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应用洗脱-推挤逆流色谱法高效分离制备人参皂苷Rg1、Rf及Rd
引用本文:程屹俊,梁琼麟,王义明,伍军,罗国安.应用洗脱-推挤逆流色谱法高效分离制备人参皂苷Rg1、Rf及Rd[J].中成药,2012,34(1):89-93.
作者姓名:程屹俊  梁琼麟  王义明  伍军  罗国安
作者单位:1. 华东理工大学中药现代化工程中心,上海200237;清华大学化学系,北京100084
2. 广州香雪制药股份有限公司,广东广州,510530
摘    要:目的 运用洗脱-推挤逆流色谱技术(EECCC)分离制备人参皂苷Rg1、Rf及Rd.方法以乙酸乙酯-正丁醇-0.1%甲酸水(2∶1∶3,v/v)为溶剂体系,上相为固定相,下相为流动相,仪器转速为1 250r/min,操作体积流量为40 mL/min,切换体积为2 400 mL.结果 在此条件下,经一步纯化从300 mg样品中分离纯化得到71 mg人参皂苷Rg1、21 mg人参皂苷Rf及53 mg人参皂苷Rd,经高效液相色谱分析,纯度分别达到96.2%、94.3%和95.1%.结论 EECCC制备方法快速,简单.对于分离分配系数高的物质十分有效.

关 键 词:高速逆流色谱  洗脱-推挤逆流色谱  人参皂苷Rg1  人参皂苷Rf  人参皂苷Rd

Elution-extrusion counter-current chromatography for preparation of ginsenoside-Rg1,Rf and Rd
CHENG Yi-jun , LIANG Qiong-lin , WANG Yi-ming , WU Jun , LUO Guo-an.Elution-extrusion counter-current chromatography for preparation of ginsenoside-Rg1,Rf and Rd[J].Chinese Traditional Patent Medicine,2012,34(1):89-93.
Authors:CHENG Yi-jun  LIANG Qiong-lin  WANG Yi-ming  WU Jun  LUO Guo-an
Institution:1,2(1.Modern Engineering Center for Traditional Chinese Medicine,School of Pharmacy,East China University of Science and Technology,Shanghai 200237,China;2.Department of Chemistry,Tsinghua University,Beijing 100084,China;3.Xiangxue Pharmaceutical Co.,Ltd.,Guangzhou 510530,China)
Abstract:AIM To use elution-extrusion counter-current chromatography(EECCC) to separate and prepare ginsenoside-Rg1,Rf and Rd in Ginseng Radix et Rhizoma.METHODS Ethyl acetate-n-butanol-0.1%formic acid(2∶ 1∶ 3,v/v) was chosen as the solvent system.The upper phase was used as stationary phase,and the lower phase used as mobile phase.The apparatus was rotated at 1 250 r/min,and the mobile(lower) phase was pumped into the column at 40 mL/min.The switch volume(VCM) was 2 400 mL.RESULTS Under the chosen condition,the preparetion yielded 71 mg,21 mg and 53 mg of ginsenoside-Rg1,Rf and Rd with a purity of 96.2%,94.3% and 95.1% by HPLC from 300 mg crude sample,respectively.CONCLUSION EECCC is a rapid and simple counter-current chromatography technique,which is effective for separation and purification of the solutes with larger partition coefficient(KD) values.
Keywords:high speed counter-current chromatography  elution-extrusion counter-current chromatography  ginsenoside-Rg1  ginsenoside-Rf  ginsenoside-Rd
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