Abstract
An analytical method for the simultaneous quantitation of ten trichothecenes of type A (HT-2 toxin, T-2 toxin, diacetoxyscirpenol, and neosolaniol) and type B (3-acetyldeoxynivalenol, 15-acetyldeoxynivalenol, deoxynivalenol, deoxynivalenol-3-glucoside, nivalenol, and fusarenon-X) in feed has been developed using liquid chromatography with tandem mass spectrometry. Mycotoxins extracted twice from samples using aqueous acetonitrile were purified using a multifunctional clean-up column, followed by a phospholipid removal column. Trichothecenes were analysed using liquid chromatography atmospheric pressure chemical ionization tandem mass spectrometry. The extraction efficiency of the mycotoxins and the repeatability of some were improved by repeated extractions. Ionization enhancement (signal enhancement) of some mycotoxins was improved by using the phospholipid removal column at the clean-up step. Spike and recovery tests of trichothecenes were conducted on maize, barley, soybean meal, rapeseed meal, and formula feeds (for starting broiler chicks, suckling pigs, and beef cattle). The mean recovery values were 70.6–119% with relative standard deviations < 17%. The limit of quantification and the limit of detection of our method were 20 and 6 μg/kg, respectively, for 3-acetyldeoxynivalenol and 15-acetyldeoxynivalenol; 10 and 3 μg/kg, respectively, for T-2 toxin, deoxynivalenol, and fusarenon-X; and 5 and 2 μg/kg, respectively, for nivalenol and the remaining mycotoxins.
Similar content being viewed by others
References
Berger U, Oehme M, Kuhn F (1999) Quantitative determination and structure elucidation of type A- and B- trichothecenes by HPLC/ ion trap multiple mass spectrometry. J Agr Food Chem 47:4240–4245
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
Berthiller F, Schuhmacher R, Buttinger G, Krska R (2005) Rapid simultaneous determination of major type A- and B-trichothecenes as well as zearalenone in maize by high performance liquid chromatography-tandem mass spectrometry. J Chromatogr A 1062:209–216
Berthiller F, Krska R, Domigc KJ, Kneifeld W, Jugee N, Schuhmacher R, Gerhard A (2011) Hydrolytic fate of deoxynivalenol-3-glucoside during digestion. Toxicol Lett 206:264–267
EC - European Commission (2006a) Commission Recommendation 2006/576/EC of 17 August 2006 on the presence of deoxynivalenol, zearalenone, ochratoxin A, T-2 and HT-2 and fumonisins in products intended for animal feeding. Off J Eur Union L229:7–9. Last consolidated version available from: https://eur-lex.europa.eu/LexUriServ/LexUriServ.do?uri=OJ:L:2006:229:0007:0009:EN:PDF
EC - European Commission (2006b) Commission regulation (EC) No 401/2006 of 23 February 2006 Laying down the methods of sampling and analysis for the official control of the levels of mycotoxins in foodstuffs. Off J Eur Union L70:12–34. Last consolidated version available from: https://fsvps.ru/fsvps-docs/ru/usefulinf/files/es401-2006.pdf
EC - European Commission (2013) Commission Recommendation 2013/165/EU of 27 March 2013 on the presence of T-2 and HT-2 toxin in cereals and cereal products. Off J Eur Union L91:12. Last consolidated version available from: https://eur-lex.europa.eu/legal-content/EN/TXT/PDF/?uri=CELEX:32013H0165
FDA - US Food and Drug Administration (2010) Guidance for industry and FDA: advisory levels for deoxynivalenol (DON) in finished wheat products for human consumption and grains and grain by- products used for animal feed. Available from: https://www.fda.gov/Food/GuidanceRegulation/GuidanceDocumentsRegulatoryInformation/ChemicalContaminantsMetalsNaturalToxinsPesticides/ucm120184.htm. Accessed 10 April 2017
JECFA - Joint FAO/WHO Expert Committee on Food Additives (2010) Seventy-second meeting, summary and conclusions (JECFA/72/SC). Last consolidated version available from: https://www.who.int/foodsafety/chem/summary72_rev.pdf
Milicevic D, Nesic K, Jaksic S (2015) Mycotoxin contamination of the food supply chain- implications for one health programme. Proc Food Sci 5:187–190
Numanoğlu E, Uygun U, Gökmen V, Köksel H (2011) Multiple-stage extraction strategy for the determination of deoxynivalenol in maize. Food Addit Contam 28:80–85
Rotter BA, Prelusky DB, Pestka JJ (1996) Toxicology of deoxynivalenol (vomitoxin). J Toxicol Environ Health 48:1–34
Tamura M, Nakagawa H, Uyama A, Mochizuki N (2014) Simultaneous trichothecenes analysis by LC-MS/MS with a pentafluorophenyl column. Food Hyg Safe Sci 55:19–24
Tanaka H, Takino M, Sugita-Konishi Y, Tanaka T, Toriba A, Hayakawa K (2009) Determination of nivalenol and deoxynivalenol by liquid chromatography/atmospheric pressure photoionization mass spectrometry. Rapid Commun Mass Spectrom 23:3119–3124
Turner NW, Subrahmanyam S, Piletsky SA (2009) Analytical methods for determination of mycotoxins: a review. Anal Chim Acta 632:168–180
Yazar S, Omuetag Z (2008) Fumonisins, trichothecenes and zearalenone in cereals. Int J Mol Sci 9:2062–2090
Yoshizawa T, Jin YZ (1995) Natural occurrence of acetylated derivatives of deoxynivalenol and nivalenol in wheat and barley in Japan. Food Addit Contam 12:689–694
Author information
Authors and Affiliations
Corresponding author
Ethics declarations
Conflict of interest
The authors declare that they have no conflict of interest.
Additional information
Publisher’s note
Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.
Electronic supplementary material
ESM 1
(PDF 426 kb)
Rights and permissions
About this article
Cite this article
Nomura, M., Shidara, K., Yasuda, I. et al. Development of a simultaneous quantification method for ten trichothecenes including deoxynivalenol-3-glucoside in feed. Mycotoxin Res 36, 353–360 (2020). https://doi.org/10.1007/s12550-020-00401-z
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s12550-020-00401-z