A method for the determination of zearalenone in corn has been developed applying pressurised liquid extraction (PLE) and using environmentally acceptable and less noxious organic solvents. The extracted samples were analysed with liquid chromatography coupled to mass spectrometry (LC-MS) equipped with an electrospray (ESI) ionisation interface. The optimised extraction mixture was isopropanol and an aqueous solution of triethylamine (1%) 50:50 (v/v), which allowed to halve the use of organic solvent compared to the method proposed by ISO. When applying the optimised method to five different naturally contaminated corn samples the obtained concentrations were slightly increased compared to the analysis using the previously used extraction solvent (acetonitrile-methanol). The relative standard deviation (RSD, n = 3) varied between 4 and 10% depending on the concentration level of the target analyte in the test material.