Development and validation of a method based on a QuEChERS procedure and heart-cutting GC-MS for determination of five mycotoxins in cereal products
Development and validation of a method based on a QuEChERS procedure and heart-cutting GC-MS for determination of five mycotoxins in cereal products
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DOI：
10.1002/jssc.200900695
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发表时间：
2010-03-01
影响因子：
3.1
通讯作者：
Fernandes, Jose O.
中科院分区：
文献类型：
--
作者：
Cunha, Sara C.;Fernandes, Jose O.
建立了一种同时测定早餐谷物和面粉中5种真菌毒素(玉米赤霉烯酮、脱氧雪腐镰刀菌烯醇、赤霉烯X、15-乙酰脱氧雪腐镰刀菌烯醇和雪腐镰刀菌烯醇)的新方法。用MeCN进行提取，采用改进的QuEChERS(快速、简单、廉价、有效、坚固和安全)程序，在研究的分析物硅烷化后对提取物进行分析。对Deans开关装置和GC-MS的参数进行了仔细的优化，以便在SIM模式下实现快速分离，总运行时间仅为8分钟。在两个不同的添加水平(20和100微克/公斤)下，所有真菌毒素的回收率均可接受，重复性良好(从9%到21%)。LOD为2~15微克/公斤，LOQ为5~50微克/公斤。低于欧洲联盟(EU)规定的最高法定限值。开发的方法被应用于商业早餐谷物和面粉；在所研究的真菌毒素中，脱氧雪腐镰刀菌烯醇和玉米赤霉烯酮是最主要的。
A new analytical method for the rapid and simultaneous determination of five mycotoxins (zearelenone, deoxynivalenol, Fusarenon X, 15-acetyldeoxynivalenol and nivalenol) in breakfast cereals and flours by heart-cutting GC-MS has been developed and validated. Extraction was performed with MeCN, applying a modified QuEChERS (QUick, Easy, CHeap, Effective, Rugged and Safe) procedure, and the extracts were analyzed after a silylation of the analytes under study. Careful optimization of the parameters of Deans Switch device and GC-MS was achieved in order to attain a fast separation in SIM mode, allowing a total run time of only 8 min. Acceptable recoveries for all mycotoxins at two different spiking levels (20 and 100 mu g/kg) were achieved with good repeatability (from 9 to 21%). LOD ranged from 2 to 15 mu g/kg and LOQ ranged from 5 to 50 mu g/kg. which were lower than the maximum limit legal established by the European Union (EU). The method developed was applied to commercial breakfast cereals and flours; among the mycotoxins studied, deoxynivalenol and zearalenone were the most predominant.