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  • A method for simultaneous determination of 20 Fusarium toxins in cereals by high-resolution liquid chromatography-Orbitrap mass spectrometry with a pentafluorophenyl column.

A method for simultaneous determination of 20 Fusarium toxins in cereals by high-resolution liquid chromatography-Orbitrap mass spectrometry with a pentafluorophenyl column.

Toxins (2015-05-27)
Masayoshi Tamura, Naoki Mochizuki, Yasushi Nagatomi, Koichi Harayama, Akira Toriba, Kazuichi Hayakawa
ABSTRACT

A high-resolution liquid chromatography-Orbitrap mass spectrometry (LC-Orbitrap MS) method was developed for simultaneous determination of 20 Fusarium toxins (nivalenol, fusarenon-X, deoxynivalenol, 3-acetyl deoxynivalenol, 15-acetyl deoxynivalenol, HT-2 toxin, T-2 toxin, neosolaniol, diacetoxyscirpenol, fumonisin B1, fumonisin B2, fumonisin B3, fumonisin A1, fumonisin A2, fumonisin A3, zearalenone, α-zearalenol, β-zearalenol, α-zearalanol, and β-zearalanol) in cereals. The separation of 20 Fusarium toxins with good peak shapes was achieved using a pentafluorophenyl column, and Orbitrap MS was able to detect accurately from cereal matrix components within ±0.77 ppm. The samples were prepared using a QuEChERS kit for extraction and a multifunctional cartridge for purification. The linearity, repeatability, and recovery of the method were >0.9964, 0.8%-14.7%, and 71%-106%, respectively. Using this method, an analysis of 34 commercially available cereals detected the presence of deoxynivalenol, 15-acetyl deoxynivalenol, fumonisin B1, fumonisin B2, fumonisin B3, fumonisn A1, fumonisin A2, fumonisin A3, and zearalenone in corn samples with high concentration and frequency. Trichothecenes was detected from wheat samples with high frequency; in particular, the concentration of deoxynivalenol was high. Conversely, α-zearalenol, β-zearalenol, α-zearalanol, and β-zearalanol were not detected in any of the samples.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Acetic acid-12C2, 99.9 atom % 12C
Sigma-Aldrich
Acetic acid, for luminescence, BioUltra, ≥99.5% (GC)
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Acetic acid, natural, ≥99.5%, FG
Sigma-Aldrich
Acetic acid, ≥99.5%, FCC, FG
Sigma-Aldrich
3-Acetyldeoxynivalenol, from Fusarium roseum
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15-O-Acetyl-4-deoxynivalenol from Fusarium graminearum
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Ammonium acetate, reagent grade, ≥98%
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Ammonium acetate, 99.999% trace metals basis
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Methanol, NMR reference standard
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Methanol, anhydrous, 99.8%
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Ammonium acetate, BioXtra, ≥98%
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Ammonium acetate solution, for molecular biology, 7.5 M
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Acetonitrile, anhydrous, 99.8%
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5α-Androstan-17β-ol-3-one, purum, ≥99.0% (TLC)
Sigma-Aldrich
Deoxynivalenol
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Fumonisin B1 from Fusarium moniliforme, ≥98% (HPLC)
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5α-Androstan-17β-ol-3-one, ≥97.5%
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Acetonitrile, electronic grade, 99.999% trace metals basis
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