Multiresidue mycotoxin analysis in wheat, barley, oats, rye and maize grain by high-performance liquid chromatography-tandem mass spectrometry

Abstract

A method has been developed for the simultaneous analysis of 22 mycotoxins in wheat, barley, oats, rye and maize grain. Analysis is carried out with liquid chromatography-electrospray ionisation tandem mass spectrometry. The compounds included in this analysis are aflatoxins, sterigmatocystin, cyclopiazonic acid, tricothecenes, ochratoxin A, fumonisins, zearalonone, and ergot alkaloids. Sample extraction (2 g) with acetonitrile:water (8 ml, 80:20) was carried out for 2 min using a commercial sample preparation apparatus (Stomacher®). The extract was then centrifuged, filtered and analysed. Extraction of fumonisins from maize (2 g) was optimised by first extracting the maize with acetonitrile: water (5 ml, 80:20) followed by the addition of water (3 ml), which permitted extraction of the 22 mycotoxins, including the fumonisins. Chromatography was carried out with a minicolumn (7.5×2.1 mm, 5 µm) (5 µl sample injection) and in 11 min, including column reconditioning. Analysis was carried out with 2 MRM transitions for the precursor ions. All method detection limits were below current maximum Canadian residue limits. Matrix effects for each compound in each of the 5 matrices were estimated and ranged from 70 to 149%, but most were 100±10%. Accuracy, repeatability and ruggedness were established. Proficiency samples from FERA (Food and Environment Research Agency, Sand Hutton, York, UK) were tested and are reported. Finally, 100 field samples of the various grains were tested with this method and are reported with the observation of numerous mycotoxins in all matrices, including ergotamine in winter wheat.