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

Abstract

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 mg/kg) were achieved with good repeatability (from 9 to 21%). LOD ranged from 2 to 15 mg/kg and LOQ ranged from 5 to 50 mg/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.

A review of recent developments and trends in the QuEChERS sample preparation approach

“…Cunha and Fernandes developed and validated 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 heartcutting GC-MS [73]. Mycotoxins were extracted from the samples using a procedure based on the QuEChERS methodology with some modifications.…”

“…Mycotoxins were extracted from the samples using a procedure based on the QuEChERS methodology with some modifications. For cereals and other samples containing less than 25% of water, authors reduced the size of the sample to 5 g and the additional water (20 mL) before the extraction was added [73]. An additional improvement was the washing of the sample (two times with 5 mL of n-hexane) after its mechanical mixing (for about 15 min) [73].…”

“…For cereals and other samples containing less than 25% of water, authors reduced the size of the sample to 5 g and the additional water (20 mL) before the extraction was added [73]. An additional improvement was the washing of the sample (two times with 5 mL of n-hexane) after its mechanical mixing (for about 15 min) [73]. In this work, several types of d-SPE clean-up sorbents were tested, namely MgSO 4 , C18, PSA, Florisil and the mixture of MgSO 4 with C18 [73].…”

“…An additional improvement was the washing of the sample (two times with 5 mL of n-hexane) after its mechanical mixing (for about 15 min) [73]. In this work, several types of d-SPE clean-up sorbents were tested, namely MgSO 4 , C18, PSA, Florisil and the mixture of MgSO 4 with C18 [73]. PSA and Florisil were discarded due to low recoveries and clean-up efficiencies.…”

“…Among the other sorbents assayed the mixture of MgSO 4 and C18 was the best clean-up solution that allowed retaining interfering compounds without significant loss of studied analytes [73]. Cunha and Fernandes achieved acceptable recoveries from 67 to 101% and from 52 to 103% for nearly all mycotoxins in breakfast cereals and in flour, respectively, with good repeatability (from 9 to 21%) [73]. LOQ values (from 5 to 50 mg kg -1 ) were lower than the maximum limit established by EU [73].…”