Quantitative analysis of mycotoxins in cereal foods by Collision Cell Fragmentation - High Resolution Mass Spectrometry: performances and comparison with triple stage quadrupole detection.
Résumé
A liquid chromatography - high resolution mass spectrometry (LC-HRMS) method for the simultaneous determination of aflatoxins (B1, B2, G1, G2), ochratoxin A, deoxynivalenol, zearalenone, T-2 and HT-2 toxins in wheat flour, barley flour and crisp bread has been developed. Data presented show the process of obtaining. Mycotoxin fragmentation patterns obtained by High Energy Collision Dissociation (HCD) have been investigated to obtain quantitative and confirmatory information (two characteristic masses per mycotoxin) using OrbitrapTM based high resolution mass spectrometry. LC-HRMS (full scan) detection carried out by HCD allowed to monitor the pseudo-molecular ion and an additional characteristic fragment (for each mycotoxin) with mass accuracy in the range 0.1 - 3.9 ppm, meeting the current European regulatory requirements for LC-MS confirmatory analysis. A sample preparation procedure based on polymeric solid phase extraction cartridges was applied, allowing recoveries higher than 74% for all tested toxins, with relative standard deviation lower than 13%. Detection limits in the range 0.5 - 3.4 µg/kg were obtained for all tested matrices. A critical comparison between the proposed method and a validated method based on triple quadrupole mass spectrometry showed similar performances in terms of detection limits, recoveries and repeatability, and matrix effects. Based on an efficient sample extraction and clean up, the LC-HCD-HRMS method developed herein represents a reliable and robust alternative tool for mycotoxin analysis in food matrices as compared to well established triple quadrupole based approaches.
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