Multi-mycotoxin stable isotope dilution LC-MS/MS method for Fusarium toxins in cereals
Multi-mycotoxin stable isotope dilution LC-MS/MS method for Fusarium toxins in cereals
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谷物中镰刀菌毒素的多霉菌毒素稳定同位素稀释液相色谱 - 串联质谱法
DOI：
10.1007/s00216-015-9110-7
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发表时间：
2016-01-01
影响因子：
4.3
通讯作者：
Rychlik, Michael
中科院分区：
文献类型：
--
作者：
Habler, Katharina;Rychlik, Michael
建立了一种多真菌毒素稳定同位素稀释LC-MS/MS方法，对谷物中的14种镰刀菌毒素（脱氧雪腐镰刀菌醇、3-乙酰脱氧雪腐镰刀菌醇、15-乙酰脱氧雪腐镰刀菌醇、ht2毒素、t2毒素、enniatin B、enniatin B1、enniatin A1、enniatin A、beauvericin、fusarenone X、雪腐镰刀菌醇、脱氧雪腐镰刀菌醇-3-葡萄糖苷和玉米赤霉烯酮）进行检测。采用c -18水球柱对毒素进行了色谱分离，重点对脱氧雪腐镰刀菌醇和脱氧雪腐镰刀菌醇-3-葡萄糖苷进行了分离。建立了一种简便的样品制备方法，采用固相萃取法纯化毛霉烯与玉米赤霉烯酮、年生苷和beauvericin，并提供了良好的验证数据。线性、日内精密度、日内精密度和加样回收率分别为0.9982、1- 6%、5- 12%和79- 117%。通过对脱氧雪腐镰刀菌醇、ht2 -毒素、t2 -毒素标准品的分析，验证了方法的准确性，偏差小于7%。结果发现，2012年、2013年和2014年的大麦麦芽样品经常被高浓度的enniatin B、脱氧雪腐镰刀菌醇及其修饰的霉菌毒素脱氧雪腐镰刀菌醇-3-葡萄糖苷污染。2012年的样本受到的污染尤其严重。在所有分析样本中均未检测到Fusarenone X。
A multi-mycotoxin stable isotope dilution LC-MS/MS method was developed for 14 Fusarium toxins including modified mycotoxins in cereals (deoxynivalenol, 3-acetyldeoxynivalenol, 15-acetyldeoxynivalenol, HT2-toxin, T2-toxin, enniatin B, enniatin B1, enniatin A1, enniatin A, beauvericin, fusarenone X, nivalenol, deoxynivalenol-3-glucoside, and zearalenone). The chromatographic separation of the toxins with particular focus on deoxynivalenol and deoxynivalenol-3-glucoside was achieved using a C-18-hydrosphere column. An expedient sample preparation method was developed that uses solid-phase extraction for the purification of trichothecenes combined with zearalenone, enniatins, and beauvericin and provides excellent validation data. Linearity, intra-day precision, inter-day precision, and recoveries were >= 0.9982, 1-6 %, 5-12 %, and 79-117 %, respectively. Method accuracy was verified by analyzing certified reference materials for deoxynivalenol, HT2-toxin, and T2-toxin with deviations below 7 %. The results of this method found barley malt samples from 2012, 2013, and 2014 frequently contaminated with high concentrations of enniatin B, deoxynivalenol, and its modified mycotoxin deoxynivalenol-3-glucoside. Samples from 2012 were especially contaminated. Fusarenone X was not detected in any of the analyzed samples.