Display options
Share it on

J Liq Chromatogr Relat Technol. 2012;35(5):737-746. doi: 10.1080/10826076.2011.608231. Epub 2012 Feb 22.

PREPARATIVE ISOLATION AND PURIFICATION OF THREE GLYCINE-CONJUGATED CHOLIC ACIDS FROM PULVIS FELLIS SUIS BY HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY COUPLED WITH ELSD DETECTION.

Journal of liquid chromatography & related technologies

Jiao He, Jing Li, Wenji Sun, Tianyou Zhang, Yoichiro Ito

Affiliations

  1. Biomedicine Key Laboratory of Shaanxi Province, Northwest University, No.229 Taibai North Road, Xi'an 710069, PR China.

PMID: 23008527 PMCID: PMC3448131 DOI: 10.1080/10826076.2011.608231

Abstract

Coupled with evaporative light scattering detection, a high-speed counter-current chromatography (HSCCC) method was developed for preparative isolation and purification of three glycine-conjugated cholic acids, glycochenodeoxycholic acid (GCDCA), glycohyodeoxycholic acid (GHDCA) and glycohyocholic acid (GHCA) from Pulvis Fellis Suis (Pig gallbladder bile) for the first time. The separation was performed with a two-phase solvent system consisted of chloroform-methanol-water-acetic acid (65:30:10:1.5, v/v/v/v) by eluting the lower phase in the head-to-tail elution mode. The revolution speed of the separation column, flow rate of the mobile phase and separation temperature were 800 rpm, 2 ml/min and 25 °C, respectively. In a single operation, 33 mg of GCDCA, 38 mg of GHDCA and 23 mg of GHCA were obtained from 200 mg of crude extract with the purity of 95.65%, 96.72% and 96.63%, respectively, in one step separation. The HSCCC fractions were analyzed by high-performance liquid chromatography (HPLC) and the structures of the three glycine-conjugated cholic acids were identified by ESI-MS, (1)H NMR and (13)C NMR.

References

  1. J Chromatogr A. 2008 Jan 18;1178(1-2):101-7 - PubMed
  2. J Chromatogr A. 2008 Sep 26;1205(1-2):177-81 - PubMed
  3. J Chromatogr A. 2001 Sep 21;929(1-2):169-73 - PubMed
  4. J Chromatogr A. 2006 Feb 3;1104(1-2):69-74 - PubMed
  5. J Chromatogr A. 2005 Feb 18;1065(2):145-68 - PubMed
  6. J Chromatogr A. 2001 Jul 20;923(1-2):271-4 - PubMed
  7. J Chromatogr. 1991 Jan 18;538(1):3-25 - PubMed

Publication Types

Grant support