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

Rasmussen, R.; Storm, I.; Rasmussen, P.; Smedsgaard, J.; Nielsen, K.
May 2010
Analytical & Bioanalytical Chemistry;May2010, Vol. 397 Issue 2, p765
Academic Journal
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 �g 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. [Figure not available: see fulltext.]


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