Abstract
An inter-laboratory study was performed in eight laboratories to evaluate the simultaneous quantification method for HT-2 toxin (HT-2), T-2 toxin (T-2), diacetoxyscirpenol (DAS), neosolaniol (NES), 3-acetyldeoxynivalenol (3-AcDON), 15-acetyldeoxynivalenol (15-AcDON), deoxynivalenol (DON), deoxynivalenol-3-glucoside (D3G), nivalenol (NIV), and fusarenon-X (FUS-X) in feed. The mycotoxins in the samples were extracted with hydrous acetonitrile, purified using a multifunctional column (InertSep® VRA-3) and a phospholipid removal column (Hybrid SPE®-Phospholipid), and then quantified using liquid chromatography-tandem mass spectrometry (LC–MS/MS) with atmospheric pressure chemical ionisation mode. The mean recovery, repeatability, reproducibility, and Horwitz ratio from the inter-laboratory validation study were 99.8–109%, 3.1–9.8%, 4.3–9.8%, and 0.19–0.45, respectively, for type A trichothecenes (HT-2, T-2, DAS, and NES). Those values for type B trichothecenes (3-AcDON, 15-AcDON, DON, NIV, and FUS-X) were 89.9–116%, 3.4–9.1%, 5.6–14%, and 0.25–0.70, and the values for modified mycotoxin (D3G) were 78.2–96.7%, 3.5–6.4%, and 13–22%, respectively.
This is a preview of subscription content, log in via an institution to check access.
Similar content being viewed by others
Data availability
The datasets of the study are not publicly available due to restrictions. Data are however available from the corresponding author upon reasonable request, and with permission.
References
AOAC International (2019) Appendix D: guidelines for collaborative study procedures to validate characteristics of a method of analysis. In Official Methods of Analysis of AOAC Int. 21th ed. Gaithersburg, MD, USA
Berthiller F, Schuhmacher R, Buttinger G, Freudenschuss M, Adam G, Krska R (2003) Synthesis of deoxynivalenol-glucosides and their characterization using a QTrap LCMS/MS. Mycotoxin Res 19:47–50. https://doi.org/10.1007/BF02940092
Berthiller F, Krska R, Domigc KJ, Kneifeld W, Jugee N, Schuhmacher R, Adamf G (2011) Hydrolytic fate of deoxynivalenol-3-glucoside during digestion. Toxicol Lett 206:264–267. https://doi.org/10.1016/j.toxlet.2011.08.006
Bessaire T, Mujahid C, Mottier P, Desmarchelier A (2019) Multiple mycotoxins determination in food by LC-MS/MS: an international collaborative study. Toxins 11:658. https://doi.org/10.3390/toxins11110658
De Girolamo A, Ciasca B, Pascale M, Lattanzio VMT (2020) 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 12:786. https://doi.org/10.3390/toxins12120786,PMID33322050
Desjardins AE, Hohn TM, Mccormick SP (1993) Trichothecene biosynthesis in Fusarium species: chemistry, genetics, and significance. Microbiol Rev 57:595–604. https://doi.org/10.1128/mr.57.3.595-604.1993
European Committee for Standardization (2019) EN17280:2019 Foodstuffs – determination of zearalenone and trichothecenes including deoxynivalenol and its acetylated derivatives (3-acetyl-deoxynivalenol and 15-acetyl-deoxynivalenol), nivalenol, T-2 toxin and HT-2 toxin in cereals and cereal products by LC-MS/MS. European Committee for Standardization: Brussels, Belgium
European Food Safety Authority (EFSA) (2013) Deoxynivalenol in food and feed: occurrence and exposure European Food Safety Authority. EFSA J 11:3379
Food and Agricultural Materials Inspection Center (FAMIC) (1988) About regulation value of dietary harmful materials, regulation value of pesticides, heavy metals and mycotoxins (administrative guideline). Food and Agricultural Materials Inspection Center, Saitama, Japan. English version is available at: http://www.famic.go.jp/ffis/feed/r_safety/r_feeds_safety22.html#mycotoxins
Habler K, Rychlik M (2016) Multi-mycotoxin stable isotope dilution LC-MS/MS method for Fusarium toxins in cereals. Anal Bioanal Chem 408:307–317. https://doi.org/10.1007/s00216-015-9110-7,PMID26514672
Kim J, Kang H-J, Lee D-H, Lee Y-W, Yoshizawa T (1993) Natural occurrence of Fusarium mycotoxins (Trichothecenes and Zearalenone) in barley and corn in Korea. Appl Environ Microbiol 59:3798–3802. https://doi.org/10.1128/aem.59.11.3798-3802.1993
Kovalsky P, Kos G, Nährer K, Schwab C, Jenkins T, Schatzmayr G, Sulyok M, Krska R (2016) Co-occurrence of regulated, masked and emerging mycotoxins and secondary metabolites in finished feed and maize—an extensive survey. Toxins 8:363. https://doi.org/10.3390/toxins8120363
Nakagawa H, Naito S, Kitani Y, Ito Y, Aoyama Y, Koyama M, Hiejima Y, Nakamura K, Miyazaki H, Morita HI, Tamura M, Mochizuki N, Nakamura M, Seki Y, Kadokura H, Ikeda H, Horie- Ishiguro T, Saito Y, Tajima M, Shigemasu Y, Kasama K, Oguma Y, Sago Y, Goto T, Hirayae K (2014) Harmonized collaborative validation of a simultaneous and multiple determination method for nivalenol, deoxynivalenol, T-2 toxin, HT-2 toxin, and zearalenone in wheat and barley by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). J Anal Bioanal Tech S6:002
Nomura M, Shidara K, Yasuda I, Aoyama K, Takahashi A, Ishibashi T (2020) Development of a simultaneous quantification method for ten trichothecenes including deoxynivalenol-3-glucoside in feed. Mycotoxin Res 36:353–360. https://doi.org/10.1007/s12550-020-00401-z
Rychlik M, Humpf H-U, Marko D, Dänicke S, Mally A, Berthiller F, Klaffke H, Lorenz N (2014) Proposal of a comprehensive definition of modified and other forms of mycotoxins including “masked” mycotoxins. Mycotoxin Res 30:197–205. https://doi.org/10.1007/s12550-014-0203-5
Tanaka T, Hasegawa A, Sugiura Y (2003) Levels and pattern of contamination with trichothecenes in cereal grains and their risk assessment. Mycotoxins 53:119–121
Thompson M (2000) Recent trends in inter-laboratory precision at ppb and sub-ppb concentrations in relation to fitness for purpose criteria proficiency testing. Analyst 125:385–386. https://doi.org/10.1039/b000282h
Tittlemier SA, Brunkhorst J, Cramer B, DeRosa MC, Lattanzio VMT, Malone R, Maragos C, Stranska M, Sumarah MW (2021) Developments in mycotoxin analysis: an update for 2019–2020. World Mycotoxin J 14:3–26. https://doi.org/10.3920/WMJ2020.2664
Van der Lee T, Zhang H, Van Diepeningen A, Waalwijk C (2015) Biogeography of Fusarium graminearum species complex and chemotypes: a review. Food Additives and Contaminants Part A 32:453–460. https://doi.org/10.1080/19440049.2014.984244
Yazar S, Omuetag Z (2008) Fumonisins, trichothecenes and zearalenone in cereals. Int J Mol Sci 9:2062. https://doi.org/10.3390/ijms9112062
Yoshizawa T (2013) Thirty-five years of research on deoxynivalenol, a trichothecene mycotoxin: with special reference to its discovery and co-occurrence with nivalenol in Japan. Food Safety 1:12–31. https://doi.org/10.14252/foodsafetyfscj.2013002
Zhang K, Schaab M, Southwood G, Tor ER, Aston LS, Song W, Eitzer B, Majumdar S, Lapainis T, Mai H, Tran K, El- Demerdash A, Vega V, Cai Y, Wong JW, Krynitsky AJ, Begley TH (2017) A collaborative study: determination of mycotoxins in corn, peanut butter, and wheat flour using stable isotope dilution assay (SIDA) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). J Agric Food Chem 65:7138–7152. https://doi.org/10.1021/acs.jafc.6b04872
Zhao Z, Liu N, Yang L, Deng Y, Wang J, Song S, Lin S, Wu A, Zhou Z, Hou J (2015) Multi-mycotoxin analysis of animal feed and animal-derived food using LC-MS/MS system with timed and highly selective reaction monitoring. Anal Bioanal Chem 407:7359–7368. https://doi.org/10.1007/s00216-015-8898-5
Acknowledgements
We are grateful to the following collaborators and organisations for their participation in the inter-laboratory study: Seiichiro Iizuka, Tama Laboratory, Japan Food Research Laboratories (JFRL), Tokyo, Japan; Yu Katsunuma, Scientific Feeds Laboratory Center, Japan Scientific Feeds Association, Chiba, Japan; Manami Kobayashi, Global Application Development Center, Analytical & Measuring Instruments Division, Shimadzu Corporation, Kanagawa, Japan; Tadashi Kitta, Yokohama Laboratory, Japan Frozen Foods Inspection Corporation, Kanagawa, Japan; Tomonari Iida, Physics and Chemistry Inspection Unit, Institute for Food and Environmental Science, Tokyo Kenbikyo-In, Tokyo, Japan; Hiroshi Takeuchi, Hygiene Research Division, Mie Prefectural Institute of Public Health and Environment Research, Mie, Japan; Kozue Satou, Sendai Regional Center, Food and Agricultural Materials Inspection Center, Miyagi, Japan.
Author information
Authors and Affiliations
Corresponding author
Ethics declarations
Conflict of interest
The authors declare no competing interests.
Additional information
Publisher's Note
Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.
Rights and permissions
Springer Nature or its licensor (e.g. a society or other partner) holds exclusive rights to this article under a publishing agreement with the author(s) or other rightsholder(s); author self-archiving of the accepted manuscript version of this article is solely governed by the terms of such publishing agreement and applicable law.
About this article
Cite this article
Nomura, M., Shidara, K. & Yasuda, I. Inter-laboratory study on simultaneous quantification of ten trichothecenes in feed. Mycotoxin Res 39, 95–108 (2023). https://doi.org/10.1007/s12550-023-00476-4
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s12550-023-00476-4