TY - JOUR
T1 - Multi-mycotoxin analysis of maize silage by LC-MS/MS
AU - Rasmussen, Rie Romme
AU - Storm, Ida Marie Lindhardt Drejer
AU - Rasmussen, Peter Have
AU - Smedsgaard, Jørn
AU - Nielsen, Kristian Fog
PY - 2010
Y1 - 2010
N2 - 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.
AB - 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.
KW - Silage
KW - Mycotoxins
KW - QuEChERS
KW - LC-MS/MS
KW - Validation
KW - Maize
U2 - 10.1007/s00216-010-3545-7
DO - 10.1007/s00216-010-3545-7
M3 - Journal article
C2 - 20213172
SN - 1618-2642
VL - 397
SP - 765
EP - 776
JO - Analytical and Bioanalytical Chemistry
JF - Analytical and Bioanalytical Chemistry
IS - 2
ER -