Formation of octreotide’s disulfide bonds can generally be achieved by oxidation of the free thiol or sulfur-protected precursors. A variety of oxidants have been explored for formation of disulfide bonds, however, there are drawbacks and limitations, Such as formation of dimers and oligomers, etc. . In this paper, we developed a highly efficient heterogenous catalysis for intramolecular disulfide bond formation in octreotide. The reaction proceeded quite rapidly without using high pseudo-dilution conditions.