PERIODATE-OXIDATION ANALYSIS OF CARBOHYDRATES .12. RAPID-DETERMINATION OF ALDEHYDES IN THE OXIDATION-PRODUCTS OF OLIGOGLYCOSIDES BY THE DITHIOACETAL METHOD

A rapid and convenient analysis for glycosidic linkages in oligoglycosides was developed by improving the ditbioacetal method. A sample (0.1-1 μmol) was oxidized with an aqueous or aqueous methanolic 0.05 M solution of sodium metaperiodate for 3 h at 50°C. An equivalent amount of silver nitrate was added and the mixture was evaporated to dryness. The residue was treated with a 2:1 (v/v) mixture of ethanethiol and trifluoroacetic acid for 10 min at 25°C, and subsequently trimethylsilylated with hexamethyldisilazane and trimethylchlorosilane for 30 min at 50°C. Gas chromatography of the product allowed the simultaneous determination of the conjugated aldehydes in the oxidation product with high reproducibility. The glycosidic linkages in various oligoglycosides were examined by this procedure. © 1979.