Determination of Zearalenone and Trichothecenes, Including Deoxynivalenol and Its Acetylated Derivatives, Nivalenol, T-2 and HT-2 Toxins, in Wheat and Wheat Products by LC-MS/MS: A Collaborative Study
An analytical method for the simultaneous determination of trichothecenes—namely, nivalenol (NIV), deoxynivalenol (DON) and its acetylated derivatives (3- and 15-acetyl-DON), T-2 and HT-2 toxins—and zearalenone (ZEN) in wheat, wheat flour, and wheat crackers was validated through a collaborative stu...
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| Format: | Article |
| Language: | English |
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MDPI AG
2020-12-01
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| Series: | Toxins |
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| Online Access: | https://www.mdpi.com/2072-6651/12/12/786 |
| _version_ | 1827700341139832832 |
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| author | Annalisa De Girolamo Biancamaria Ciasca Michelangelo Pascale Veronica M.T. Lattanzio |
| author_facet | Annalisa De Girolamo Biancamaria Ciasca Michelangelo Pascale Veronica M.T. Lattanzio |
| author_sort | Annalisa De Girolamo |
| collection | DOAJ |
| description | An analytical method for the simultaneous determination of trichothecenes—namely, nivalenol (NIV), deoxynivalenol (DON) and its acetylated derivatives (3- and 15-acetyl-DON), T-2 and HT-2 toxins—and zearalenone (ZEN) in wheat, wheat flour, and wheat crackers was validated through a collaborative study involving 15 participants from 10 countries. The validation study, performed within the M/520 standardization mandate of the European Commission, was carried out according to the IUPAC (International Union of Pure and Applied Chemistry) International Harmonized Protocol. The method was based on mycotoxin extraction from the homogenized sample material with a mixture of acetonitrile-water followed by purification and concentration on a solid phase extraction column. High-performance liquid chromatography coupled with tandem mass spectrometry was used for mycotoxin detection, using isotopically labelled mycotoxins as internal standards. The tested contamination ranges were from 27.7 to 378 μg/kg for NIV, from 234 to 2420 μg/kg for DON, from 18.5 to 137 μg/kg for 3-acetyl-DON, from 11.4 to 142 μg/kg for 15-acetyl-DON, from 2.1 to 37.6 μg/kg for T-2 toxin, from 6.6 to 134 μg/kg for HT-2 toxin, and from 31.6 to 230 μg/kg for ZEN. Recoveries were in the range 71–97% with the lowest values for NIV, the most polar mycotoxin. The relative standard deviation for repeatability (RSD<sub>r</sub>) was in the range of 2.2–34%, while the relative standard deviation for reproducibility (RSD<sub>R</sub>) was between 6.4% and 45%. The HorRat values ranged from 0.4 to 2.0. The results of the collaborative study showed that the candidate method is fit for the purpose of enforcing the legislative limits of the major <i>Fusarium</i> toxins in wheat and wheat-based products. |
| first_indexed | 2024-03-10T14:09:53Z |
| format | Article |
| id | doaj.art-927beef291754e88b24b20f4f13bf8fb |
| institution | Directory Open Access Journal |
| issn | 2072-6651 |
| language | English |
| last_indexed | 2024-03-10T14:09:53Z |
| publishDate | 2020-12-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Toxins |
| spelling | doaj.art-927beef291754e88b24b20f4f13bf8fb2023-11-21T00:16:54ZengMDPI AGToxins2072-66512020-12-01121278610.3390/toxins12120786Determination of Zearalenone and Trichothecenes, Including Deoxynivalenol and Its Acetylated Derivatives, Nivalenol, T-2 and HT-2 Toxins, in Wheat and Wheat Products by LC-MS/MS: A Collaborative StudyAnnalisa De Girolamo0Biancamaria Ciasca1Michelangelo Pascale2Veronica M.T. Lattanzio3Institute of Sciences of Food Production, National Research Council of Italy, via Amendola 122/O, 70126 Bari, ItalyInstitute of Sciences of Food Production, National Research Council of Italy, via Amendola 122/O, 70126 Bari, ItalyInstitute of Sciences of Food Production, National Research Council of Italy, via Amendola 122/O, 70126 Bari, ItalyInstitute of Sciences of Food Production, National Research Council of Italy, via Amendola 122/O, 70126 Bari, ItalyAn analytical method for the simultaneous determination of trichothecenes—namely, nivalenol (NIV), deoxynivalenol (DON) and its acetylated derivatives (3- and 15-acetyl-DON), T-2 and HT-2 toxins—and zearalenone (ZEN) in wheat, wheat flour, and wheat crackers was validated through a collaborative study involving 15 participants from 10 countries. The validation study, performed within the M/520 standardization mandate of the European Commission, was carried out according to the IUPAC (International Union of Pure and Applied Chemistry) International Harmonized Protocol. The method was based on mycotoxin extraction from the homogenized sample material with a mixture of acetonitrile-water followed by purification and concentration on a solid phase extraction column. High-performance liquid chromatography coupled with tandem mass spectrometry was used for mycotoxin detection, using isotopically labelled mycotoxins as internal standards. The tested contamination ranges were from 27.7 to 378 μg/kg for NIV, from 234 to 2420 μg/kg for DON, from 18.5 to 137 μg/kg for 3-acetyl-DON, from 11.4 to 142 μg/kg for 15-acetyl-DON, from 2.1 to 37.6 μg/kg for T-2 toxin, from 6.6 to 134 μg/kg for HT-2 toxin, and from 31.6 to 230 μg/kg for ZEN. Recoveries were in the range 71–97% with the lowest values for NIV, the most polar mycotoxin. The relative standard deviation for repeatability (RSD<sub>r</sub>) was in the range of 2.2–34%, while the relative standard deviation for reproducibility (RSD<sub>R</sub>) was between 6.4% and 45%. The HorRat values ranged from 0.4 to 2.0. The results of the collaborative study showed that the candidate method is fit for the purpose of enforcing the legislative limits of the major <i>Fusarium</i> toxins in wheat and wheat-based products.https://www.mdpi.com/2072-6651/12/12/786trichotheceneszearalenone<i>Fusarium</i> toxinswheatliquid chromatography–mass spectrometryofficial control |
| spellingShingle | Annalisa De Girolamo Biancamaria Ciasca Michelangelo Pascale Veronica M.T. Lattanzio Determination of Zearalenone and Trichothecenes, Including Deoxynivalenol and Its Acetylated Derivatives, Nivalenol, T-2 and HT-2 Toxins, in Wheat and Wheat Products by LC-MS/MS: A Collaborative Study Toxins trichothecenes zearalenone <i>Fusarium</i> toxins wheat liquid chromatography–mass spectrometry official control |
| title | Determination of Zearalenone and Trichothecenes, Including Deoxynivalenol and Its Acetylated Derivatives, Nivalenol, T-2 and HT-2 Toxins, in Wheat and Wheat Products by LC-MS/MS: A Collaborative Study |
| title_full | Determination of Zearalenone and Trichothecenes, Including Deoxynivalenol and Its Acetylated Derivatives, Nivalenol, T-2 and HT-2 Toxins, in Wheat and Wheat Products by LC-MS/MS: A Collaborative Study |
| title_fullStr | Determination of Zearalenone and Trichothecenes, Including Deoxynivalenol and Its Acetylated Derivatives, Nivalenol, T-2 and HT-2 Toxins, in Wheat and Wheat Products by LC-MS/MS: A Collaborative Study |
| title_full_unstemmed | Determination of Zearalenone and Trichothecenes, Including Deoxynivalenol and Its Acetylated Derivatives, Nivalenol, T-2 and HT-2 Toxins, in Wheat and Wheat Products by LC-MS/MS: A Collaborative Study |
| title_short | Determination of Zearalenone and Trichothecenes, Including Deoxynivalenol and Its Acetylated Derivatives, Nivalenol, T-2 and HT-2 Toxins, in Wheat and Wheat Products by LC-MS/MS: A Collaborative Study |
| title_sort | determination of zearalenone and trichothecenes including deoxynivalenol and its acetylated derivatives nivalenol t 2 and ht 2 toxins in wheat and wheat products by lc ms ms a collaborative study |
| topic | trichothecenes zearalenone <i>Fusarium</i> toxins wheat liquid chromatography–mass spectrometry official control |
| url | https://www.mdpi.com/2072-6651/12/12/786 |
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