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Combinative application of pH-zone-refining and conventional high-speed counter-current chromatography for preparative separation of alkaloids from Stephania kwangsiensis.
J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Apr 15; 879(13-14):945-9.JC

Abstract

A method which involves the combination of pH-zone-refining counter-current chromatography (pH-zone-refining CCC) and conventional high-speed counter-current chromatography (HSCCC) was established for the preparative separation of alkaloids from the crude extracts of Stephania kwangsiensis. pH-zone-refining CCC was first performed with the solvent system composed of n-hexane-ethyl acetate-methanol-water (3:7:1:9, v/v), where triethylamine (10 mM) was added to the upper organic stationary phase as a retainer and hydrochloric acid (5 mM) to the aqueous mobile phase as an eluter. From 2.0 g of crude extract, 370 mg of sinoacutine and 600 mg of a mixture of three other alkaloids were obtained. Then, the mixture was further separated by conventional HSCCC with the solvent system composed of n-hexane-ethyl acetate-methanol-water (7:3:6:4, v/v), yielding 42 mg of (-)-crebanine, 50 mg of (-)-stephanine and 30 mg of l-romerine from 150 mg mixture of three other alkaloids, respectively. The purities of the four compounds were all over 98% as determined by HPLC, and the chemical structures of the four compounds were confirmed by positive ESI-MS and (1)H NMR data. Results of the present study successfully indicated that this method was efficient for the preparative separation of alkaloids from natural plants.

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Publisher Full Text (DOI)

Authors+Show Affiliations

Dong H
Shandong Analysis and Test Center, Shandong Academy of Sciences, Jinan, Shandong, China.
Zhang Y
No affiliation info available
Fang L
No affiliation info available
Duan W
No affiliation info available
Wang X
No affiliation info available
Huang L
No affiliation info available

MeSH

AcetatesAporphinesChromatography, High Pressure LiquidCountercurrent DistributionHexanesHydrogen-Ion ConcentrationMethanolMorphinansNuclear Magnetic Resonance, BiomolecularPlant ExtractsSpectrometry, Mass, Electrospray IonizationStephaniaWater

Pub Type(s)

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

Language

eng

PubMed ID

21450539

Citation

Dong, Hongjing, et al. "Combinative Application of pH-zone-refining and Conventional High-speed Counter-current Chromatography for Preparative Separation of Alkaloids From Stephania Kwangsiensis." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 879, no. 13-14, 2011, pp. 945-9.
Dong H, Zhang Y, Fang L, et al. Combinative application of pH-zone-refining and conventional high-speed counter-current chromatography for preparative separation of alkaloids from Stephania kwangsiensis. J Chromatogr B Analyt Technol Biomed Life Sci. 2011;879(13-14):945-9.
Dong, H., Zhang, Y., Fang, L., Duan, W., Wang, X., & Huang, L. (2011). Combinative application of pH-zone-refining and conventional high-speed counter-current chromatography for preparative separation of alkaloids from Stephania kwangsiensis. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 879(13-14), 945-9. https://doi.org/10.1016/j.jchromb.2011.02.051
Dong H, et al. Combinative Application of pH-zone-refining and Conventional High-speed Counter-current Chromatography for Preparative Separation of Alkaloids From Stephania Kwangsiensis. J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Apr 15;879(13-14):945-9. PubMed PMID: 21450539.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Combinative application of pH-zone-refining and conventional high-speed counter-current chromatography for preparative separation of alkaloids from Stephania kwangsiensis. AU - Dong,Hongjing, AU - Zhang,Yongqing, AU - Fang,Lei, AU - Duan,Wenjuan, AU - Wang,Xiao, AU - Huang,Luqi, Y1 - 2011/03/28/ PY - 2011/01/27/received PY - 2011/02/28/revised PY - 2011/02/28/accepted PY - 2011/4/1/entrez PY - 2011/4/1/pubmed PY - 2011/8/4/medline SP - 945 EP - 9 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J Chromatogr B Analyt Technol Biomed Life Sci VL - 879 IS - 13-14 N2 - A method which involves the combination of pH-zone-refining counter-current chromatography (pH-zone-refining CCC) and conventional high-speed counter-current chromatography (HSCCC) was established for the preparative separation of alkaloids from the crude extracts of Stephania kwangsiensis. pH-zone-refining CCC was first performed with the solvent system composed of n-hexane-ethyl acetate-methanol-water (3:7:1:9, v/v), where triethylamine (10 mM) was added to the upper organic stationary phase as a retainer and hydrochloric acid (5 mM) to the aqueous mobile phase as an eluter. From 2.0 g of crude extract, 370 mg of sinoacutine and 600 mg of a mixture of three other alkaloids were obtained. Then, the mixture was further separated by conventional HSCCC with the solvent system composed of n-hexane-ethyl acetate-methanol-water (7:3:6:4, v/v), yielding 42 mg of (-)-crebanine, 50 mg of (-)-stephanine and 30 mg of l-romerine from 150 mg mixture of three other alkaloids, respectively. The purities of the four compounds were all over 98% as determined by HPLC, and the chemical structures of the four compounds were confirmed by positive ESI-MS and (1)H NMR data. Results of the present study successfully indicated that this method was efficient for the preparative separation of alkaloids from natural plants. SN - 1873-376X UR - https://www.unboundmedicine.com/medline/citation/21450539/Combinative_application_of_pH_zone_refining_and_conventional_high_speed_counter_current_chromatography_for_preparative_separation_of_alkaloids_from_Stephania_kwangsiensis_ DB - PRIME DP - Unbound Medicine ER -