Small sized starch particles have attracted attention because of their novel physical properties.In this study,nanocrystals were prepared by complex formation and successive enzymatic hydrolysis.High amylose corn starch (25g) was hydrolyzed in acidic n-butnaol solution (35% HCl 8ml and n-butanol 100 ml) at 60℃ for 5 days,to starch dextrin of average 4,000.The dextrin was dissolved in 90% dimethyl sulfoxide (0.5% w/v),and complexed with n-butanol by a gravimetric migration into n-butanol layer separated by a membrane filter (PTFE,10μm),at 70℃ for 3 days.