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Chromatographia. 2011;73(3):361-365. doi: 10.1007/s10337-010-1893-2.

Semi-Preparative Isolation and Purification of Three Tauro-Conjugated Cholic Acids from Pulvis Fellis Suis by HSCCC Coupled with ELSD Detection.

Chromatographia

Jiao He, Yongmin Zhang, Yoichiro Ito, Wenji Sun

Affiliations

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

PMID: 21442029 PMCID: PMC3063647 DOI: 10.1007/s10337-010-1893-2

Abstract

Coupled with evaporative light scattering detection, a high-speed counter-current chromatography (HSCCC) method was applied to the separation and purification of three tauro-conjugated cholic acids of taurochenodeoxycholic acid (TCDCA), taurohyodeoxycholic acid (THDCA) and taurohyocholic acid (THCA) from Pulvis Fellis Suis (Pig gallbladder bile) for the first time. The two-phase solvent system composed of chloroform-methanol-water-acetic acid (4:4:2:0.3, v/v/v/v) was selected for the one-step separation where the lower phase was used as the mobile 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, 1.5 ml/min and 25°C respectively. From 100 mg of the crude extract, 10.2 mg of TCDCA, 11.8 mg of THDCA and 5.3 mg of THCA were obtained with the purity of 94.6%, 96.5% and 95.4%, respectively. in one step separation The HSCCC fractions were analyzed by high-performance liquid chromatography (HPLC) and the structures of the three tauro-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

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