(2013). Development and application of salting-out assisted liquid/liquid extraction for multi-mycotoxin biomarkers analysis in pig urine with high performance liquid chromatography/tandem mass spectrometry. Journal of Chromatography A, 1292Chromatography A, , 111-120. 10.1016Chromatography A, /j.chroma.2012
AbstractDirect determination of urinary mycotoxins is a better approach to assess individual's exposure than the indirect estimation from average dietary intakes. In this study, a new analytical method was developed and validated for simultaneous analysis of aflatoxin B 1 , deoxynivalenol, fumonisin B 1 , ochratoxin A, zearalenone and T2 toxin and their metabolites in pig urine. In total 12 analytes were selected. A salting-out assisted liquid-liquid extraction procedure was used for sample preparation. High performance liquid chromatography tandem mass spectrometry was used for the separation and detection of all the analytes. The extraction recoveries were in a range of 70% to 108%, with the intra-day relative standard deviation and inter-day relative standard deviation of lower than 25% for most of the compounds at 3 different concentration levels. Meanwhile method bias for all the analytes did not exceed 20%. The method limits of quantification ranged from 0.07 ng mL -1 for ochratoxin A to 3.3 ng mL -1 for deoxynivalenol. Matrix effect was evaluated in this study and matrixmatched calibration was used for quantification. The developed method was also validated for human urine as an extension of its application. Finally, the developed method was applied in a pilot study to analyze 28 pig urine samples. Deoxynivalenol, aflatoxin B 1 , fumonisin B 1 and ochratoxin A were detected in these samples.