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

Rie Romme Rasmussen, Ida Marie Lindhardt Drejer Storm, Peter Have Rasmussen, Jørn Smedsgaard, Kristian Fog Nielsen

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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 (pH7). 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 mu g kg(-1). Validation results for citrinin, fumonisin B-1 and fumonisin B-2 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.
Original languageEnglish
JournalAnalytical and Bioanalytical Chemistry
Issue number2
Pages (from-to)765-776
Publication statusPublished - 2010


  • Silage
  • Mycotoxins
  • QuEChERS
  • LC-MS/MS
  • Validation
  • Maize


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