Development and validation of a method based on a QuEChERS procedure and heart-cutting GC-MS for determination of five mycotoxins in cereal products.
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 microg/kg) were achieved with good repeatability (from 9 to 21%). LOD ranged from 2 to 15 microg/kg and LOQ ranged from 5 to 50 microg/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.
Cunha
Sara C
SC
REQUIMTE, Department of Bromatology, Faculty of Pharmacy, University of Porto, Porto, Portugal. sara.cunha@ff.up.pt
Fernandes
José O
JO
D002523:Edible Grain / Q000737:chemistry*; D005433:Flour / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000191:economics / Q000379:methods; D015394:Molecular Structure; D009183:Mycotoxins / Q000032:analysis* / Q000737:chemistry / Q000145:classification; D015203:Reproducibility of Results; D012449:Safety; D013997:Time Factors; D014255:Trichothecenes / Q000032:analysis / Q000138:chemical synthesis / Q000737:chemistry*; D015025:Zearalenone / Q000737:chemistry*
D009183:Mycotoxins; D014255:Trichothecenes; D015025:Zearalenone; C038405:nivalenol; C046760:15-acetyldeoxynivalenol; C007262:deoxynivalenol