Cyclodextrin(CD) loaded MCM-41 was used for adsorption of L-Valine in dilute aqeuous solution. Incorporation of CD on MCM-41 was performed at 170℃ by dehydration. β-CD loaded MCM-41 showed the best adsorption activity among α-CD, β-CD, and crown ether. As pH of solution increased the amount of L-Valine adsorption on CD/MCM-41 increased. The selective separation of L-Valine from glucose mixture could be achieved by using CD/MCM-41 adsorbents.