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Development and validation of a method based on a QuEChERS procedure and heart‐cutting GC‐MS for determination of five mycotoxins in cereal products
Author(s) -
Cunha Sara C.,
Fernandes José O.
Publication year - 2010
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200900695
Subject(s) - quechers , gas chromatography–mass spectrometry , chromatography , mycotoxin , gas chromatography , chemistry , mass spectrometry , environmental chemistry , pesticide , pesticide residue , biology , food science , agronomy
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 μg/kg) were achieved with good repeatability (from 9 to 21%). LOD ranged from 2 to 15 μg/kg and LOQ ranged from 5 to 50 μg/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.