Development and validation of an UHPLC-MS/MS method for the determination of mycotoxins in grass silages

Cormac McElhinney, Pádraig O’Kiely, Chris Elliott, Martin Danaher*

*Corresponding author for this work

Research output: Contribution to journalArticle

12 Citations (Scopus)

Abstract

An ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) multi-mycotoxin analytical method was developed to simultaneously identify and quantify 20 mycotoxins in grass silages, inclusive of mycotoxins that are currently regulated in European Union feeds. Extraction of mycotoxins from dried grass silages was performed using of a modified QuEChERS extraction employing an acidified aqueous extraction (0.1 N HCl) with no further clean-up. Following chromatographic separation, analytes were detected using a fast polarity-switching MS/MS method that allowed both positive and negative ions to be analysed from a single injection, thus the reducing time and cost of analysis. The limits of detection and quantification ranged between 3 µg kg–1 DM (aflatoxin B1, beauvericin and enniatin A and A1) and 200 µg kg–1 DM (deoxynivalenol), and between 10 µg kg–1 DM (aflatoxin B1, beauvericin and enniatin A1) and 500 µg kg–1 DM (deoxynivalenol), respectively. Inter-assay accuracy and precision ranged between 90% and 107% and between 3.9% and 15.0% CV, respectively. The accuracy of the method was assessed through the application to a range of incurred samples in an inter-laboratory study.

Original languageEnglish
Pages (from-to)2101-2112
JournalFood Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment
Volume32
Issue number12
Early online date19 Oct 2015
DOIs
Publication statusPublished - 02 Dec 2015

Keywords

  • extraction
  • grass
  • mycotoxins
  • silage
  • UHPLC-MS/MS

ASJC Scopus subject areas

  • Food Science
  • Chemistry(all)
  • Toxicology
  • Public Health, Environmental and Occupational Health
  • Health, Toxicology and Mutagenesis

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