A novel 2,6-dimethyl-b-CD bonded and silica based HPLC chiral stationary phase(CSP) was prepared.The diphenylmethane diisocyanate(MDI) was applied for the first time in the immobilization of 2,6-dimethyl-b-CD onto the surface of aminized silica gel under mild conditions. The composite materials obtained were used as the CSP for chiral separation processes and this kind of CSP exhibits good enantioselectivity for a variety of chiral compounds under reversed-phase conditions. A novel 2,6-dimethyl-b-CD bonded and silica based HPLC chiral stationary phase (CSP) was prepared. The diphenylmethane diisocyanate (MDI) was applied for the first time in the immobilization of 2,6-dimethyl-b-CD onto the surface of aminized silica gel under mild conditions. The composite materials obtained were used as the CSP for chiral separation processes and this kind of CSP exhibits good enantioselectivity for a variety of chiral compounds.