Skip to Content
Merck
  • Development and validation of an UHPLC-MS/MS method for the determination of mycotoxins in grass silages.

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

Food additives & contaminants. Part A, Chemistry, analysis, control, exposure & risk assessment (2015-09-17)
Cormac McElhinney, Pádraig O'Kiely, Chris Elliott, Martin Danaher
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.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Hydrochloric acid, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., fuming, ≥37%, APHA: ≤10
Sigma-Aldrich
Acetic acid, glacial, puriss., 99-100%
Sigma-Aldrich
Acetic acid, glacial, puriss., meets analytical specification of Ph. Eur., BP, USP, FCC, 99.8-100.5%
Sigma-Aldrich
Hydrogen chloride solution, 1.0 M in diethyl ether
Sigma-Aldrich
Hydrochloric acid, ACS reagent, 37%
Sigma-Aldrich
Hydrochloric acid, ACS reagent, 37%
Sigma-Aldrich
Acetic acid, glacial, ReagentPlus®, ≥99%
Sigma-Aldrich
Acetic acid, glacial, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8%
Sigma-Aldrich
Methanol, BioReagent, ≥99.93%
Sigma-Aldrich
Acetic acid solution, suitable for HPLC
Sigma-Aldrich
Ammonium acetate, ≥99.99% trace metals basis
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Hydrogen chloride solution, 1.0 M in acetic acid
Sigma-Aldrich
Acetic acid, glacial, ≥99.99% trace metals basis
Sigma-Aldrich
Hydrogen chloride solution, 4.0 M in dioxane
Sigma-Aldrich
Hydrochloric acid, 37 wt. % in H2O, 99.999% trace metals basis
Sigma-Aldrich
Sodium chloride, BioPerformance Certified, ≥99% (titration), suitable for insect cell culture, suitable for plant cell culture
Sigma-Aldrich
Methanol, NMR reference standard
Sigma-Aldrich
Sodium chloride solution, 0.85%
Sigma-Aldrich
Hydrochloric acid solution, 32 wt. % in H2O, FCC
Sigma-Aldrich
Ammonium acetate, BioXtra, ≥98%
Sigma-Aldrich
Ammonium acetate solution, for molecular biology, 7.5 M
Sigma-Aldrich
Sodium chloride solution, 5 M
Sigma-Aldrich
Sodium chloride solution, 5 M in H2O, BioReagent, for molecular biology, suitable for cell culture
Sigma-Aldrich
Zearalanone
Sigma-Aldrich
Mecamylamine hydrochloride
Sigma-Aldrich
Hydrochloric acid solution, 1.0 N, BioReagent, suitable for cell culture
Sigma-Aldrich
Aflatoxin B2
Sigma-Aldrich
Aflatoxin B1 from Aspergillus flavus, from Aspergillus flavus
Sigma-Aldrich
Sodium chloride, for molecular biology, DNase, RNase, and protease, none detected, ≥99% (titration)