Journal
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
Volume 879, Issue 24, Pages 2403-2415Publisher
ELSEVIER
DOI: 10.1016/j.jchromb.2011.06.036
Keywords
Mycotoxins; Trichothecenes; Deoxynivalenol; T-2 toxin; LC-MS/MS; Plasma; Bile
Funding
- Institute for the Promotion of Innovation by Science and Technology in Flanders (IWT-Vlaanderen), Brussels, Belgium [070574, 101301]
- Ghent University [01J08309]
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A sensitive and specific method for the quantitative determination of deoxynivalenol (DON), deepoxydeoxynivalenol (DOM-1), T-2 toxin (1-2) and HT-2 toxin (HT-2) in animal body fluids (plasma and bile) using liquid chromatography combined with electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) is presented. The extraction of plasma consisted of a deproteinization step using methanol, followed by a clean-up using an Oasis (R) HLB solid-phase extraction column. For bile analysis, an extraction using a methanol/water mixture (70/30, v/v), followed by a liquid-liquid extraction using ethyl acetate, was performed. Chromatographic separation was achieved on a reversed-phase Nucleosil (100-5 C18 G100 x 3.0 mm) column. For the analysis of DON and DOM-1, a mixture of 0.1% acetic acid in water and methanol was used as the mobile phase. 1-2 and its metabolite HT-2 were separated using 5 mM ammonium acetate in a mixture of water/methanol/acetic acid. The mass spectrometer was operated in the negative or positive ESI selected reaction monitoring mode for DON and 1-2 analysis, respectively. Calibration graphs (1-250 ng mL(-1)) were prepared for all matrices and correlation and goodness-of-fit coefficients were between 0.9978-1.000 and 2.96-11.77%, respectively. Limits of quantification were between 1 and 2.5 ng mL(-1) for all compounds. Limits of detection ranged from 0.01 to 0.63 ng mL(-1). The results for the within-clay precision and accuracy fell within the ranges specified. The method has been successfully used for the quantitative determination of DON, DOM-1, T-2 and HT-2 in plasma and the semi-quantitative determination of the same compounds in bile from broiler chickens and pigs, respectively. (C) 2011 Elsevier B.V. All rights reserved.
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