Octreotide, a disulfide-cyclized eight amino acids long analogue of somatostatin, has been used to treat the symptoms associated with metastatic carcinoid tumors (flushing and diarrhea), and vasoactive intestinal peptide secreting adenomas (watery diarrhea). As composed by D-amino acids, C-terminal alcohol, and disulfide bond, octreotide can be only prepared using chemistry synthesis method, which increases difficulty of the traditional reversed-phase separation. In this paper, we report a very fast separation of octreotide from synthetic peptide crude mixtures on a poly(styrene co-divinylbenzene) (PSt)-based reversed phases prepared by a quick membrane emulsification process. In general, fourier-transformed infrared resonance (FT-IR) spectroscopy, reversed-phase high performance liquid chromatography (HPLC) combined with electrospray ionisation mass spectrometry (ESI-MS), and nuclear magnetic resonance (NMR) spectroscopy are routinely used for analyses of resultant peptides. Under the optimized conditions, the octreotide is purified from 42.89% to 99.99%. Consequently, the poly(styrene co-divinylbenzene)-based phase can provide more flexibility to improve separation efficiency for the octreotide from the synthetic peptide crude mixtures. (C) 2015 Elsevier B.V. All rights reserved.