A Rapid Determination of Ergosterol in Grains Using Gas Chromatography–Mass Spectrometry Method Without Derivatization
2015
Zakir Hossain, Md. | Goto, Tetsuhisa
A simple, rapid and sensitive GC-MS method using on-column injection was developed and validated to determine ergosterol (ERG) levels in maize and wheat. In this method, ERG was extracted from grains with methanol and partitioned into hexane. The hexane layer was then directly injected onto the on-column GC-MS injection system without column-clean up or derivatization. Optimization of different GC-MS parameters was evaluated to obtain maximum sensitivity. Matrix-matched calibration curves were constructed to compensate for matrix effects in both matrices. Good recoveries in maize (98–110 %) and wheat (96–110 %) samples were obtained at three spiking levels (1, 3, and 8 mg/kg), with relative standard deviations less than 8 % in maize and 7 % in wheat. The limits of detection and quantification of ERG were less than 40 μg/kg and 200 μg/kg of grain sample, respectively. The method was successfully applied to 37 marketed grains, with ERG concentrations ranging from 1.0 to 14.4 mg/kg. Moreover, GC-MS analyses data were compared with an HPLC method, and no significant difference was observed. This new GC-MS method is quick and reliable for routine analysis of ERG to monitor fungal invasion and possible mycotoxin contamination in grains.
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