Development, in-house validation and application of a method using high-performance liquid chromatography with fluorescence detection (HPLC-FLD) for the quantification of 12 ergot alkaloids in compound feeds

1. Arroyo-Manzanares N., Rodríguez-Estévez V., García-Campaña A.M., Castellón-Rendón E., Gámiz-Gracia L.: Determination of principal ergot alkaloids in swine feeding. J Sci Food Agric 2021, 101, 5214–5224, doi: 10.1002/jsfa.11169. Arroyo-Manzanares N. Rodríguez-Estévez V. García-Campaña A.M. Castellón-Rendón E. Gámiz-Gracia L .: Determination of principal ergot alkaloids in swine feeding . J Sci Food Agric 2021 , 101 , 5214 – 5224 , doi: 10.1002/jsfa.11169 . Open DOISearch in Google Scholar

2. Babič J., Tavčar-Kalcher G., Celar F.A., Kos K., Červek M., Jakovac-Strajn B.: Ergot and Ergot Alkaloids in Cereal Grains Intended for Animal Feeding Collected in Slovenia: Occurrence, Pattern and Correlations. Toxins 2020, 12, 1–18, doi:10.3390/toxins12110730. Babič J. Tavčar-Kalcher G. Celar F.A. Kos K. Červek M. Jakovac-Strajn B .: Ergot and Ergot Alkaloids in Cereal Grains Intended for Animal Feeding Collected in Slovenia: Occurrence, Pattern and Correlations . Toxins 2020 , 12 , 1 – 18 , doi: 10.3390/toxins12110730 . Open DOISearch in Google Scholar

3. Bryła M., Ksieniewicz-Woźniak E., Podolska G., Waśkiewicz A., Szymczyk K., Jędrzejczak R.: Occurrence of ergot and its alkaloids in winter rye harvested in Poland. World Mycotoxin J 2018, 11, 635–646, doi: 10.3920/WMJ2018.2322. Bryła M. Ksieniewicz-Woźniak E. Podolska G. Waśkiewicz A. Szymczyk K. Jędrzejczak R .: Occurrence of ergot and its alkaloids in winter rye harvested in Poland . World Mycotoxin J 2018 , 11 , 635 – 646 , doi: 10.3920/WMJ2018.2322 . Open DOISearch in Google Scholar

4. Craig A.M., Klotz J.L., Duringer J.M.: Cases of ergotism in livestock and associated ergot alkaloid concentrations in feed. Front Chem 2015, 18, 3, 1–6, doi: 10.3389/fchem.2015.00008. Craig A.M. Klotz J.L. Duringer J.M .: Cases of ergotism in livestock and associated ergot alkaloid concentrations in feed . Front Chem 2015 , 18 , 3 , 1 – 6 , doi: 10.3389/fchem.2015.00008 . Open DOISearch in Google Scholar

5. Di Mavungu J.D., Malysheva S.V., Sanders M., Larionova D., Robbens J., Dubruel P., Van Peteghem C., De Saeger S.: Development and validation of a new LC–MS/MS method for the simultaneous determination of six major ergot alkaloids and their corresponding epimers. Application to some food and feed commodities. Food Chem 2012, 135, 292–303, doi:10.1016/j.foodchem.2012.04.098. Di Mavungu J.D. Malysheva S.V. Sanders M. Larionova D. Robbens J. Dubruel P. Van Peteghem C. De Saeger S .: Development and validation of a new LC–MS/MS method for the simultaneous determination of six major ergot alkaloids and their corresponding epimers . Application to some food and feed commodities . Food Chem 2012 , 135 , 292 – 303 , doi: 10.1016/j.foodchem.2012.04.098 . Open DOISearch in Google Scholar

6. Eurachem/Co-operation on International Traceability in Analytical Chemistry: Guide: CG 4 Quantifying Uncertainty in Analytical Measurement, Third Edition, edited by S.L.R. Ellison, A. Williams, Eurachem/CITAC, LGC, Teddington, 2012. Eurachem/Co-operation on International Traceability in Analytical Chemistry : Guide: CG 4 Quantifying Uncertainty in Analytical Measurement , Third Edition , edited by Ellison S.L.R. Williams A. , Eurachem/CITAC , LGC, Teddington , 2012 . Search in Google Scholar

7. European Commission: Commission Recommendation 2012/154/EU of 15 March 2012 on the monitoring of the presence of ergot alkaloids in feed and food. OJEU L 2012, 77, 55, 16/03/2012, 20–21, https://eur-lex.europa.eu/legal-content/EN/TXT/PDF/?uri=CELEX:32012H0154. European Commission : Commission Recommendation 2012/154/EU of 15 March 2012 on the monitoring of the presence of ergot alkaloids in feed and food . OJEU L 2012 , 77 , 55 , 16/03/2012, 20 – 21 , https://eur-lex.europa.eu/legal-content/EN/TXT/PDF/?uri=CELEX:32012H0154 . Search in Google Scholar

8. European Commission: Commission Implementing Regulation (EU) 2021/808 of 22 March 2021 on the performance of analytical methods for residues of pharmacologically active substances used in food-producing animals and on the interpretation of results as well as on the methods to be used for sampling and repealing Decisions 2002/657/EC and 98/179/EC. OJEU L 2021, 180, 64, 21/05/2021, 84–109, https://eur-lex.europa.eu/legal-content/EN/TXT/PDF/?uri=CELEX:32021R0808. European Commission : Commission Implementing Regulation (EU) 2021/808 of 22 March 2021 on the performance of analytical methods for residues of pharmacologically active substances used in food-producing animals and on the interpretation of results as well as on the methods to be used for sampling and repealing Decisions 2002/657/EC and 98/179/EC . OJEU L 2021 , 180 , 64, 21/05/2021, 84 – 109 , https://eur-lex.europa.eu/legal-content/EN/TXT/PDF/?uri=CELEX:32021R0808 . Search in Google Scholar

9. European Commission: Commission Regulation (EU) 2023/915 of 25 April 2023 on maximum levels for certain contaminants in food and repealing Regulation (EC) No 1881/2006. OJEU L 2023, 119, 66, 05/05/2023, 103–157, https://eur-lex.europa.eu/legal-content/EN/TXT/PDF/?uri=CELEX:32023R0915. European Commission : Commission Regulation (EU) 2023/915 of 25 April 2023 on maximum levels for certain contaminants in food and repealing Regulation (EC) No 1881/2006 . OJEU L 2023 , 119 , 66, 05/05/2023, 103 – 157 , https://eur-lex.europa.eu/legal-content/EN/TXT/PDF/?uri=CELEX:32023R0915 . Search in Google Scholar

10. European Food Safety Authority, Panel on Contaminants in the Food Chain (CONTAM), Alexander J., Benford D., Boobis A., Ceccatelli S., Cottrill B., Cravedi J.-P., Di Domenico A., Doerge D., Dogliotti E., Edler L., Farmer P., Filipič M., Fink-Gremmels J., Fürst P., Guérin T., Knutsen H.K., Machala M., Mutti A., Rose M., Schlatter J., van Leeuwen R.: Scientific Opinion on Ergot alkaloids in food and feed. EFSA J 2012, 10, 2798, 1–158, doi: 10.2903/j.efsa.2012.2798. European Food Safety Authority, Panel on Contaminants in the Food Chain (CONTAM) , Alexander J. Benford D. Boobis A. Ceccatelli S. Cottrill B. Cravedi J.-P. Di Domenico A. Doerge D. Dogliotti E. Edler L. Farmer P. Filipič M. Fink-Gremmels J. Fürst P. Guérin T. Knutsen H.K. Machala M. Mutti A. Rose M. Schlatter J. van Leeuwen R .: Scientific Opinion on Ergot alkaloids in food and feed . EFSA J 2012 , 10 , 2798 , 1 – 158 , doi: 10.2903/j.efsa.2012.2798 . Open DOISearch in Google Scholar

11. European Food Safety Authority, Arcella D., Gomez Ruiz J.A., Innocenti M.L., Roldan R.: Scientific report on human and animal dietary exposure to ergot alkaloids. EFSA J 2017, 15, 4902, 1–53, doi: 10.2903/j.efsa.2017.4902. European Food Safety Authority , Arcella D. Gomez Ruiz J.A. Innocenti M.L. Roldan R .: Scientific report on human and animal dietary exposure to ergot alkaloids . EFSA J 2017 , 15 , 4902 , 1 – 53 , doi: 10.2903/j.efsa.2017.4902 . Open DOISearch in Google Scholar

12. Holderied I., Rychlik M., Elsinghorst P.W.: Optimized Analysis of Ergot Alkaloids in Rye Products by Liquid Chromatography Fluorescence Detection Applying Lysergic Acid Diethylamide as an Internal Standard. Toxins 2019, 11, 1–9, doi:10.3390/toxins11040184. Holderied I. Rychlik M. Elsinghorst P.W .: Optimized Analysis of Ergot Alkaloids in Rye Products by Liquid Chromatography Fluorescence Detection Applying Lysergic Acid Diethylamide as an Internal Standard . Toxins 2019 , 11 , 1 – 9 , doi: 10.3390/toxins11040184 . Open DOISearch in Google Scholar

13. Kemboi D.C., Ochieng P.E., Antonissen G., Croubels S., Scippo M.L., Okoth S., Kangethe E.K., Faas J., Doupovec B., Lindahl J.F., Gathumbi J.K.: Multi-Mycotoxin Occurrence in Dairy Cattle and Poultry Feeds and Feed Ingredients from Machakos Town, Kenya. Toxins 2020, 12, 1–16, doi: 10.3390/toxins12120762. Kemboi D.C. Ochieng P.E. Antonissen G. Croubels S. Scippo M.L. Okoth S. Kangethe E.K. Faas J. Doupovec B. Lindahl J.F. Gathumbi J.K .: Multi-Mycotoxin Occurrence in Dairy Cattle and Poultry Feeds and Feed Ingredients from Machakos Town, Kenya . Toxins 2020 , 12 , 1 – 16 , doi: 10.3390/toxins12120762 . Open DOISearch in Google Scholar

14. Kokkonen M., Jestoi M.: Determination of ergot alkaloids from grains with UPLC-MS/MS. J Sep Sci 2010, 33, 2322–2327, doi: 10.1002/jssc.201000114. Kokkonen M. Jestoi M .: Determination of ergot alkaloids from grains with UPLC-MS/MS . J Sep Sci 2010 , 33 , 2322 – 2327 , doi: 10.1002/jssc.201000114 . Open DOISearch in Google Scholar

15. Krska R., Stubbings G., Macarthur R., Crews C.: Simultaneous determination of six major ergot alkaloids and their epimers in cereals and foodstuffs by LC-MS-MS. Anal Bioanal Chem 2008, 391, 563–576, doi: 10.1007/s00216-008-2036-6. Krska R. Stubbings G. Macarthur R. Crews C .: Simultaneous determination of six major ergot alkaloids and their epimers in cereals and foodstuffs by LC-MS-MS . Anal Bioanal Chem 2008 , 391 , 563 – 576 , doi: 10.1007/s00216-008-2036-6 . Open DOISearch in Google Scholar

16. Maruo V.M., Bracarense A.P., Metayer J.P., Vilarino M., Oswald I.P., Pinton P.: Ergot Alkaloids at Doses Close to EU Regulatory Limits Induce Alterations of the Liver and Intestine. Toxins (Basel) 2018, 10, 183, doi: 10.3390/toxins10050183. Maruo V.M. Bracarense A.P. Metayer J.P. Vilarino M. Oswald I.P. Pinton P .: Ergot Alkaloids at Doses Close to EU Regulatory Limits Induce Alterations of the Liver and Intestine . Toxins (Basel) 2018 , 10 , 183 , doi: 10.3390/toxins10050183 . Open DOISearch in Google Scholar

17. Mulder P.P.J., van Raamsdonk L.W.D., van Egmond H.J., Voogt J., van Brakel M.W., van der Horst G.M., de Jong J.: Dutch survey ergot alkaloids and sclerotia in animal feeds. 2012, RIKILT Report 2012.005. https://edepot.wur.nl/234699. Mulder P.P.J. van Raamsdonk L.W.D. van Egmond H.J. Voogt J. van Brakel M.W. van der Horst G.M. de Jong J .: Dutch survey ergot alkaloids and sclerotia in animal feeds . 2012 , RIKILT Report 2012.005 . https://edepot.wur.nl/234699 . Search in Google Scholar

18. Oellig C.: Lysergic acid amide as chemical marker for the total ergot alkaloids in rye flour – Determination by high-performance thin-layer chromatography–fluorescence detection. J Chromatogr A 2017, 1507, 124–131, doi: 10.1016/j.chroma.2017.05.043. Oellig C .: Lysergic acid amide as chemical marker for the total ergot alkaloids in rye flour – Determination by high-performance thin-layer chromatography–fluorescence detection . J Chromatogr A 2017 , 1507 , 124 – 131 , doi: 10.1016/j.chroma.2017.05.043 . Open DOISearch in Google Scholar

19. Poapolathep S., Klangkaew N., Zhang Z., Giorgi M., Logrieco A.F., Poapolathep A.: Simultaneous Determination of Ergot Alkaloids in Swine and Dairy Feeds Using Ultra High-Performance Liquid Chromatography-Tandem Mass Spectrometry. Toxins 2021, 13, 724, 1–11, doi: 10.3390/toxins13100724. Poapolathep S. Klangkaew N. Zhang Z. Giorgi M. Logrieco A.F. Poapolathep A .: Simultaneous Determination of Ergot Alkaloids in Swine and Dairy Feeds Using Ultra High-Performance Liquid Chromatography-Tandem Mass Spectrometry . Toxins 2021 , 13 , 724 , 1 – 11 , doi: 10.3390/toxins13100724 . Open DOISearch in Google Scholar

20. Schardl C.L.: Introduction to the Toxins Special Issue on Ergot Alkaloids. Toxins (Basel) 2015, 7, 4232–4237, doi:10.3390/toxins7104232. Schardl C.L .: Introduction to the Toxins Special Issue on Ergot Alkaloids . Toxins (Basel) 2015 , 7 , 4232 – 4237 , doi: 10.3390/toxins7104232 . Open DOISearch in Google Scholar

21. Schummer C., Brune L., Moris G.: Development of a UHPLC-FLD method for the analysis of ergot alkaloids and application to different types of cereals from Luxembourg. Mycotoxin Res 2018, 34, 279–287, doi: 10.1007/s12550-018-0322-5. Schummer C. Brune L. Moris G .: Development of a UHPLC-FLD method for the analysis of ergot alkaloids and application to different types of cereals from Luxembourg . Mycotoxin Res 2018 , 34 , 279 – 287 , doi: 10.1007/s12550-018-0322-5 . Open DOISearch in Google Scholar

22. Schummer C., Zandonella I., van Nieuwenhuyse A., Moris G.: Epimerization of ergot alkaloids in feed. Heliyon 2020, 6, 1–10, doi: 10.1016/j.heliyon.2020.e04336. Schummer C. Zandonella I. van Nieuwenhuyse A. Moris G .: Epimerization of ergot alkaloids in feed . Heliyon 2020 , 6 , 1 – 10 , doi: 10.1016/j.heliyon.2020.e04336 . Open DOISearch in Google Scholar

23. Waret-Szkuta A., Larraillet L., Oswald I.P., Legrand X., Guerre P., Martineau G.: Unusual acute neonatal mortality and sow agalactia linked with ergot alkaloid contamination of feed. Porc Health Manag 2019, 5, 1–5, doi: 10.1186/s40813-019-0131-z. Waret-Szkuta A. Larraillet L. Oswald I.P. Legrand X. Guerre P. Martineau G .: Unusual acute neonatal mortality and sow agalactia linked with ergot alkaloid contamination of feed . Porc Health Manag 2019 , 5 , 1 – 5 , doi: 10.1186/s40813-019-0131-z . Open DOISearch in Google Scholar