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

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

Journal of chromatography. A (2006-06-30)
Eldra Delannay, Alix Toribio, Leslie Boudesocque, Jean-Marc Nuzillard, Monique Zèches-Hanrot, Emmanuel Dardennes, Gwennaël Le Dour, Janos Sapi, Jean-Hugues Renault
ABSTRACT

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 elution 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.

MATERIALS
Product Number
Brand
Product Description

Supelco
Acenaphthylene, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
Supelco
Acenaphthylene, analytical standard
Sigma-Aldrich
Acenaphthylene, 99%
Sigma-Aldrich
Acenaphthylene, 75%