title: Simultaneous determination of major type B trichothecenes and deoxynivalenol-3-glucoside in animal feed and raw materials using improved DSPE combined with LC-MS/MS.
abstract: A simple and reliable method for simultaneous determination of deoxynivalenol-3-glucoside and major type B trichothecenes (deoxynivalenol, nivalenol, fusarenon X, 3-acetyldeoxynivalenol, 15-acetyldeoxynivalenol and deepoxy-deoxynivalenol) in animal feed and raw materials has been developed and validated in this study. The method was based on an improved dispersive solid-phase extraction (DSPE) followed by analysis using high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS). Also, matrix-matched calibration curve (R(2)>0.99) was employed to minimize matrix effects and ensure accurate quantification. The recoveries during sample preparation process (including extraction and clean-up) ranged from 79.03% to 118.39%, with intra-day and inter-day relative standard deviation lower than 20% for all the analytes. The limit of quantification ranged from 5.0 μg/kg for deoxynivalenol to 13.6 μg/kg for fusarenon X. The validated method was successfully applied to the analysis of animal feed and corn. The pilot study showed that 37 out of 41 samples were contaminated with deoxynivalenol-3-glucoside at the levels of 6.0-121.0 μg/kg. Most of the type B trichothecenes were also found with the exception of fusarenon X, at the contaminated levels of 10.0-1,382 μg/kg. To the best of our knowledge, this was the first scientific report on the co-occurrence of masked deoxynivalenol and type B trichothecenes in animal feed and raw materials.
authors.affiliation: Institute for Agro-food Standards and Testing Technology, Laboratory of Quality & Safety Risk Assessment for Agro-products (Shanghai), Ministry of Agriculture, Shanghai Academy of Agricultural Sciences, 1000 Jinqi Road, Shanghai 201403, PR China; College of Veterinary Medicine, Nanjing Agricultural University, No. 1 Weigang Street, Nanjing, Jiangsu 210095, PR China.
authors.forename: Zhiyong
authors.initials: Z
authors.lastname: Zhao
authors.affiliation: Institute for Agro-food Standards and Testing Technology, Laboratory of Quality & Safety Risk Assessment for Agro-products (Shanghai), Ministry of Agriculture, Shanghai Academy of Agricultural Sciences, 1000 Jinqi Road, Shanghai 201403, PR China.
authors.forename: Qinxiong
authors.initials: Q
authors.lastname: Rao
authors.affiliation: Institute for Agro-food Standards and Testing Technology, Laboratory of Quality & Safety Risk Assessment for Agro-products (Shanghai), Ministry of Agriculture, Shanghai Academy of Agricultural Sciences, 1000 Jinqi Road, Shanghai 201403, PR China.
authors.forename: Suquan
authors.initials: S
authors.lastname: Song
authors.affiliation: Institute for Agro-food Standards and Testing Technology, Laboratory of Quality & Safety Risk Assessment for Agro-products (Shanghai), Ministry of Agriculture, Shanghai Academy of Agricultural Sciences, 1000 Jinqi Road, Shanghai 201403, PR China.
authors.forename: Na
authors.initials: N
authors.lastname: Liu
authors.affiliation: Institute for Agro-food Standards and Testing Technology, Laboratory of Quality & Safety Risk Assessment for Agro-products (Shanghai), Ministry of Agriculture, Shanghai Academy of Agricultural Sciences, 1000 Jinqi Road, Shanghai 201403, PR China.
authors.forename: Zheng
authors.initials: Z
authors.lastname: Han
authors.affiliation: College of Veterinary Medicine, Nanjing Agricultural University, No. 1 Weigang Street, Nanjing, Jiangsu 210095, PR China.
authors.forename: Jiafa
authors.initials: J
authors.lastname: Hou
authors.affiliation: Institute for Agro-food Standards and Testing Technology, Laboratory of Quality & Safety Risk Assessment for Agro-products (Shanghai), Ministry of Agriculture, Shanghai Academy of Agricultural Sciences, 1000 Jinqi Road, Shanghai 201403, PR China. Electronic address: wuaibo2007@yahoo.com.cn.
authors.forename: Aibo
authors.initials: A
authors.lastname: Wu
mesh_terms: D000821:Animal Feed / Q000032:analysis* / Q000382:microbiology; D000818:Animals; D002853:Chromatography, Liquid / Q000379:methods*; D005960:Glucosides / Q000032:analysis*; D057230:Limit of Detection; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods; D014255:Trichothecenes / Q000032:analysis*; D003313:Zea mays / Q000737:chemistry / Q000382:microbiology
chemical_list: D005960:Glucosides; D014255:Trichothecenes; C542050:deoxynivalenol-3-glucoside
keywords: Animal feed; Deoxynivalenol-3-glucoside; LC-MS/MS; Mycotoxin; Simultaneous determination; Type B trichothecenes