Preparative separation of quinolines by centrifugal partition chromatography with gradient elution.

J Chromatogr A

Laboratoire de Pharmacognosie, Associé au CNRS (BIOCIS-UMR 8076), Université Paris Sud, Faculté de Pharmacie, Rue Jean-Baptiste Clément, F-92296 Châtenay-Malabry, France.

Published: September 2003

Centrifugal partition chromatography has been successfully applied to the separation of 2-alkylquinolines from liquid combinatorial synthesis crude samples. Original gradient elution using the ternary two-phase solvent systems heptane-water-acetonitrile and heptane-acetonitrile-methanol were used to separate them with high purity degrees. Part of the effluent was monitored with evaporative light scattering detection, for direct control, and the collected fractions were analyzed by thin-layer chromatography, GC, nuclear magnetic resonance spectroscopy and MS. It was thus possible to purify in one run more than 3 g of crude mixture using only 1.31 of solvents to obtain more than 300 mg of several alkylquinolines homologues with 99% purity and in less than 7 h.

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http://dx.doi.org/10.1016/s0021-9673(03)01020-3DOI Listing

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