Direct analysis in real time (DART®) ionization coupled to an
(ultra)high resolution mass spectrometer based on orbitrap technology
(orbitrapMS) was used for rapid quantitative analysis of multiple
mycotoxins isolated from wheat and maize by modified QuEChERS
procedure. After initial evaluation of ionization efficiencies for
major groups of mycotoxins achievable with DART® technology, sample
preparation procedure and instrument parameter settings were optimized
to obtain sensitive and accurate determination of most intensively
ionizing toxins (deoxynivalenol, nivalenol, zearalenon,
actyldeoxynivalenol, deepoxy-deoxynivalenol, fusarenon-X, altenuene,
alternariol, alternariolmethylether, diacetoxyscirpenol,
sterigmatocystin). The lowest calibration levels (LCLs) estimated for
the respective analytes ranged from 50 to 150 [mu]g kg-1. Quantitative
analysis was performed either with the use of matrix-matched standards
or by employing commercially available 13C-labeled internal standards
(available for deoxynivalenol, nivalenol and zearalenon). Good
recoveries (100-108%) and repeatabilities (RSD 5.4-6.9%) were obtained
at spiking level 500 [mu]g kg-1 with isotope dilution technique. Based
on matrix-matched calibration, recoveries and repeatabilities were in
the range 84-118% and 7.9-12.0% (RSD), respectively. The trueness of
data obtained for deoxynivalenol and zearalenon in wheat/maize by DART®-
orbitrapMS was demonstrated by analysis of certified reference
materials (CRMs). Good agreement of these results with data generated
by validated ultra-high pressure liquid chromatography-time-of-flight
mass spectrometry method was documented.
(ultra)high resolution mass spectrometer based on orbitrap technology
(orbitrapMS) was used for rapid quantitative analysis of multiple
mycotoxins isolated from wheat and maize by modified QuEChERS
procedure. After initial evaluation of ionization efficiencies for
major groups of mycotoxins achievable with DART® technology, sample
preparation procedure and instrument parameter settings were optimized
to obtain sensitive and accurate determination of most intensively
ionizing toxins (deoxynivalenol, nivalenol, zearalenon,
actyldeoxynivalenol, deepoxy-deoxynivalenol, fusarenon-X, altenuene,
alternariol, alternariolmethylether, diacetoxyscirpenol,
sterigmatocystin). The lowest calibration levels (LCLs) estimated for
the respective analytes ranged from 50 to 150 [mu]g kg-1. Quantitative
analysis was performed either with the use of matrix-matched standards
or by employing commercially available 13C-labeled internal standards
(available for deoxynivalenol, nivalenol and zearalenon). Good
recoveries (100-108%) and repeatabilities (RSD 5.4-6.9%) were obtained
at spiking level 500 [mu]g kg-1 with isotope dilution technique. Based
on matrix-matched calibration, recoveries and repeatabilities were in
the range 84-118% and 7.9-12.0% (RSD), respectively. The trueness of
data obtained for deoxynivalenol and zearalenon in wheat/maize by DART®-
orbitrapMS was demonstrated by analysis of certified reference
materials (CRMs). Good agreement of these results with data generated
by validated ultra-high pressure liquid chromatography-time-of-flight
mass spectrometry method was documented.
