The high molecular weight (HMW) material (> 12,000 Da) of ten raw cane sugars from seven countries and two U.S. states was isolated by dialysis and analyzed by gel permeation chromatography (GPC). Simultaneous detection of colorant polymers and polysaccharides was accomplished by using two detectors in series — UV at 214 nm for colorant polymers and refractive index (RI) for carbohydrate polymers. The monosaccharide composition of the nondialyzable raw sugar fraction (the tenate) was determined by hydrolysis with trifluoroacetic acid and with oxalic acid. Aconitic acid was associated with the tenate. The raw sugars were categorized into two types according to their GPC patterns and aconitic acid content. Hydrolysis of individually collected GPC peaks demonstrated that one particular peak contained most of the aconitic acid.