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
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
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改进的 DSPE 结合 LC-MS/MS 同时测定动物饲料和原料中的主要 B 型单端孢霉烯族化合物和脱氧雪腐镰刀菌烯醇-3-葡萄糖苷
DOI：
10.1016/j.jchromb.2014.05.053
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发表时间：
2014-07-15
影响因子：
3
通讯作者：
Wu, Aibo
中科院分区：
文献类型：
--
作者：
Zhao, Zhiyong;Rao, Qinxiong;Wu, Aibo
本研究建立了一种简单可靠的同时测定动物饲料和原料中脱氧雪腐镰刀菌醇-3-葡萄糖苷和主要B型毛霉烯（脱氧雪腐镰刀菌醇、雪腐镰刀菌醇、fusarenon X、3-乙酰脱氧雪腐镰刀菌醇、15-乙酰脱氧雪腐镰刀菌醇和深氧脱氧雪腐镰刀菌醇）含量的方法，并进行了验证。该方法采用改进的分散固相萃取（DSPE），然后采用高效液相色谱-串联质谱（HPLC-MS/MS）进行分析。此外，采用矩阵匹配校准曲线（R-2 > 0.199），以尽量减少矩阵效应，确保准确定量。样品制备过程（包括提取和清理）的回收率为79.03% ~ 118.39%，日内和日内相对标准偏差均小于20%。脱氧雪腐镰刀菌烯醇的定量限为5.0 μ g/kg ~ 13.6 μ g/kg。该方法可成功应用于动物饲料和玉米的定量分析。中试结果表明，41个样品中有37个样品被脱氧雪梨酚-3-葡萄糖苷污染，污染水平为6.0 ~ 121.0 μ g/kg。除fusarenon X外，其余均为B型毛孢烯，污染水平为10.0 ~ 1382 μ g/kg。据我们所知，这是第一个在动物饲料和原料中同时存在蒙面脱氧雪腐镰刀菌烯和B型毛霉烯的科学报告。(C) 2014 Elsevier B.V.版权所有
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 > 0.199) 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 mu g/kg for deoxynivalenol to 13.6 mu g/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 mu g/kg. Most of the type B trichothecenes were also found with the exception of fusarenon X, at the contaminated levels of 10.0-1382 mu g/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. (C) 2014 Elsevier B.V. All rights reserved.