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In this study, a novel kind of core-shell structured superparamagnetic microsphere decorated with 1,3-alternate calix[4]arene-crown-6 host molecules at the periphery was developed for selective recognition and magnetic separation of Pb(Ⅱ)for the first time.The four-component microsphere consists of a super paramagnetic Fe3O4 core, two-layer silica serving as protection shell and functional spacer, and a macrocyclic host molecule 1,3-alternate calix[4]arene-crown-6 decorated periphery.