Cereal Chem 45:154 - 161.  |  VIEW ARTICLE
Gas Chromatography of Carbohydrates.

T. Cayle, F. Viebrock, and J. Schiaffino. Copyright 1968 by the American Association of Cereal Chemists, Inc. 

Conditions have been established for quantitatively determining the major carbohydrate components in starch syrups without the formation of the anomeric forms associated with the ordinary trimethylsilyl (TMS) derivatives. The carbohydrates, including an internal standard of ribose, are reduced with borohydride. Excess reagent is destroyed by HF, and the borate is removed by treatment with a mixed-bed ion-exchange resin, followed by distillation as methyl borate. The relatively insoluble reduced carbohydrates are dissolved in a mixture of dimethylsulfoxide and pyridine, and TMS derivatives are prepared with the conventional reagents, hexamethyldisilazane and trimethylchlorosilane. By controlling the relative concentration of reagents, intermediates are obtained within a single liquid phase, providing for easy handling of the sample. Reducing the total number of peaks obtainable from a mixture of carbohydrates allows for more precise quantitative evaluation of the data. This also allows for estimation of components having retention times similar to one of the anomeric pairs present as unreduced TMS derivative.