Abstract:This study aimed to accurately determine the fructose content in Polygonatum sibiricum polysaccharides.A hydrophilic interaction liquid chromatography-charged aerosol detector（HILIC-CAD）method was employed to systematically investigate the four single factors on polysaccharide hydrolysis，i.e.，polysaccharide concentration，acid concentration，temperature，and hydrolysis time. Optimal hydrolysis conditions were determined through orthogonal testing. The results indicated that the optimal conditions for the hydrolysis of P. sibiricum polysaccharides were as follows：1.0 mg/mL P. sibiricum polysaccharides were hydrolyzed in a 0.100 mol/L trifluoroacetic acid solution at 80 ℃for 30 min. Under these conditions，fructose was completely released without conversion to other substances.By combining HILIC-CAD with pre-column derivatization and reverse-phase chromatography，the exact content of fructose and six other monosaccharides in P. sibiricum polysaccharides from five different regions（Shandong，Anhui，Gansu，Sichuan，and Shaanxi）was determined. It was found that the fructose content in the P. sibiricum polysaccharides from Anhui was relatively low（51.74%），while the fructose content from the other four regions was higher and similar（78.71%-83.08%）.