TECNICA MOLITORIA Vol. 70 - SEPTEMBER 2019
CONTENTS
52 - Multimycotoxin analysis by LC-MS/ MS in cereal food and feed: comparison of different approaches for extraction, purification and calibratio
L. Gambacorta - I. Pecorelli - R. Bibi - M. Ciriaci - A. Paoloni - M. Solfrizzo
Twelve approaches currently used for the simultaneous LCMS/ MS determination of the principal mycotoxins in cereal food and feed materials were tested. The method based on the extraction with methanol-water (70+30, v/v), clean-up with two multi-antibody immunoaffinity columns coupled in tandem was validated for corn, rice and feed spiked at low, medium and high levels of mycotoxins gave the best results. To study the matrix effect two types of calibration curves were prepared in pure solvent with and without the addition of 13C-labelled mycotoxin standards. For corn and rice spiked at low levels a significant matrix effect was observed and needed to be compensated by using calibration curves with 13C-labelled standards. At medium and high spiking levels no matrix effect was observed therefore mycotoxins were readily quantified by using external calibration curves. Although the LC-MS/MS method validated herein need some minor improvements it was successfully tested in four proficiency tests for the determination of the above mentioned mycotoxins in buckwheat, corn, rice and feed giving acceptable values of z-score for 97% of results.
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