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Supercritical fluid chromatography for separation and preparation of tautomeric 7-epimeric spiro oxindole alkaloids from Uncaria macrophylla

文献类型：期刊论文

作者Yang, Wenzhi2; Zhang, Yibei2; Pan, Huiqin1,2; Yao, Changliang1,2; Hou, Jinjun2; Yao, Shuai2; Cai, Luying2; Feng, Ruihong2; Wu, Wanying2; Guo, Dean2
刊名JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
出版日期2017-02-05
卷号134页码:352-360
关键词Spiro oxindole alkaloid Uncaria macrophylla Isomerization Ultra-performance convergence chromatography Preparative scale supercritical fluid chromatography
ISSN号0731-7085
DOI10.1016/j.jpba.2016.10.021
文献子类Article
英文摘要Increasing challenge arising from configurational interconversion in aqueous solvent renders it rather difficult to isolate high-purity tautomeric reference standards and thus largely hinders the holistic quality control of traditional Chinese medicine (TCM). Spiro oxindole alkaloids (SOAs), as the markers for the medicinal Uncaria herbs, can easily isomerize in polar or aqueous solvent via a retro-Mannich reaction. In the present study, supercritical fluid chromatography (SFC) is utilized to separate and isolate two pairs of 7-epimeric SOAs, including rhynchophylline (R) and isorhynchophylline (IR), corynoxine (C) and corynoxine B (CB), from Uncaria macrophylla. Initially, the solvent that can stabilize SOA epimers was systematically screened, and acetonitrile was used to dissolve and as the modifier in SFC. Then, key parameters of ultra-high performance SFC (ultra-performance convergence chromatography, UPC2), comprising stationary phase, additive in modifier, column temperature, ABPR pressure, and flow rate, were optimized in sequence. Two isocratic UPC2 methods were developed on the achiral Torus 1-AA and Torus Diol columns, suitable for UV and MS detection, respectively. MCI gel column chromatography fractionated the U. macrophylla extract into two mixtures (R/IR and C/CB). Preparative SFC, using a Viridis Prep Silica 2-EP OBD column and acetonitrile-0.2% diethylamine in CO2 as the mobile phase, was finally employed for compound purification. As a result, the purity of four SOA compounds was all higher than 95%. Different from reversed-phase HPLC, SFC, by use of water-free mobile phase (inert CO2 and aprotic modifier), provides a solution to rapid analysis and isolation of tautomeric reference standards for quality control of TCM. (C) 2016 Elsevier B.V. All rights reserved.
WOS关键词PERFORMANCE LIQUID-CHROMATOGRAPHY ; MASS-SPECTROMETRY ; INDOLE ALKALOIDS ; RHYNCHOPHYLLA ; PHYTOCHEMISTRY ; ISOMERIZATION ; PHARMACOLOGY ; KINETICS ; RADIX ; RATS
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]
WOS研究方向Chemistry ; Pharmacology & Pharmacy
语种英语
WOS记录号WOS:000392909900045
出版者ELSEVIER SCIENCE BV
源URL[http://119.78.100.183/handle/2S10ELR8/275636]  
专题上海中药现代化研究中心
通讯作者Wu, Wanying
作者单位1.Univ Chinese Acad Sci, 19A Yuquan Rd, Beijing 100049, Peoples R China
2.Chinese Acad Sci, Shanghai Inst Mat Med, Natl Engn Lab TCM Standardizat Technol, Shanghai Res Ctr Modernizat Tradit Chinese Med, Haike Rd 501, Shanghai 201203, Peoples R China;
推荐引用方式
GB/T 7714		 Yang, Wenzhi,Zhang, Yibei,Pan, Huiqin,et al. Supercritical fluid chromatography for separation and preparation of tautomeric 7-epimeric spiro oxindole alkaloids from Uncaria macrophylla[J]. JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS,2017,134:352-360.
APA Yang, Wenzhi.,Zhang, Yibei.,Pan, Huiqin.,Yao, Changliang.,Hou, Jinjun.,...&Guo, Dean.(2017).Supercritical fluid chromatography for separation and preparation of tautomeric 7-epimeric spiro oxindole alkaloids from Uncaria macrophylla.JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS,134,352-360.
MLA Yang, Wenzhi,et al."Supercritical fluid chromatography for separation and preparation of tautomeric 7-epimeric spiro oxindole alkaloids from Uncaria macrophylla".JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS 134(2017):352-360.

入库方式： OAI收割

来源：上海药物研究所

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