Determination of zearalenone from wheat and corn by pressurized liquid extraction and liquid chromatography-electrospray mass spectrometry

Zearalenone (ZON) was extracted from wheat and corn by using pressurized liquid extraction (PLE) and the PLE extracts were analyzed using liquid-chromatography-mass spectrometry (LC-MS) without further clean-up procedures. A statistical design approach was applied to evaluate the influence of several extraction parameters such as temperature (40degreesC; 80degreesC; 120degreesC), time (5 min; 10 min) and solvent extraction mixture [acetonitrile-water (9:1, v/v); methanol-water (8:2, v/v); methanol-acetonitrile (1:1, v/v)] on fortified cereals. The results showed a strong influence of the solvent composition on recovery of ZON. Quantification of the analytes was performed by LC-MS analysis of the raw extract using matrix-matched standard curves. The method performance was tested in the selected conditions (80degreesC; 5 min; two cycles; methanol-acetonitrile) on samples which had been previously used for an international proficiency test. Compared to the assigned value, the recovered ZON was 118% [relative standard deviation (RSD) = 5.2%, n = 3)] and 107% (RSD = 2.2%, n = 3) in wheat and corn, respectively. Therefore, PLE can be used for ZON extraction, achieving good performances and allowing for an automated handling of the sample extraction step. Successively, the influence of temperature and number of cycles was investigated on naturally contaminated corn. From these results it could be concluded that fortified experiments perfectly mimicked naturally contaminated samples. (C) 2003 Elsevier Science B.V. All rights reserved.