Tomoyuki Kadota1,2, Makoto Kimura3, Satoshi Hirano1, O. Tajima1, Tomoyuki Nakajima4, Yoichi Kamata5, Yoshiko Sugita‐Konishi5
1Food Safety Assurance Center Kirin Group Office Co., Ltd. 1‐13‐5 Fukuura Kanazawa‐ku Yokohama 236‐0004 Japan
2United Graduate School of Veterinary Sciences Gifu University 1‐1 Yanagido Gifu City Gifu 501‐1193 Japan
3Plant & Microbial Metabolic Engineering Research Unit Discovery Research Institute (DRI) RIKEN ASI, 2‐1 Hirosawa Wako Saitama 351‐0198 Japan
4Research Team for Fusarium Head Blight Control National Agricultural Research Center for Kyushu Okinawa Region 2421 Suya, Koshi Kumamoto 861‐1192 Japan
5Division of Microbiology National Institute of Health Sciences 1‐18‐1 Kamiyouga Setagayaku Tokyo 158‐8501 Japan
Tóm tắt
A method coupling liquid chromatography with tandem mass spectrometry (LC/MS/MS) was developed for the simultaneous quantitative determination of trichothecenes, nivalenol, deoxynivalenol, deoxynivalenol‐3‐glucoside, fusarenon‐X, 3‐acetyldeoxynivalenol, 15‐acetyldeoxynivalenol, isotrichodermin, calonectrin, 3‐deacetylcalonectrin, 15‐deacetylcalonectrin, 3,15‐diacetylnivalenol, 4,15‐diacetylnivalenol, 3,15‐diacetyldeoxynivalenol, and 3,4,15‐triacetylnivalenol. The analytical parameters of trichothecenes and their derivatives were optimized to enable their highly sensitive detection. Evaluation of clean‐up procedures using Multisep #226 and #227 indicated that Multisep #227 was more suitable for their simultaneous detection in wheat. In performance validation studies using the LC/MS/MS method with Multisep #227 cleanup, good recoveries ranging from 84% to 115% with relative standard deviations from 0.4% to 7.2% were measured. The limits of detection and quantification ranged from 0.03 to 1.4 ng·g−1 and from 0.1 to 4.7 ng·g−1, respectively. The effect of matrices using matrix‐matched calibration was estimated to range from 80% to 117% after Multisep #227 cleanup. Multisep #227 clean‐up procedure with matrix‐free standard calibration achieved accurate quantification without having a considerable effect on matrix compounds. Using the developed method, several trichothecene derivatives and precursors were detected in fungally inoculated wheat samples. The developed LC/MS/MS method is a practical technique that can be used for the quantification of trichothecenes in wheat. This study is the first report of an analytical method used for the simultaneous quantification of major trichothecenes, their derivatives and precursors. Copyright © 2011 John Wiley & Sons, Ltd.
