title: Development and validation of a high performance liquid chromatographic-mass spectrometry method for the simultaneous quantification of 10 trichothecenes in ultra-high temperature processed cow milk.
abstract: An LC-MS/MS (QqQ) method has been developed and validated for simultaneous determination of the following trichothecenes in UHT cow milk: nivalenol (NIV), deoxynivalenol (DON), deepoxy-deoxynivalenol (DOM-1), 3-acetyldeoxynivalenol (3-ADON), 15-acetyldeoxynivalenol (15-ADON), neosolaniol (NEO), diacetoxyscirpenol (DAS), fusarenon X (FUS-X), T-2 and HT-2 toxins. Sample treatment is simple and based on the extraction with acetonitrile (ACN), acidified with 0.2% formic acid, followed by a purification process, adding sodium acetate to the ACN/water extract in order to separate aqueous phase and, consequently, polar components of the milk. Validation of the method for all the 10 mycotoxins was successful; validation parameters taken into account were as follows: limits of detection (LOD) and quantification (LOQ), linearity, precision (within-day and between-day variability), recovery, matrix effect and stability. The LODs were 10.1, 2.5, 1.5, 1.9, 0.1, 0.5, 1.0, 0.08, 0.4 and 0.05ng/mL for NIV, DON, DOM-1, FUS-X, NEO, 3-ADON, 15-ADON, DAS, HT-2 and T-2, respectively. Mean recovery values (obtained in intermediate precision conditions) were between 63.5 and 75.8 (RSDR≤15%) for all the mycotoxins. All the mycotoxins suffered from matrix effects, especially DON.
authors.affiliation: Organic and Pharmaceutical Chemistry Department, Faculty of Pharmacy, University of Navarra, , C/Irunlarrea 1, 31008 Pamplona, Navarra, Spain. Electronic address: mflores.6@alumni.unav.es.
authors.forename: Myra E
authors.initials: ME
authors.lastname: Flores-Flores
authors.affiliation: Organic and Pharmaceutical Chemistry Department, Faculty of Pharmacy, University of Navarra, , C/Irunlarrea 1, 31008 Pamplona, Navarra, Spain. Electronic address: mgpenas@unav.es.
authors.forename: Elena
authors.initials: E
authors.lastname: González-Peñas
mesh_terms: D000818:Animals; D002851:Chromatography, High Pressure Liquid; D006358:Hot Temperature; D057230:Limit of Detection; D008892:Milk / Q000737:chemistry*; D053719:Tandem Mass Spectrometry / Q000379:methods; D014255:Trichothecenes / Q000032:analysis*
chemical_list: D014255:Trichothecenes
keywords: LC–MS/MS; Milk; Mycotoxin; Trichothecenes; UHT cow milk