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Publication type: Journal Article
Document type: Full Paper

Year: 2003

Author(s): Razzazi-Fazeli, E; Böhm, J; Jarukamjorn, K; Zentek, J

Title: Simultaneous determination of major B-trichothecenes and the de-epoxy-metabolite of deoxynivalenol in pig urine and maize using high-performance liquid chromatography-mass spectrometry.

Source: J Chromatogr B Analyt Technol Biomed Life Sci. 2003; 796(1):21-33

Authors Vetmeduni Vienna:

Böhm Josef
Razzazi-Fazeli Ebrahim
Zentek Jürgen

Vetmed Research Units
Institute of Animal Nutrition and Functional Plant Compounds

A selective analytical method based on high-performance liquid chromatography (HPLC), combined with atmospheric pressure chemical ionisation (APCI-) mass spectrometry (MS), has been developed for simultaneous determination of B-trichothecenes and the major metabolites of deoxynivalenol. The method allows simultaneous analysis of nivalenol (NIV), deoxynivalenol (DON), 15-acetyldeoxynivalenol (15-AcDON), 3-acetyldeoxynivalenol (3-AcDON), fusarenon X (Fus-X) and de-epoxydeoxynivalenol (DOM-1). The method is based on one-step sample clean-up using a multifunctional MycoSep column. A linear gradient mobile phase system, consisting of water:acetonitrile:methanol (H2O:ACN:MeOH) at a flow-rate of 1 ml/min, and a Polar-RP C18 column, were utilised to obtain the best resolution of all tested compounds along with column and equilibrating within 30 min. Dexamethasone (Dex) was used as internal standard. The developed method shows good repeatability for inter- and intra-day precisions as well as good linearity of calibration curves (r2 ranged from 0.9936 to 0.9998). Average recoveries for tested compounds in both matrices have been determined ranging from 63.7 to 102.3% and limit of quantification (LOQ) ranged from 25 to 150 ng/g. The utility and practical impact of the method is demonstrated using contaminated pig urine and maize samples.

Keywords Pubmed: Animals
Atmospheric Pressure
Chromatography, High Pressure Liquid/methods*
Mass Spectrometry/methods*
Reproducibility of Results
Sensitivity and Specificity
Zea mays/chemistry*

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