An efficient and target-oriented sample enrichment method for preparative separation of minor alkaloids by pH-zone-refining counter-current chromatography
文献类型：期刊论文
| 作者 | Feng, Rui-Hong; Hou, Jin-Jun ; Zhang, Yi-Bei; Pan, Hui-Qin; Yang, Wenzhi; Qi, Peng; Yao, Shuai; Cai, Lu-Ying; Yang, Min; Jiang, Bao-hong
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| 刊名 | JOURNAL OF CHROMATOGRAPHY A
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| 出版日期 | 2015-08-28 |
| 卷号 | 1409页码:159-165 |
| ISSN号 | 0021-9673 |
| 关键词 | Target-oriented sample enrichment method Indole alkaloids pH-zone-refining counter-current chromatography Uncaria rhynchophylla |
| DOI | 10.1016/j.chroma.2015.07.066 |
| 文献子类 | Article |
| 英文摘要 | An efficient and target-oriented sample enrichment method was established to increase the content of the minor alkaloids in crude extract by using the corresponding two-phase solvent system applied in pH-zone-refining counter-current chromatography. The enrichment and separation of seven minor indole alkaloids from Uncaria rhynchophylla (Miq.) Miq. ex Havil(UR) were selected as an example to show the advantage of this method. An optimized two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (3:7:1:9, v/v) was used in this study, where triethylamine (TEA) as the retainer and hydrochloric acid (HCl) as the eluter were added at the equimolar of 10 mM. Crude alkaloids of UR dissolved in the corresponding upper phase (containing 10 mM TEA) were extracted twice with lower phase (containing 10 mM TEA) and lower phase (containing 10 mM HCl), respectively, the second lower phase extract was subjected to pH-zone-refining CCC separation after alkalization and desalination. Finally, from 10 g of crude alkaloids, 4g of refined alkaloids was obtained and the total content of seven target indole alkaloids was increased from 4.64% to 15.78%. Seven indole alkaloids, including 54 mg isocorynoxeine, 21 mg corynoxeine, 46 mg isorhynchophylline, 35 mg rhynchophylline, 65 mg hirsutine, 51 mg hirsuteine and 27 mg geissoschizine methylether were all simultaneously separated from 2.5 g of refined alkaloids, with the purity of 86.4%, 97.5%, 90.3%, 92.1%, 98.5%, 92.3%, and 92.8%, respectively. The total content and purities of the seven minor indole alkaloids were tested by HPLC and their chemical structures were elucidated by ESI-HRMS and H-1 NMR. (C) 2015 Elsevier B.V. All rights reserved. |
| WOS关键词 | UNCARIA-RHYNCHOPHYLLA ; INDOLE ALKALOIDS |
| 资助项目 | National Science and Technology Major Project for Major Drug Development[2013ZX09508104] ; National Science and Technology Major Project for Major Drug Development[2014ZX09304-307-001-007] ; Traditional Chinese Medicine Industry Research Special Project[201307002] ; Chinese Academy of Sciences, China[KSZD-EW-Z-004-01] |
| WOS研究方向 | Biochemistry & Molecular Biology ; Chemistry |
| 语种 | 英语 |
| 出版者 | ELSEVIER SCIENCE BV |
| WOS记录号 | WOS:000359882600018 |
| 源URL | [http://119.78.100.183/handle/2S10ELR8/276432]  |
| 专题 | 上海中药现代化研究中心 |
| 通讯作者 | Wu, Wan-Ying |
| 作者单位 | Chinese Acad Sci, Shanghai Res Ctr Modernizat Tradit Chinese Med, Natl Engn Lab TCM Standardizat Technol, Shanghai Inst Mat Med, Shanghai 201203, Peoples R China |
| 推荐引用方式 GB/T 7714 | Feng, Rui-Hong,Hou, Jin-Jun,Zhang, Yi-Bei,et al. An efficient and target-oriented sample enrichment method for preparative separation of minor alkaloids by pH-zone-refining counter-current chromatography[J]. JOURNAL OF CHROMATOGRAPHY A,2015,1409:159-165. |
| APA | Feng, Rui-Hong.,Hou, Jin-Jun.,Zhang, Yi-Bei.,Pan, Hui-Qin.,Yang, Wenzhi.,...&Guo, De-An.(2015).An efficient and target-oriented sample enrichment method for preparative separation of minor alkaloids by pH-zone-refining counter-current chromatography.JOURNAL OF CHROMATOGRAPHY A,1409,159-165. |
| MLA | Feng, Rui-Hong,et al."An efficient and target-oriented sample enrichment method for preparative separation of minor alkaloids by pH-zone-refining counter-current chromatography".JOURNAL OF CHROMATOGRAPHY A 1409(2015):159-165. |
入库方式： OAI收割
来源：上海药物研究所
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