Two kinds of novel chelating adsorbents have been synthesized to separate boron from aqueous solutions. One is the boron-specific chelating resin, synthesized by the functionalization of macroporous poly (glycidyl methacrylate-cotrimethylolpropane trimethacrylate), with N-methylglucamine. The other is the organic-inorganic hybrid mesoporous SBA-15 with polyol functional groups, prepared by a two-step post-grafting method. The resin can adsorb boron in almost all pH range, and its maximum uptake capacity reaches 1.15 mmol/g. The present study of the polyol-functionalized SBA-15 shows that the post-grafting is successful and the resulting adsorbent has the uptake capacity of 0.63 mmol/g.