A stable and sensitive method has been developed for use in food and livestock product safety for the detection of mycotoxins. This newly developed method allows for the determination of T-2 toxin, HT-2 toxin and diacetoxyscirpenol (DAS) in heart, liver, spleen, lung, kidney, Glandular stomach, muscular stomach, small intestine, muscle, bone and brain samples from broilers using liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). The samples were initially extracted with ethyl acetate before being filtered through a 0.22μm nylon syringe filter and subjected to chromatographic separation on a reversed-phase C18 (50×2.1mm, 3μm) column. A mobile phase composed of 0.1% acetic acid and 10mM ammonium acetate in methanol and water was used in an assay of the levels of T-2 toxin, HT-2 toxin and DAS. For the analysis of the target compounds, the mass spectrometer was operated under positive electrospray ionization conditions in the selected reaction monitoring mode. The limit of detection was in the range of 0.02-0.05ng/g, whereas the limit of quantification was in the range of 0.08-0.15ng/g. The extraction recoveries of spiked samples from the high, intermediate and low levels ranged from 58.5% to 110.5%, and the relative standard deviation (RSD (%)) values were less than 17.0%. The results of inter- and intra-day precision (RSD (%)) were within 14.7%. The results revealed that the present method could be successfully applied to the analysis of T-2 toxin, HT-2 toxin and DAS in the real samples.
Keywords: , the limit of quantification; Broiler biological matrice; DAS; Diacetoxyscirpenol; ESI; HT-2; HT-2 toxin; LC–MS/MS; LOD,; LOQ; ME; PE; R(E); RSD; SRM; T-2; T-2 toxin; diacetoxyscirpenol; electrospray ionization; extraction recovery; liquid chromatography coupled to tandem mass spectrometry; matrix effects; process efficiency; relative standard deviation; selected reaction monitoring; the limit of detection.
Copyright © 2013 Elsevier B.V. All rights reserved.