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Original Articles

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

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Pages 2101-2112 | Received 28 Apr 2015, Accepted 07 Sep 2015, Published online: 19 Oct 2015
 

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.

Graphical Abstract

Acknowledgements

Authors would like to acknowledge Jeroen Walravens (Ghent University, Belgium) for facilitating the inter-laboratory study; Dr John O’Mahony for guidance on UHPLC-MS/MS method development; and Teagasc Ashtown laboratory staff for assistance with the analysis.

Additional information

Funding

This work was supported by the Walsh Fellowship programme [grant number RMIS 6087].

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