Stationary sorbents play a key role in the separation process. We present here a kind of unique separative material, called thiophilic affinity MOFs, as specific sorbent for the capture of compounds containing disulfide-bond. The sorbent was obtained through epoxide ring-opening reaction among MOF-5-NH 2 , tris(2,3-epoxypropyl) isocyanurate, and thiophilic reagents under mild reaction condition. The synthesized sorbent was characterized with X-ray diffraction, scanning electron microscope, transmission electron microscope, Fourier transform infrared, thermogravimetric analysis and N 2 absorption. The capillary electrophoresis experiments verified their high specific recognization and separation for disulfide bond-containing compounds.