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

• Published in: Analytical and bioanalytical chemistry Vol. 397; no. 2; pp. 765 - 776
• Main Authors: Rasmussen, R. R, Storm, I. M. L. D, Rasmussen, P. H, Smedsgaard, J, Nielsen, K. F
• Format: Journal Article
• Language: English
• Published: Berlin/Heidelberg Berlin/Heidelberg : Springer-Verlag 01.05.2010; Springer-Verlag; Springer
• Subjects: Analytical Chemistry; Biochemistry; Characterization and Evaluation of Materials; Chemistry; Chemistry and Materials Science; Chromatographic methods and physical methods associated with chromatography; Chromatography, Liquid - methods; Corn; Exact sciences and technology; Food Science; Health aspects; Laboratory Medicine; Limit of Detection; Maize; Mathematical analysis; Monitoring/Environmental Analysis; Mycoses; Mycotoxins - analysis; Original Paper; Other chromatographic methods; Pesticides; Plant metabolites; Silage; Silage - analysis; Spectrometric and optical methods; Tandem Mass Spectrometry - methods; Zea mays; Zea mays - chemistry; Validation; LC-MS/MS; Maize; Silage; Mycotoxins; QuEChERS; Mycotoxin; Laboratory; Calibration standards; Sample preparation; Detection limit; pH; Extraction; Secondary metabolism; Ether; Sample; Use; Pesticides; Liquid chromatography; Foodstuff; Infection; Toxin; Repeatability; Analysis method; Reproducibility; Residue; Mass spectrometry MS/MS; Mass spectrometry; Contaminant
• ISSN: 1618-2642; 1618-2650
• DOI: 10.1007/s00216-010-3545-7

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. [graphic removed]