Development of a simultaneous quantification method for ten trichothecenes including deoxynivalenol-3-glucoside in feed

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ORIGINAL ARTICLE

Development of a simultaneous quantification method for ten trichothecenes including deoxynivalenol-3-glucoside in feed Masayo Nomura 1

&

Kenji Shidara 1 & Iyo Yasuda 2 & Koji Aoyama 1 & Akiko Takahashi 1 & Takayuki Ishibashi 1

Received: 15 December 2019 / Revised: 17 June 2020 / Accepted: 7 July 2020 # Society for Mycotoxin (Research Gesellschaft für Mykotoxinforschung e.V.) and Springer-Verlag GmbH Germany, part of Springer Nature 2020

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. Keywords Liquid chromatography-tandem mass spectrometry . Atmospheric pressure chemical ionization . Repeated extraction . Phospholipid removal

Introduction Some reports have indicated that toxicity is higher for type A than for type B trichothecenes (Rotter et al. 1996), but cases of type A contamination are less than those of type B. Natural contamination of cereals with the type B trichothecenes

Electronic supplementary material The online version of this article (https://doi.org/10.1007/s12550-020-00401-z) contains supplementary material, which is available to authorized users. * Masayo Nomura [email protected] 1

Food and Agricultural Materials Inspection Center, Saitama Shintoshin National Government Building, Kensato Building, Shintoshin 2-1, Chuo-Ku, Saitama-Shi, Saitama 330-9731, Japan

2

Sendai Regional Center, Food and Agricultural Materials Inspection Center, Sendai National Government Building III, 1-3-15, Gorin, Miyagino-Ku, Sendai-Shi, Miyagi 983-0842, Japan

deoxynivalenol (DON) and nivalenol (NIV) has been widely reported (Yazar and Omuetag 2008; Milicevic et