Development and validation of a method based on a QuEChERS procedure and heart-cutting GC-MS for determination of five mycotoxins in cereal products

被引:121
作者
Cunha, Sara C. [1 ]
Fernandes, Jose O. [1 ]
机构
[1] Univ Porto, Dept Bromatol, Fac Pharm, REQUIMTE, P-4099030 Oporto, Portugal
关键词
Deans Switch; Deoxynivalenol (DON); Heart-cutting GC-MS; QuEChERS; Trichothecenes; Zearelenone (ZON); CHROMATOGRAPHY-MASS SPECTROMETRY; GAS-CHROMATOGRAPHY; BREAKFAST CEREALS; TRICHOTHECENES; DEOXYNIVALENOL; ZEARALENONE; IDENTIFICATION; TOXINS; WHEAT;
D O I
10.1002/jssc.200900695
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
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.
引用
收藏
页码:600 / 609
页数:10
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