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Novel amphiphilic β-cyclodextrins1 (β-CDs),6-O-(dodecyloxy-2-hydroxypropyl)-2-O-(2-hydroxypropyl)-β-cyclodextrin (1),6-O-(tetradecyloxy-2-hydroxypropyl)-2-O-(2-hydroxypropyl)-1β-cyclodextrin (2),6-O-(hexadecyloxy-2-hydroxypropyl)-2-O-(2-hydroxypropyl)-β-cyclodextrin (3) and 6-O-(octadecyloxy-2-hydroxypropyl)-2-O-(2-hydroxypropyl)-β-cyclodextrin (4) were designed and synthesized in about 10% yield.These structures (1~4) were characterized and confirmed by 1H-NMR,13C-NMR, and ESI-MS.The average substituted degrees of hydroxypropyl groups and alkoxyl groups,calculated according to literatures2, were about six and two, respectively.Nanoparticles were prepared from these novel amphiphilic β-CDs (1~4) by ultra-sonicating.