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Application of high-speed countercurrent chromatography-evaporative light scattering detection for the separation of seven steroidal saponins from Dioscorea villosa.
Phytochem Anal. 2012 Sep-Oct; 23(5):462-8.PA

Abstract

INTRODUCTION

Steroidal saponins in Dioscorea species are chemically characterised as spirostanol and furostanol saponins, and have been used as standard marker compounds due to their chemotaxonomical significance and their important biological activities.

OBJECTIVE

To design a simple, rapid and efficient method for the separation of steroidal saponins with a high degree of purity using high-speed countercurrent chromatography (HSCCC) coupled with evaporative light scattering detection (ELSD).

METHODOLOGY

In the first step, reversed-phase mode HSCCC (flow rate: 1.5 mL/min; revolution speed: 800 rpm) using n-hexane:n-butanol:water [3:7:10 (v/v/v)] was employed to separate furostanol saponins from n-butanol soluble extracts of Dioscorea villosa. After the first HSCCC run, spirostanol saponins retained in the stationary phase were subjected to the second HSCCC (normal-phase mode; flow rate: 2.0 mL/min; revolution speed: 800 rpm). A two-phase solvent system composed of chloroform:methanol:isopropanol:water [10:6:1:4 (v/v/v/v)] was employed in the second HSCCC. The structures of isolates were elucidated by (1) H-NMR, (13) C-NMR, ESI-MS and HPLC analysis.

RESULTS

Three furostanol saponins, parvifloside (27.3 mg), methyl protodeltonin (67.1 mg) and trigofoenoside A-1 (18.5 mg) were isolated from the n-butanol soluble extract of D. villosa by the first HSCCC run. Subsquent normal-phase HSCCC of the spirostanol-rich extract led to the separation of four spirostanol saponins: zingiberensis saponin I (15.2 mg), deltonin (31.5 mg), dioscin (7.7 mg) and prosapogenin A of dioscin (3.4 mg).

Links

Publisher Full Text (DOI)

Authors+Show Affiliations

Yoon KD
College of Pharmacy, The Catholic University of Korea, Bucheon-si, Gyeonggi-do 420-743, Korea.
Chin YW
No affiliation info available
Yang MH
No affiliation info available
Choi J
No affiliation info available
Kim J
No affiliation info available

MeSH

Chemical FractionationCountercurrent DistributionDioscoreaDiosgeninMagnetic Resonance SpectroscopyPhytosterolsPlant ExtractsRhizomeSaponinsScattering, RadiationSolubilitySolventsSpectrometry, Mass, Electrospray IonizationSpirostans

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

22407490

Citation

Yoon, Kee Dong, et al. "Application of High-speed Countercurrent Chromatography-evaporative Light Scattering Detection for the Separation of Seven Steroidal Saponins From Dioscorea Villosa." Phytochemical Analysis : PCA, vol. 23, no. 5, 2012, pp. 462-8.
Yoon KD, Chin YW, Yang MH, et al. Application of high-speed countercurrent chromatography-evaporative light scattering detection for the separation of seven steroidal saponins from Dioscorea villosa. Phytochem Anal. 2012;23(5):462-8.
Yoon, K. D., Chin, Y. W., Yang, M. H., Choi, J., & Kim, J. (2012). Application of high-speed countercurrent chromatography-evaporative light scattering detection for the separation of seven steroidal saponins from Dioscorea villosa. Phytochemical Analysis : PCA, 23(5), 462-8. https://doi.org/10.1002/pca.2342
Yoon KD, et al. Application of High-speed Countercurrent Chromatography-evaporative Light Scattering Detection for the Separation of Seven Steroidal Saponins From Dioscorea Villosa. Phytochem Anal. 2012 Sep-Oct;23(5):462-8. PubMed PMID: 22407490.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Application of high-speed countercurrent chromatography-evaporative light scattering detection for the separation of seven steroidal saponins from Dioscorea villosa. AU - Yoon,Kee Dong, AU - Chin,Young-Won, AU - Yang,Min Hye, AU - Choi,Janggyoo, AU - Kim,Jinwoong, Y1 - 2012/03/09/ PY - 2011/09/10/received PY - 2011/10/27/revised PY - 2011/11/16/accepted PY - 2012/3/13/entrez PY - 2012/3/13/pubmed PY - 2012/12/15/medline SP - 462 EP - 8 JF - Phytochemical analysis : PCA JO - Phytochem Anal VL - 23 IS - 5 N2 - INTRODUCTION: Steroidal saponins in Dioscorea species are chemically characterised as spirostanol and furostanol saponins, and have been used as standard marker compounds due to their chemotaxonomical significance and their important biological activities. OBJECTIVE: To design a simple, rapid and efficient method for the separation of steroidal saponins with a high degree of purity using high-speed countercurrent chromatography (HSCCC) coupled with evaporative light scattering detection (ELSD). METHODOLOGY: In the first step, reversed-phase mode HSCCC (flow rate: 1.5 mL/min; revolution speed: 800 rpm) using n-hexane:n-butanol:water [3:7:10 (v/v/v)] was employed to separate furostanol saponins from n-butanol soluble extracts of Dioscorea villosa. After the first HSCCC run, spirostanol saponins retained in the stationary phase were subjected to the second HSCCC (normal-phase mode; flow rate: 2.0 mL/min; revolution speed: 800 rpm). A two-phase solvent system composed of chloroform:methanol:isopropanol:water [10:6:1:4 (v/v/v/v)] was employed in the second HSCCC. The structures of isolates were elucidated by (1) H-NMR, (13) C-NMR, ESI-MS and HPLC analysis. RESULTS: Three furostanol saponins, parvifloside (27.3 mg), methyl protodeltonin (67.1 mg) and trigofoenoside A-1 (18.5 mg) were isolated from the n-butanol soluble extract of D. villosa by the first HSCCC run. Subsquent normal-phase HSCCC of the spirostanol-rich extract led to the separation of four spirostanol saponins: zingiberensis saponin I (15.2 mg), deltonin (31.5 mg), dioscin (7.7 mg) and prosapogenin A of dioscin (3.4 mg). SN - 1099-1565 UR - https://www.unboundmedicine.com/medline/citation/22407490/Application_of_high_speed_countercurrent_chromatography_evaporative_light_scattering_detection_for_the_separation_of_seven_steroidal_saponins_from_Dioscorea_villosa_ L2 - https://doi.org/10.1002/pca.2342 DB - PRIME DP - Unbound Medicine ER -