Determination of trichothecenes and zearalenones in grain cereal, flour and bread by liquid chromatography tandem mass spectrometry

Determination of trichothecenes and zearalenones in grain cereal, flour and bread by liquid chromatography tandem mass spectrometry
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DOI:
10.1016/j.foodchem.2012.04.051
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发表时间:
2012-10-15
期刊:
影响因子:
8.8
通讯作者:
Manes, Jordi
Manes, Jordi
中科院分区:
农林科学1区
文献类型:
--
作者:
Juan, Cristina;Ritieni, Alberto;Manes, Jordi

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虽然分析方法已经报道了立法真菌毒素,如单孢霉烯和玉米赤霉烯酮(ZON)分别,我们描述了一个简单,快速的多真菌毒素方法的优化,共12个真菌毒素,9个单孢霉烯,(NIV、DON、FUS-X、DAS、15-AcDON、3-AcDON、NEO、HT-2、T-2 T2)和玉米赤霉烯酮及其代谢物(ZON、α-ZOL、β-ZOL),不同来源(小麦、燕麦、大麦和斯佩耳特小麦)和三种不同的产品中可能存在这些物质(谷物、面粉和面包)进入食物链,对人类或动物造成毒性影响。提取程序是基于乙腈/水(84/16,v/v)的混合物,它提供了最高的回收率和最低的基质效应。以DON-d1为内标物,这有助于补偿在某些基质中观察到的显著基质效应,并在方法验证中获得高度成功,达到委员会决定2002/657/EC中汇编的参数。通过液相色谱-串联质谱法(LC-MS/MS)测定分析物。四种谷物中霉菌毒素的相对回收率均大于70%.获得了良好的线性(r(2)> 0.992),定量限(2.5-25纳克/克)低于欧洲监管水平。重复性,表示为相对标准偏差,总是低于11%,而日间精密度低于11%的开发方法。(C)2012爱思唯尔有限公司保留所有权利。
Although analytical methods have been already reported for legislated mycotoxins as trichothecenes and zearalenone (ZON) separately, we describe the optimization of a simple and rapid multimycotoxin method for the determination of a total of 12 mycotoxins simultaneously, nine trichothecenes (NIV, DON, FUS-X, DAS, 15-AcDON, 3-AcDON, NEO, HT-2, T-2 T2), and zearalenone and its metabolites (ZON, alpha-ZOL, beta-ZOL), of different origin (wheat, oat, barley and spelt) and in three different products where these substance can be present (grain, flour and bread) reach the food chain and cause toxic effect either in humans or animals. The extraction procedure was based on a mixture of acetonitrile/water (84/16, v/v), which provided the highest recoveries and the lowest matrix effect. DON-d1 was used as internal standard (IS.) which helped to compensate the significant matrix effect observed for some matrices, and to obtain high success in the method validation and to reach the parameters compiled in Commission Decision, 2002/657/EC. Analytes were determinate by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). Relative recoveries obtained were higher than 70% for the studied mycotoxins the four cereal. Good linearity (r(2) > 0.992) was obtained and quantification limits (2.5-25 ng/g) were below European regulatory levels. Repeatability, expressed as relative standard deviation, was always lower than 11%, whereas interday precision was lower than 11% for the developed method. (C) 2012 Elsevier Ltd. All rights reserved.