Oligosaccharide analysis is commonly done by acid hydrolysis and following HPLC analysis. A major problem is the incomplete hydrolysis of oligosaccharides and disaccharides and the increasing formation of volatile furfural from pentose monomers and hydroxymethylfurfural (HMF) from hexose monomers. This paper optimizes the conditions of hydrolysis approaches and proposes a method for oligosaccharide quantification. The optimal condition for hydrolysis of model xylan from corn cob was found to be for 100 °C hydrolysis temperature, 120 min hydrolysis time, and 2 wt% sulfuric acid concentration. Under these conditions, the total free and bound xylose yield was 77.4% and hemicellulose conversion 87.4% respectively; no degradation products were found. The optimal conditions for hydrolysis of model xylan from beech wood were found to be for 120 °C hydrolysis temperature, 120 min hydrolysis time, and 2 wt% sulfuric acid concentration. Under these conditions, the total free and bound xylose yield was 65.1% and hemicellulose conversion 70.5% respectively; no degradation products were found. For pentosan hydrolysate, conditions were further optimized (110 °C, 60 min, 2 wt% H2SO4). Standard addition of xylan from the corn cob for hydrolysation showed similar conversion rates (< 2% deviation); no matrix effects were detected.
