Sulfation of sucrose with pyridine-sulfur trioxide was carried out in dimethylformamide and pyridine, and the degree of sulfation of the sodium salt of sucrose sulfate thus obtained was estimated from the ratio of sulfur to carbon content (S/C). The sulfates prepared with 9-15 molar equivalents of pyridine-sulfur trioxide in dimethylformamide and those prepared with 5 and 9 equivalents in pyridine were identified as sucrose octasulfate. Potassium, cesium, rubidium, and ammonium salts of sucrose octasulfate were obtained as crystals.