高速逆流色谱分离技术解析.pptVIP

Introduction of Countercurrent Chromatography, CCC Table 1 Partition coefficients and separation factors (a) of honokiol and magnolol 高速逆流色谱分离与纯化 PH区带精制逆流色谱 PH Zone Refining CCC Preparative separation of salvianolic acids from the crude extract of Salvia miltiorrhiza Bunge by PH-Z-CCC Journal of Separation Science 2007 Structure of salvianolic acid B Chromatogram of the crude extract from S. miltiorrhiza Bunge by pH-z- CCC separation. Solvent system: MtBE–water (1:1, v/v), 10 mM TFA in the upper organic stationary phase and 10 mM aqueous ammonia in the lower phasesample size: 2.0 g; (Crude sample) 1 2 3 （A） 1 (B) 3 (C) 2 Preparative separation of cichoric acid from Echinacea Purpurea by pH-zone-refining counter-current chromatography Journal of Chromatography A, 2006， 1103，166-169 () () b a 采用MTBE-乙腈-水系统，以三氟乙酸为保留酸，氨水为洗脱碱，分离紫锥菊提取物，从3.0提取物中获得563mg，纯度为95%的菊苣酸 Preparative separation of alkaloids from the crude extract of Corydalis decumbens Journal of Chromatography A, 1115 (2006) 267–270 Analysis and identification Selection of solvent system Sample Separation by pH zone refining CCC Sample preparation Extracted by 95% EtOH Residue 1%HCl deposit Acidic extract NH3-water ● Selection of solvent system ● Kbase 1 ● Good solubility of the sample in the solvent ● Kacid 1 MtBE : H2O =1:1 MtBE : CH3CN:H2O=2:2:3 system Ⅰ Ⅱ Ⅲ (A) (B) (C) Ⅲ Ⅲ Ⅱ Ⅱ Ⅰ Ⅰ Fig.2. pH-Zone-refining CCC separation of the extract from C. decumbens. (A) retainer: 5 mM TEA, eluter: 5 mM HCl; (B) retainer: 10 mM TEA, eluter: 10 mM HCl 10 mM (C) retainer: 10 mM TEA, eluter: 10 mM HCl A B C 3 2 1 A C 3 D protopine tetrahydropalmatine bicuculline Preparative separation of neferine from Nelumbo nucifera Gaertn by pH-zone-refining counter-current chromatography Fig. 1. Structure of neferine Fig. 2 Chromatogram of the crude neferine extracted from Nelumbo nucifera Gaertn by pH-zone-refining counter-current chromatography (C) Fig. 3.