Development of a liquid chromatography–tandem mass spectrometry with ultrasound-assisted extraction and auto solid-phase clean-up method for the determination of Fusarium toxins in animal derived foods

A liquid chromatography–tandem mass spectrometry (LC–MS/MS) was developed for the simultaneous determination of 19 Fusarium toxins and their metabolites including deoxynivalenol (DON), nivalenol (NIV), T-2 toxin (T-2), HT-2 toxin (HT-2), 3-acetyldeoxynivalenol (3-AcDON), 15-acetyldeoxynivalenol (15-AcDON), neosolaniol (NEO), fusarenon-X (F-X), diacetoxyscirpenol (DAS), monoacetoxyscirpenol (MAS), zearalanone (ZAN), zearalenone (ZON), α-Zearalenol (α-ZOL), β-Zearalenol (β-ZOL), a-Zearalanol (α-ZAL), β-Zearalanol (β-ZAL), T-2 triol, T-2 tetraol, deepoxy-deoxynialenol (DOM-1) in the muscle, liver, kidney, fat of swine, bovine and sheep, muscle and liver of chicken, muscle and skin of fish, as well as milk and eggs. Sample preparation procedure includes ultrasound-assisted extraction with acetonitrile/water (90/10, v/v), defatting with n-hexane and final clean-up with auto solid phase extraction (SPE) on Bond Elut Mycotoxin cartridges. The detection and quantification of the analytes were performed by a reversed-phase liquid chromatography coupled with electrospray ionization triple quadrupole mass spectrometry (LC/ESI-MS/MS). DON, NIV, DOM-1, 3-AcDON, 15-AcDON, F-X, ZON, ZAN, α-ZOL, β-ZOL, α-ZAL, β-ZAL, T-2 triol and T-2 tetraol were detected in a negative ion mode, while T-2 toxin, HT-2 toxin, NEO, DAS and MAS were detected in a positive ion mode. The CCα and CCβ of the analytes in different samples varied from 0.16 to 1.37 μg/kg and 0.33 to 2.34 μg/kg, respectively. The recoveries of spiked sample from 0.5 μg/kg to 8 μg/kg ranged from 64.8% to 108.2% with the relative standard deviations of less than 19.4%. Performances of the whole analytical procedure meet the criteria established by the European Commission for mass spectrometric detection.