Determination of trichothecenes in cereals and derived products by liquid chromatography tandem mass spectrometry
Résumé
A sensitive, accurate and precise method for the simultaneous determination of nivalenol (NIV), deoxynivalenol (DON), T-2 toxin (T-2) and HT-2 toxin (HT-2) in different food matrices, including wheat, maize, barley, cereal-based infant foods, snacks, biscuits and wafers has been developed. The method, using liquid chromatography coupled with atmospheric pressure chemical ionization triple quadrupole mass spectrometry (LC-APCI-MS/MS), allowed unambiguous identification of the selected trichothecenes at low µg/kg levels in such complex food matrices. A clean up procedure, based on reversed phase SPE Oasis® HLB columns was used, allowing good recoveries for all studied trichothecenes. In particular, NIV recoveries resulted significantly improved as compared with those obtained by using Mycosep® #227 columns for the clean up of the extracts. Limits of detection in the various investigated matrices, ranged from 2.5 to 4.0 µg/kg for NIV, from 2.8 to 5.3 µg/kg for DON, from 0.4 to 1.7 µg/kg for HT-2, from 0.4 to 1.0 µg/kg for T-2. Mean recovery values, obtained from cereals and cereal products spiked with NIV, DON, HT-2 and T-2 toxins at levels from 10 to 1000 µg/kg, ranged from 72% to 110% with mean relative standard deviation lower than 10%. A systematic investigation of matrix effects in different cereals and cereal products was also carried out by statistically comparing the slopes of standard calibration curve with matrix-matched calibration curve for each of the 4 toxins and the 8 matrices tested herein. For seven out of the 8 matrices tested statistically significant matrix effects were observed, indicating that for accurate quantitative analysis matrix-matched calibration was necessary. The method was applied to the analysis of 57 samples of ground wheat originated from South Italy, and of 9 cereal food samples collected from retail market.
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