A Multi-compound LC-MS/MS Method for the Screening of Mycotoxins in Grains

Abstract

A method development and its validation are described for determining 31 selected Aspergillus, Fusarium, Penicillium, and Claviceps mycotoxins in small grain cereals (wheat, barley, oats). The method comprises an automated solvent extraction step followed by filtering, concentrating, and the analysis of the crude extract with liquid chromatographic-tandem mass spectrometric determination. The analytes included trichothecenes, zearalenone, fumonisins, moniliformin, enniatins, beauvericin, antibiotic Y, aflatoxins, ochratoxin A, mycophenolic acid, penicillic acid, and ergot alkaloids. These were separated in two consecutive chromatographic runs, both involving negative and positive electrospray ionization modes of mass spectrometry. The validation showed that the method performance was good for (semi-)quantitative work, limits of quantification varying between 1 and 1,250 μg kg −1 , recoveries mostly between 51% and 122%, and repeatability being from 2% to 26% within day and from 14% to 28% between days (as relative standard deviation). A distinctive suppressive matrix effect, which depended on the analyte and the matrix, was observed but could be compensated for by using matrix-assisted standards. The developed multimycotoxin method permits simultaneous, simple, and rapid determination of several co-existing toxins and is ideal for, e.g., screening-type work or at concentration levels relevant in animal welfare.

Novel approaches in analysis of Fusarium mycotoxins in cereals employing ultra performance liquid chromatography coupled with high resolution mass spectrometry

“…Considering this difficulty, similarly to Kokkonen and Jestoy [9], we preferred as a compromise two chromatographic runs, each providing optimal detection conditions for target analytes. With regard to high retention factors of fumonisins in acidic mobile phase, even steeper gradient could be employed under routine conditions to reduce the total analysis time as much as possible.…”

“…LOD (g/kg) for analyte/matrix combination a Sulyok et al [13] Mol et al [11] Spanjer et al [12] Herebian et al [8] Herebian et al [8] Kokkonen and Jestoy [9] Frenich et al [14] Mavungu et al [ recent three years, several multi-mycotoxin methods for mycotoxin determination in foodstuffs have been developed [8][9][10][11][12][13][14]. The overview of their characteristics is summarized in Table 1.…”

Simultaneous determination of carbamate insecticides and mycotoxins in cereals by reversed phase liquid chromatography tandem mass spectrometry using a quick, easy, cheap, effective, rugged and safe extraction procedure

“…Therefore, a large number of multi-residue analytical methods have been established for the determination of carbamate insecticides and mycotoxins since the 1980s [6][7][8][9][10][11][12][13]. Especially in recent years, many liquid chromatography tandem mass spectrometry (LC-MS/MS) methods have been developed for simultaneous determination of multi-class mycotoxins in food [13][14][15][16][17][18][19][20][21][22][23].…”

Improved positive electrospray ionization of patulin by adduct formation: Usefulness in liquid chromatography–tandem mass spectrometry multi-mycotoxin analysis

“…The current method proved to be sensitive. Remarkably, the LODs of patulin (0.2 ng on column), zearalenone (0.2 ng), zearalanone (0.05 ng), neosolaniol (2 ng), HT-2 toxin (0.15 ng), deoxynivalenol (0.8 ng) and nivalenol (6 ng) in standard solution were 1.2 -100-fold lower than those of some methods [15,19,23,24]. Other studies, demonstrated, however, lower LODs for patulin (0.0125 ng on column) [25] and fumonisins (0.001-0.005 ng) [26].…”