Evaluation of different derivatisation approaches for gas chromatographic–mass spectrometric analysis of carbohydrates in complex matrices of biological and synthetic origin

摘要: Abstract Gas chromatographic analysis of complex carbohydrate mixtures requires highly effective and reliable derivatisation strategies for successful separation, identification, quantitation all constituents. Different single-step (per-trimethylsilylation, isopropylidenation) two-step approaches (ethoximation–trimethylsilylation, ethoximation–trifluoroacetylation, benzoximation–trimethylsilylation, benzoximation–trifluoroacetylation) have been comprehensively studied with regard to characteristics, informational value mass spectra, ease peak assignment, robustness toward matrix effects, using a set reference compounds that comprise eight monosaccharides (C 5 –C 6 ), glycolaldehyde, dihydroxyacetone. It has shown isopropylidenation the two oximation-trifluoroacetylation are least suitable matrices. Whereas former is limited contain vicinal dihydroxy moieties in cis configuration, latter methods sensitive traces trifluoroacetic acid which strongly supports decomposition ketohexoses. demonstrated “real” carbohydrate-rich matrices biological synthetic origin, respectively, ethoximation–trimethylsilylation superior other due low number peaks obtained per carbohydrate, good separation performance, structural information limits detection quantitation, minor relative standard deviations, sensitivity effects.