Determination of monosaccharides by reaction gas chromatography/mass spectrometry with reagent removal from the reaction mixture

A method for determining monosaccharides has been developed, which involves their derivatization with N,O-bis-(trimethylsilyl)trifluoracetamide in the presence of pyridine in an ultrasonic field followed by the removal of the remaining derivatizing agent and pyridine and their substitution with methyl-tert-butyl ether (MTBE). Two peaks have been obtained in the chromatogram of D-galactose and D-fructose, corresponding to different forms of trimethylsilyl derivatives of D-galactose and D-fructose, respectively. For 1-O-octyl-β-D-glucopyranozide, one intense peak has been revealed in the chromatogram, which has been attributed to the trimethylsilyl derivative of 1-O-octyl-β-D-glucopyranozide. It has been demonstrated that, under the chosen conditions, the solutions of trimethylsilyl derivatives of the considered monosaccharides in MTBE are stable in the concentration range corresponding to the amount of monosaccharide from n × 10−10 to n × 10−8 g/μL for at least three days.