Multiple dual-mode centrifugal partition chromatography, a semi-continuous development mode for routine laboratory-scale purifications

被引:80
作者
Delannay, Eldra [1 ]
Toribio, Alix [1 ]
Boudesocque, Leslie [1 ]
Nuzillard, Jean-Marc [1 ]
Zeches-Hanrot, Monique [1 ]
Dardennes, Emmanuel [1 ]
Le Dour, Gwennael [1 ]
Sapi, Janos [1 ]
Renault, Jean-Hugues [1 ]
机构
[1] Univ Reims, IFR 53, FRE CNRS 2715, F-51687 Reims 2, France
关键词
D O I
10.1016/j.chroma.2006.05.069
中图分类号
Q5 [生物化学];
学科分类号
071010 [生物化学与分子生物学]; 081704 [应用化学];
摘要
Nowadays, centrifugal partition chromatography (CPC) separations can be routinely achieved at the laboratory scale. The solvent system selection has been made easy, as generic sets of solvent systems are described in publications and books. This approach, however, generally reduces the scope of optimization strategies for two important parameters: selectivity and sample solubility. This can be very limiting for the preparative separation of structurally similar compounds. Multiple dual-mode (MDM) CPC has been developed to provide an easy-to-use alternative technique to circumvent this problem. A MDM separation consists of a succession of dual-mode runs (i.e. multiple inversion of stationary and mobile phase) that can only be achieved because both chromatographic phases are liquids. This original elation mode is thus a semi-continuous process with a classical sample injection and which only requires a single CPC column. Underlying mechanisms of MDM were studied using a model mixture of acenaphthylene and naphthalene. A mixture of two synthetic pairs of diastereomers was then successfully submitted to MDM CPC, in the framework of the synthesis of biologically active compounds. (c) 2006 Elsevier B.V. All rights reserved.
引用
收藏
页码:45 / 51
页数:7
相关论文
共 18 条
[1]
[Anonymous], 1994, CHROMATOGRAPHIC SCI
[2]
Alkane effect in the Arizona liquid systems used in countercurrent chromatography [J].
Berthod, A ;
Hassoun, M ;
Ruiz-Angel, MJ .
ANALYTICAL AND BIOANALYTICAL CHEMISTRY, 2005, 383 (02) :327-340
[3]
BERTHOD A, 2002, WILSON WILSONS COMPR, V38
[4]
COUILLARD F, Patent No. 2856933
[5]
PREPARATIVE CHROMATOGRAPHIC RESOLUTION OF RACEMATES ON CHIRAL STATIONARY PHASES ON LABORATORY AND PRODUCTION SCALES BY CLOSED-LOOP RECYCLING CHROMATOGRAPHY [J].
DINGENEN, J ;
KINKEL, JN .
JOURNAL OF CHROMATOGRAPHY A, 1994, 666 (1-2) :627-650
[6]
Counter-current chromatography: instrumentation, solvent selection and some recent applications to natural product purification [J].
Foucault, AP ;
Chevolot, L .
JOURNAL OF CHROMATOGRAPHY A, 1998, 808 (1-2) :3-22
[7]
FOUCAULT AP, 1994, CHROMATOGRAPHIC SCI, V68, P87
[8]
Resolution of a racemic pharmaceutical intermediate - A comparison of preparative HPLC, steady state recycling, and simulated moving bed [J].
Grill, CA ;
Miller, L ;
Yan, TQ .
JOURNAL OF CHROMATOGRAPHY A, 2004, 1026 (1-2) :101-108
[9]
Closed-loop recycling with periodic intra-profile injection: a new binary preparative chromatographic technique [J].
Grill, CM .
JOURNAL OF CHROMATOGRAPHY A, 1998, 796 (01) :101-113
[10]
Application of the "VARICOL" process to the separation of the isomers of the SB-553261 racemate [J].
Ludemann-Hombourger, O ;
Pigorini, G ;
Nicoud, RM ;
Ross, DS ;
Terfloth, G .
JOURNAL OF CHROMATOGRAPHY A, 2002, 947 (01) :59-68