Determination of zearalenone and its metabolites alpha- and beta-zearalenol in beer samples by high-performance liquid chromatography-tandem mass spectrometry.


A fast, robust and sensitive LC-MS-MS method for the determination of zearalenone (ZON) and its metabolites alpha-zearalenol (alpha-ZOL) and beta-zearalenol (beta-ZOL) in beer samples is described. Sample preparation was performed by direct RP-18 solid-phase extraction of undiluted beer samples followed by selective determination of analytes by LC-MS-MS applying an atmospheric pressure chemical ionization (APCI) interface. Using the negative ion mode limits of determination of 0.03-0.06 microg l(-1) beer and limits of quantification of 0.07-0.15 microg l(-1) beer were achieved, which was distinctly more sensitive than in the positive ion mode. Twenty-three beer samples from different countries, produced from different grains and under different brewing conditions, were investigated by this method, but only in one sample could beta-ZOL and ZON be detected. Independently of the type of beer, relative standard deviations between 2.1% and 3.3%, a linear working range of 0.15 microg l(-1) to 500 microg l(-1) beer and recovery rates around 100% could be achieved when zearalanone (ZAN) was used as internal standard.