Development and Validation of an LC-MS/MS Based Method for the Determination of Deoxynivalenol and Its Modified Forms in Maize
The Fusarium mycotoxin deoxynivalenol (DON) is a common contaminant of cereals and is often co-occurring with its modified forms DON-3-glucoside (D3G), 3-acetyl-DON (3ADON) or 15-acetyl-DON (15ADON). A stable-isotope dilution liquid chromatography-tandem mass spectrometry (LC-MS/MS) based method for...
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MDPI AG
2021-08-01
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| Series: | Toxins |
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| Online Access: | https://www.mdpi.com/2072-6651/13/9/600 |
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| author | Iris Fiby Marta Magdalena Sopel Herbert Michlmayr Gerhard Adam Franz Berthiller |
| author_facet | Iris Fiby Marta Magdalena Sopel Herbert Michlmayr Gerhard Adam Franz Berthiller |
| author_sort | Iris Fiby |
| collection | DOAJ |
| description | The Fusarium mycotoxin deoxynivalenol (DON) is a common contaminant of cereals and is often co-occurring with its modified forms DON-3-glucoside (D3G), 3-acetyl-DON (3ADON) or 15-acetyl-DON (15ADON). A stable-isotope dilution liquid chromatography-tandem mass spectrometry (LC-MS/MS) based method for their determination in cereals was developed and validated for maize. Therefore, <sup>13</sup>C-labelled D3G was enzymatically produced using <sup>13</sup>C-DON and [<sup>13</sup>C<sub>6</sub>Glc]-sucrose and used as an internal standard (IS) for D3G, while uniformly <sup>13</sup>C labelled IS was used for the other mycotoxins. Baseline separation was achieved for the critical peak pair DON/D3G, while 3ADON/15ADON could not be fully baseline separated after testing various reversed phase, fluorinated phase and chiral LC columns. After grinding, weighing and extracting the cereal samples, the raw extract was centrifuged and a mixture of the four <sup>13</sup>C-labelled ISs was added directly in a microinsert vial. The subsequent analytical run took 7 min, followed by negative electrospray ionization and selected reaction monitoring on a triple quadrupole MS. Maize was used as a complex cereal model matrix for validation. The use of the IS corrected the occurring matrix effects efficiently from 76 to 98% for D3G, from 86 to 103% for DON, from 68 to 100% for 15ADON and from 63 to 96% for 3ADON. |
| first_indexed | 2024-03-10T07:09:39Z |
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| institution | Directory Open Access Journal |
| issn | 2072-6651 |
| language | English |
| last_indexed | 2024-03-10T07:09:39Z |
| publishDate | 2021-08-01 |
| publisher | MDPI AG |
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| series | Toxins |
| spelling | doaj.art-6acef759dc8c450d8961e55479ef3ba62023-11-22T15:30:46ZengMDPI AGToxins2072-66512021-08-0113960010.3390/toxins13090600Development and Validation of an LC-MS/MS Based Method for the Determination of Deoxynivalenol and Its Modified Forms in MaizeIris Fiby0Marta Magdalena Sopel1Herbert Michlmayr2Gerhard Adam3Franz Berthiller4Institute of Bioanalytics and Agro-Metabolomics, Department of Agrobiotechnology (IFA-Tulln), University of Natural Resources and Life Sciences, Vienna (BOKU), Konrad Lorenz Str. 20, 3430 Tulln, AustriaInstitute of Bioanalytics and Agro-Metabolomics, Department of Agrobiotechnology (IFA-Tulln), University of Natural Resources and Life Sciences, Vienna (BOKU), Konrad Lorenz Str. 20, 3430 Tulln, AustriaInstitute of Microbial Genetics, Department of Applied Genetics and Cell Biology, BOKU, Konrad Lorenz Str. 24, 3430 Tulln, AustriaInstitute of Microbial Genetics, Department of Applied Genetics and Cell Biology, BOKU, Konrad Lorenz Str. 24, 3430 Tulln, AustriaInstitute of Bioanalytics and Agro-Metabolomics, Department of Agrobiotechnology (IFA-Tulln), University of Natural Resources and Life Sciences, Vienna (BOKU), Konrad Lorenz Str. 20, 3430 Tulln, AustriaThe Fusarium mycotoxin deoxynivalenol (DON) is a common contaminant of cereals and is often co-occurring with its modified forms DON-3-glucoside (D3G), 3-acetyl-DON (3ADON) or 15-acetyl-DON (15ADON). A stable-isotope dilution liquid chromatography-tandem mass spectrometry (LC-MS/MS) based method for their determination in cereals was developed and validated for maize. Therefore, <sup>13</sup>C-labelled D3G was enzymatically produced using <sup>13</sup>C-DON and [<sup>13</sup>C<sub>6</sub>Glc]-sucrose and used as an internal standard (IS) for D3G, while uniformly <sup>13</sup>C labelled IS was used for the other mycotoxins. Baseline separation was achieved for the critical peak pair DON/D3G, while 3ADON/15ADON could not be fully baseline separated after testing various reversed phase, fluorinated phase and chiral LC columns. After grinding, weighing and extracting the cereal samples, the raw extract was centrifuged and a mixture of the four <sup>13</sup>C-labelled ISs was added directly in a microinsert vial. The subsequent analytical run took 7 min, followed by negative electrospray ionization and selected reaction monitoring on a triple quadrupole MS. Maize was used as a complex cereal model matrix for validation. The use of the IS corrected the occurring matrix effects efficiently from 76 to 98% for D3G, from 86 to 103% for DON, from 68 to 100% for 15ADON and from 63 to 96% for 3ADON.https://www.mdpi.com/2072-6651/13/9/600mycotoxinstrichothecenesmasked mycotoxinsmodified mycotoxinsmass spectrometrystable-isotope dilution assay |
| spellingShingle | Iris Fiby Marta Magdalena Sopel Herbert Michlmayr Gerhard Adam Franz Berthiller Development and Validation of an LC-MS/MS Based Method for the Determination of Deoxynivalenol and Its Modified Forms in Maize Toxins mycotoxins trichothecenes masked mycotoxins modified mycotoxins mass spectrometry stable-isotope dilution assay |
| title | Development and Validation of an LC-MS/MS Based Method for the Determination of Deoxynivalenol and Its Modified Forms in Maize |
| title_full | Development and Validation of an LC-MS/MS Based Method for the Determination of Deoxynivalenol and Its Modified Forms in Maize |
| title_fullStr | Development and Validation of an LC-MS/MS Based Method for the Determination of Deoxynivalenol and Its Modified Forms in Maize |
| title_full_unstemmed | Development and Validation of an LC-MS/MS Based Method for the Determination of Deoxynivalenol and Its Modified Forms in Maize |
| title_short | Development and Validation of an LC-MS/MS Based Method for the Determination of Deoxynivalenol and Its Modified Forms in Maize |
| title_sort | development and validation of an lc ms ms based method for the determination of deoxynivalenol and its modified forms in maize |
| topic | mycotoxins trichothecenes masked mycotoxins modified mycotoxins mass spectrometry stable-isotope dilution assay |
| url | https://www.mdpi.com/2072-6651/13/9/600 |
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