We have occluded functional nanoparticles into hollow organosilica microspheres using the sol-gel reactions of alkylsilyl trichlorides around water droplets in a water-in-oil emulsion. Metallic cobalt and magnetite nanoparticles was encapsulated into the hollow particles to give a magnetically collectable, reusable adsorbent and catalyst for concentrating heavy metal ions in acidic aqueous solutions and solid acid catalysis in aqueous media. Sulfonic groups, that acted as adsorption sites for Zn and Pb ions under an acidic condition, were immobilized on the external surface through silylation with 3-mercaptopropyl(trimethoxysilane) and subsequent oxidization of the thiol groups by 7 MHNO3. The adsorbent was regenerated using 1 M HCl without eroding the magnetic nanoparticles.