Abstract

A method based on the QuEChERS (quick, easy, cheap, effective, rugged, and safe) purification combined with ultrahigh performance liquid chromatography tandem mass spectrometry (UPLC–MS/MS), was optimized for the simultaneous quantification of 25 mycotoxins in cereals. Samples were extracted with a solution containing 80% acetonitrile and 0.1% formic acid, and purified with QuEChERS before being separated by a C18 column. The mass spectrometry was conducted by using positive electrospray ionization (ESI+) and multiple reaction monitoring (MRM) models. The method gave good linear relations with regression coefficients ranging from 0.9950 to 0.9999. The detection limits ranged from 0.03 to 15.0 µg·kg−1, and the average recovery at three different concentrations ranged from 60.2% to 115.8%, with relative standard deviations (RSD%) varying from 0.7% to 19.6% for the 25 mycotoxins. The method is simple, rapid, accurate, and an improvement compared with the existing methods published so far.

Highlights

  • Mycotoxins can be analyzed by various methods, including thin layer chromatography (TLC) [1], enzyme-linked immunosorbent assay [2], gas chromatography [3,4], and immunoaffinity column/high-performance liquid chromatography with fluorescence and diode array detection [5,6]

  • The specific determination of multiclass mycotoxins in cereals requires highly selective and sensitive techniques such as ultrahigh-performance liquid chromatography tandem mass spectrometry (UPLC–MS/MS) [7,8,9,10,11] and direct analysis in real time (DART) ionization coupled to anhigh-resolution mass spectrometer based on orbitrap technology [12]

  • The results showed that the response of fumonisins was 15 times higher when using methanol/water than when using acetonitrile/water, with an acceptable peak shape

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Summary

Introduction

Mycotoxins can be analyzed by various methods, including thin layer chromatography (TLC) [1], enzyme-linked immunosorbent assay [2], gas chromatography [3,4], and immunoaffinity column/high-performance liquid chromatography with fluorescence and diode array detection [5,6].The specific determination of multiclass mycotoxins in cereals requires highly selective and sensitive techniques such as ultrahigh-performance liquid chromatography tandem mass spectrometry (UPLC–MS/MS) [7,8,9,10,11] and direct analysis in real time (DART) ionization coupled to an (ultra)high-resolution mass spectrometer based on orbitrap technology (orbitrap MS) [12].Several methods have been developed to purify mycotoxins from crude samples such as solid-phase extraction (SPE) [13], immunoaffinity columns (IACs) [14], and MycoSep columns [15].A direct and simple method for the purification of multiple mycotoxins is challenging because of their diverse chemical structures and properties. Mycotoxins can be analyzed by various methods, including thin layer chromatography (TLC) [1], enzyme-linked immunosorbent assay [2], gas chromatography [3,4], and immunoaffinity column/high-performance liquid chromatography with fluorescence and diode array detection [5,6]. The most prominent feature of IACs is their low matrix effects, high selectivity, and increased rate of recovery. They present some drawbacks such as being too expensive and unsuitable for the determination of a large number of Toxins 2016, 8, 375; doi:10.3390/toxins8120375 www.mdpi.com/journal/toxins

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