Determination of methionine and selenomethionine in food matrices by gas chromatography mass spectrometry after aqueous derivatization with triethyloxonium salts

A novel analytical method for the simultaneous gas chromatography-mass spectrometry (GC-MS) determination of methionine and selenomethionine in food samples is described. Samples were digested with methanesulfonic acid in a closed vessel without the need for reflux. A single step derivatization using triethyloxonium tetrafluoroborate was optimized for the conversion of the analytes into their ethyl derivatives, followed by their extraction with hexane and GC-MS analysis.. This derivatization approach was simpler and/or safer with respect to current methods based on alkyl chloroformate or silylating reagents and it yielded very clean chromatography. A design of experiment approach, based on an open source chemometric software, was used to optimize the experimental conditions. When analysis of a 1 mL volume of aqueous standard was performed, detection limits of 1 ng/g methionine and 10 ng/g for selenomethionine were obtained.The method was validated by analysis of a selenized yeast Certified Reference Material NRC SELM-1.