OCTOXYNOL PRESENCE IN BEAR-BILE

The presence of octoxynol from dried bear-bile was examined. Octoxynol was coextracted when glycolipids by Folch-Suzuki partition method. Oc toxynol formed mixed-micelles with glycosphingolipids. The glycolipids were purified by DEAE-Sephadex A-25 column chromatography. The fracti ons containing mixed micelles were obtained from linear gradient solve nt of 0.05M-0.5M ammonium acetate in methanol. HPLC (Bondapak-NH2 - li nked to a Bondapak-C-18 column) chromatogram showed five peaks. Two po ssible structures for the fourth peak fraction were proposed as (CH3)( 3)C-CH2-C(CH3)(2)-C6H4-OR and (CH3)(3)C-C(CH3)(2)-CH2-C6H4-OR by NMR s pectroscopy. The structure was further confirmed by electrospray tande m mass spectrometry (ESI MS/MS). The spectrum showed a protonated mole cule at m/z 559 and three different series of ions with mass differenc e of 44 were detected in the MS/MS spectrum. Therefore, the structure of the fourth peak fraction from HPLC was confirmed as octoxynol, (CH3 )(3)C-CH2-C(CH3)(2)-C6H4-(OCHZ-CH2)n-OH, based on mass spectrometry an d NMR spectroscopy.