Multimycotoxin Analysis by LC-MS/MS in Cereal Food and Feed: Comparison of Different Approaches for Extraction, Purification, and Calibration
Abstract
Twelve different approaches commonly used forthe simultaneous LC tandem MS (MS/MS)determination of mycotoxins (deoxynivalenol,aflatoxins, ochratoxin A, T-2 and HT-2 toxins,fumonisins, and zearalenone) were tested in cerealsand feed materials. They comprised differentextraction solvents, types of cleanup [solid-phaseextraction, QuEChERS, and immunoaffinity (IMA)],and calibration approaches (external or matrixmatched).The percentage of mycotoxins withacceptable recovery, according to Regulation (EC)No. 401/2006, ranged from 9 to 100%. The approachgiving the highest percentage of acceptable resultswas selected and further tested for corn, rice, andfeed spiked at three different mycotoxin levels (low,medium, and high). The method is based onextraction with MeOH-water (70 + 30, v/v) andcleanup with two multiantibody IMA columns. Forcorn and rice spiked at low mycotoxin levels, asignificant matrix effect was observed and wascompensated by using 13C calibration. At highermycotoxin levels (medium and high), matrix effectswere negligible as no significant differences wereobserved for the majority of recovery resultscalculated by 13C calibration and external calibration.Although the proposed method still needsimprovement in terms of accuracy and, to a lesserextent, precision, it was successfully tested with fourproficiency tests in buckwheat, corn, rice, and feed,giving acceptable z-scores for 97% (34 out of 35) ofresults.
Autore Pugliese
Tutti gli autori
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M. Solfrizzo; L. Gambacorta; R. Bibi; M. Ciriaci ; A. Paoloni; I. Pecorelli
Titolo volume/Rivista
Journal of AOAC International
Anno di pubblicazione
2017
ISSN
1944-7922
ISBN
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