Technical Abstract: While the most accurate method for analysis of sugars in biomass is based on gas chromatography of trimethylsilane or alditol acetate derivitives of sugars, the derivation method is time consuming and laborious. In comparison, sample preparation for sugar analysis using liquid chromatography is a simple water extraction procedure, however analysis of hydrolyzed biomass materials are either poorly resolved for some sugars or analysis times are long. High performance ion moderated partition (HPIMP) chromatography using a lead or calcium column does not give good resolution for some sugars present in enzyme or chemical hydrolysates of biomass. In addition, galacturonic acid (an indicator of pectin hydrolysis) is retained and not eluted by these columns. Since pectin is a major polysaccharide component in citrus waste, galacturonic acid analysis is of interest in our research and requires a separate analytical technique if a lead based HPMIP column is used for sugar analysis. High performance anion-exchange chromatography using a Dionex PA-1 column with pulsed-amperometric detection (PAD) provides a much better separation of mono and disaccharide sugars. A gradient method developed previously using post column addition was modified to reduce analysis time from 70 to 40 min and provide good resolution of arabinose, rhamnose, galactose, xylose, glucose, fructose, sucrose, cellobiose, galacturonic acid, and glucuronic acid in hydrolyzed citrus waste materials.