Abstract
A liquid chromatography-high-resolution mass spectrometry-based method is reported for the quantification of 20 selected mycotoxins and the simultaneous screening for 200 fungal metabolites in food. For regulated mycotoxins, such as aflatoxins, fumonisins, ochratoxin A, zearalenone and trichothecenes, the evaluation of the method performance characteristics, such as precision, trueness, limit of detection and matrix effects, has been exemplified for the matrix maize. In the case of the limit of detection, an alternative evaluation approach for high-resolution FT-Orbitrap data is proposed. Measurements of the signal-to-noise ratios obtained from ‘full-profile mode’ data led to detection limits between 8 and 160 ng g−1. Eight naturally contaminated wheat- and maize-based matrix test materials, originating from interlaboratory comparison studies, were used to confirm the trueness of the method for deoxynivalenol, zearalenone, fumonisin B1 and B2, HT-2, and T-2 toxin. In addition to accurate quantification of the most relevant mycotoxins, the full-scan chromatograms were used to investigate the potential of the FT-Orbitrap to screen simultaneously for a large number of fungal metabolites. First, a list of 200 metabolites, potentially being present in food samples, was established. Next, specific detection and identification criteria were defined, which are based on accurate mass, peak intensity and isotopologue ratio. The application of these criteria to the suspected metabolites from the list resulted in the putative identification of 13 fungal metabolites in addition to the target toxins.
Highlights
In our work we present the successful application of an alternative approach for the estimation of limit of detection (LOD) values which is based ie on “full profile mode” LC-MS chromatograms that can be used in case of FT-Orbitrap instruments
Alternariol, mycophenolic acid (MPA) and tentoxin were purchased from SigmaAldrich (Vienna, Austria)
Concentration values for the LODs obtained by this procedure were a factor three to four higher compared to the values achieved ee according to Harris (2006) and are given in Table 2 (LODsolvent) and Table 3 (LODmatrix)
Summary
Mycotoxins are fungal secondary metabolites, produced by various mold species. By definition, they are toxic to vertebrates and other animal groups in low concentrations (Bennet and Klich, 2003). New generations of high-resolution mass spectrometers, such as time-of-flight (TOF), fourier-transformation-ion-cyclotron resonance (FT-ICR) and FT-Orbitrap instruments are promising alternatives for the simultaneous analysis of multiple compounds. Their particular strength lies in their high mass resolving power and high mass accuracy. Retrospective analysis of full scan data makes it possible to assess virtually all compounds present in a sample This makes liquid chromatography – high-resolution ie. LC-HR-MS using FT-Orbitrap instruments in full scan mode has been ie successfully used for the (semi-)quantitative determination of e.g. small molecules in w biological samples (Zhang et al, 2009), veterinary drugs in food matrices In our work we present the successful application of an alternative approach for the estimation of LOD values which is based ie on “full profile mode” LC-MS chromatograms that can be used in case of FT-Orbitrap instruments
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