Abstract:A method for the determination of D-psicose sugar in sugar-free beverages by high performance liquid chromatography-evaporative light detection was established.After 20% acetonitrile extraction，the samples were purified and enriched by HLB solid phase extraction column，and then detected on the machine after filtration membrane.The separation of targeted compound used acetonitrile∶water （30∶70，volume ratio）as mobile phase，with evaporative light scattering detector and external standard method peak area quantification.The linear range of D-psicose was in the range of 0.01 g/100 mL-0.80 g/100 mL with a correlation coefficient of 0.999 4.The detection limit was 0.002 g/100 mL and the quantitative limit was 0.006 g/100 mL.The recovery rate was 91.5 %-94.2 %.The method is suitable for the quantitative detection of D-psicose in sugar-free beverage.