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Analytical and Bioanalytical Chemistry

, Volume 397, Issue 2, pp 765–776 | Cite as

Multi-mycotoxin analysis of maize silage by LC-MS/MS

  • R. R. RasmussenEmail author
  • I. M. L. D. Storm
  • P. H. Rasmussen
  • J. Smedsgaard
  • K. F. Nielsen
Original Paper

Abstract

This paper describes a method for determination of 27 mycotoxins and other secondary metabolites in maize silage. The method focuses on analytes which are known to be produced by common maize and maize-silage contaminants. A simple pH-buffered sample extraction was developed on the basis of a very fast and simple method for analysis of multiple pesticide residues in food known as QuEChERS. The buffering effectively ensured a stable pH in samples of both well-ensiled maize (pH < 4) and of hot spots with fungal infection (pH > 7). No further clean-up was performed before analysis using liquid chromatography–tandem mass spectrometry. The method was successfully validated for determination of eight analytes qualitatively and 19 quantitatively. Matrix-matched calibration standards were used giving recoveries ranging from 37% to 201% with the majority between 60% and 115%. Repeatability (5–27% RSDr) and intra-laboratory reproducibility (7–35% RSDIR) was determined. The limit of detection (LOD) for the quantitatively validated analytes ranged from 1 to 739 µg kg−1. Validation results for citrinin, fumonisin B1 and fumonisin B2 were unsatisfying. The method was applied to 20 selected silage samples and alternariol monomethyl ether, andrastin A, alternariol, citreoisocoumarin, deoxynivalenol, enniatin B, fumigaclavine A, gliotoxin, marcfortine A and B, mycophenolic acid, nivalenol, roquefortine A and C and zearalenone were detected.

Maize silage fed to cows can be contaminated with mycotoxins from pre- and post-harvest fungi. Several metabolites were detected by LC-MS/MS; including zearalenone and mycophenolic acid from Fusarium (red) and Penicillium (green) infections, respectively.

Keywords

Mycotoxins Maize Silage LC-MS/MS Validation QuEChERS 

Notes

Acknowledgements

Funding for this study was provided by The Directorate for Food, Fisheries, and Agri Business (Copenhagen, Denmark (#FFS05)), Danish Cattle Federation, the Research School FOOD and the Technical University of Denmark.

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Copyright information

© Springer-Verlag 2010

Authors and Affiliations

  • R. R. Rasmussen
    • 1
    Email author
  • I. M. L. D. Storm
    • 2
  • P. H. Rasmussen
    • 1
  • J. Smedsgaard
    • 1
  • K. F. Nielsen
    • 2
  1. 1.National Food Institute, Division of Food ChemistryTechnical University of DenmarkSøborgDenmark
  2. 2.Center for Microbial Biotechnology, Department of Systems BiologyTechnical University of DenmarkKgs. LyngbyDenmark

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