Ethoximation-silylation approach for mono- and disaccharide analysis and characterization of their identification parameters by GC/MS.
The qualitative and quantitative analysis of complex carbohydrate mixtures is a challenging problem. When tackled by GC/MS, close retention times and largely similar mass spectra with no specific features complicate unambiguous identification, especially of monosaccharides. An optimized pre-capillary ethoximation-silylation GC/MS method for determination of monosaccharides and disaccharides was applied to a wide range of analytes (46 compounds). The two-step derivatization resulted in a pair of syn and anti peaks with specific retention and intensity ratio. The resulting dataset of mass spectra was subjected to a PCA-based pattern recognition. An oxime peak identifier (OPI) of the carbohydrate analytes, based on the combination of an internal standard and the corresponding syn/anti peak ratios, increased the reliability of the identification of reducing carbohydrates. Finally, the introduced EtOx-TMS derivatization method was applied to four different carbohydrate matrices (agave sirup, maple sirup, palm sugar, and honey).
University of Natural Resources and Life Sciences, Department of Chemistry, Division of Chemistry of Renewables and Christian-Doppler Laboratory "Advanced Cellulose Chemistry and Analytics", Muthgasse 18, A-1190 Vienna, Austria. Electronic address: manuel.becker@boku.ac.at.
M
M
Becker
F
F
Liebner
T
T
Rosenau
A
A
Potthast
D031002:Acer / Q000737:chemistry; D027882:Agave / Q000737:chemistry; D003059:Cocos / Q000737:chemistry; D004187:Disaccharides / Q000032:analysis* / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry; D006722:Honey / Q000032:analysis; D009005:Monosaccharides / Q000032:analysis* / Q000737:chemistry; D010091:Oximes / Q000737:chemistry*; D025341:Principal Component Analysis; D012015:Reference Standards; D012680:Sensitivity and Specificity; D012821:Silanes / Q000737:chemistry*
D004187:Disaccharides; D009005:Monosaccharides; D010091:Oximes; D012821:Silanes
Carbohydrates; Derivatization; Ethoximation; GC/MS; Retention index; Trimethylsilylation