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Flow rate gradient high-speed counter-current chromatography separation of five diterpenoids from Triperygium wilfordii and scale-up.
J Chromatogr A. 2008 Jul 25; 1200(2):129-35.JC

Abstract

In this paper, high-speed counter-current chromatography (HSCCC) instruments with different gravitational forces were applied for the separation of bioactive compounds from Triperygium wilfordii Hook.f. The critical parameters including sample concentration, sample volume and flow rate were first optimized on an analytical Mini-DE HSCCC system, and then scaled up to a preparative TBE 300A HSCCC system. Although this scale-up process was performed using different CCC instruments with different centrifuges and gravitational forces, the same resolutions were obtained and the elution time could be predictable. Five diterpenoid compounds and one unknown compound were separated from Triperygium wilfordii Hook.f. by HSCCC with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (HEMW) (3:2:3:2, v/v/v/v). This one-step flow gradient separation produced triptonide (25 mg), isoneotriptophenolide (77 mg), hypolide (83 mg), unknown compound (1 mg), triptophenolide (42 mg), triptonoterpene methyl ether VI (37 mg) from 320 mg crude extract with purities of 98.2%, 96.6%, 98.1%, 95.3%, 95.1%, and 96.5%, respectively. Their purities and structures were identified by high-performance liquid chromatography, mass spectrometry and NMR. This paper demonstrates that analytical CCC plays an important role in optimizing parameters and scale-up process when analytical CCC and preparative CCC are supplied by different manufacturers with different gravitational forces, and the scale-up process from analytical CCC to preparative CCC is still predictable.

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Authors+Show Affiliations

Peng A
State Key Laboratory of Biotherapy, West China Hospital, West China Medical School, Sichuan University, Gaopeng Street, Keyuan Road 4, Chengdu 610041, China.
Li R
No affiliation info available
Hu J
No affiliation info available
Chen L
No affiliation info available
Zhao X
No affiliation info available
Luo H
No affiliation info available
Ye H
No affiliation info available
Yuan Y
No affiliation info available
Wei Y
No affiliation info available

MeSH

CelastraceaeChromatographyChromatography, High Pressure LiquidCountercurrent DistributionDiterpenesMolecular StructureSpectrometry, Mass, Electrospray Ionization

Pub Type(s)

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

Language

eng

PubMed ID

18554602

Citation

Peng, Aihua, et al. "Flow Rate Gradient High-speed Counter-current Chromatography Separation of Five Diterpenoids From Triperygium Wilfordii and Scale-up." Journal of Chromatography. A, vol. 1200, no. 2, 2008, pp. 129-35.
Peng A, Li R, Hu J, et al. Flow rate gradient high-speed counter-current chromatography separation of five diterpenoids from Triperygium wilfordii and scale-up. J Chromatogr A. 2008;1200(2):129-35.
Peng, A., Li, R., Hu, J., Chen, L., Zhao, X., Luo, H., Ye, H., Yuan, Y., & Wei, Y. (2008). Flow rate gradient high-speed counter-current chromatography separation of five diterpenoids from Triperygium wilfordii and scale-up. Journal of Chromatography. A, 1200(2), 129-35. https://doi.org/10.1016/j.chroma.2008.05.041
Peng A, et al. Flow Rate Gradient High-speed Counter-current Chromatography Separation of Five Diterpenoids From Triperygium Wilfordii and Scale-up. J Chromatogr A. 2008 Jul 25;1200(2):129-35. PubMed PMID: 18554602.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Flow rate gradient high-speed counter-current chromatography separation of five diterpenoids from Triperygium wilfordii and scale-up. AU - Peng,Aihua, AU - Li,Rui, AU - Hu,Jia, AU - Chen,Lijuan, AU - Zhao,Xia, AU - Luo,Houding, AU - Ye,Haoyu, AU - Yuan,Yuan, AU - Wei,Yuquan, Y1 - 2008/05/23/ PY - 2007/12/12/received PY - 2008/05/19/revised PY - 2008/05/20/accepted PY - 2008/6/17/pubmed PY - 2008/9/27/medline PY - 2008/6/17/entrez SP - 129 EP - 35 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1200 IS - 2 N2 - In this paper, high-speed counter-current chromatography (HSCCC) instruments with different gravitational forces were applied for the separation of bioactive compounds from Triperygium wilfordii Hook.f. The critical parameters including sample concentration, sample volume and flow rate were first optimized on an analytical Mini-DE HSCCC system, and then scaled up to a preparative TBE 300A HSCCC system. Although this scale-up process was performed using different CCC instruments with different centrifuges and gravitational forces, the same resolutions were obtained and the elution time could be predictable. Five diterpenoid compounds and one unknown compound were separated from Triperygium wilfordii Hook.f. by HSCCC with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (HEMW) (3:2:3:2, v/v/v/v). This one-step flow gradient separation produced triptonide (25 mg), isoneotriptophenolide (77 mg), hypolide (83 mg), unknown compound (1 mg), triptophenolide (42 mg), triptonoterpene methyl ether VI (37 mg) from 320 mg crude extract with purities of 98.2%, 96.6%, 98.1%, 95.3%, 95.1%, and 96.5%, respectively. Their purities and structures were identified by high-performance liquid chromatography, mass spectrometry and NMR. This paper demonstrates that analytical CCC plays an important role in optimizing parameters and scale-up process when analytical CCC and preparative CCC are supplied by different manufacturers with different gravitational forces, and the scale-up process from analytical CCC to preparative CCC is still predictable. SN - 0021-9673 UR - https://www.unboundmedicine.com/medline/citation/18554602/Flow_rate_gradient_high_speed_counter_current_chromatography_separation_of_five_diterpenoids_from_Triperygium_wilfordii_and_scale_up_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(08)00901-1 DB - PRIME DP - Unbound Medicine ER -
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