Determination of zearalenone in grains by high-performance liquid chromatography–tandem mass spectrometry after solid-phase extraction with RP-18 columns or immunoaffinity columns

Abstract

In this paper a robust, sensitive and selective LC–MS–MS method for the determination of zearalenone (ZON) in several cereals is described. Sample preparation was performed by extraction of the commodities with a mixture of acetonitrile and water followed by solid-phase extraction with RP-18 columns or immunoaffinity columns. The selective determination of ZON was achieved with an atmospheric pressure chemical ionization interface. Using the negative ion mode a detection limit of 0.5 μg/kg and a determination limit of 1 μg/kg grain was achieved, which is by a factor of 100 more sensitive than the positive ion mode. Zearalanone (ZAN), which does not occur in nature, was used as internal standard for quantification. A linear working range from 1.0 μg/kg to 1000 μg/kg could be achieved in grains with a standard deviation of 4% and recovery rates around 100%. All these results were independent from the grain matrices (maize, barley, oats, wheat) when ZAN was used as internal standard. Sample preparation with RP-18 and immunoaffinity materials gave comparable results. In addition, the method was successfully used for the investigation of naturally contaminated maize samples in the course of an interlaboratory comparison test.