniol (NEO), zearalanone and zearalenone (ZON) belong to the most common mycotoxins in food matrix grains, e.g., wheat and maize. The proposed method is a multitoxin analytical method that combines high‐performance liquid chromatography (HPLC), atmospheric pressure chemical ionization (APCI), triple‐quadrupole tandem mass spectrometry (LC‐MS/MS) under the selected reaction monitoring (SRM) mode, and it is focused on the optimization of the sample preparation without the need for any cleanup.RESULTS: Three different methods for sample preparation and for the simultaneous extractions of the above‐mentioned fusariotoxins were tested: two of these were followed by a different cleanup step for comparison, while the extraction method proposed in this work, which uses an 84% (v/v) acetonitrile aqueous solution, sample homogenization and subsequent filtration, was validated without any further cleanup step.CONCLUSION: Calibration curves for all analytes are linear, except DAS, HT‐2 and ZON, over the working range of 10–1000 µg kg−1. The calibration curve of DAS was linear between 10 and 500 µg kg−1, although the curves of HT‐2 and ZON were linear in the range 10–250 µg kg−1. Squared correlation coefficients (R2) were in the range 0.995–0.998 for the all point calibration curves. The lowest limits of detection (LOD) were found for DON and ZAN with 0.5 and 0.2 µg kg−1, respectively, while the highest LODs were obtained for NIV, FUS‐X and NEO, with 3.3 µg kg−1 for each toxin. Copyright © 2009 Society of Chemical Industry