Separação do racemato N-Boc-Rolipram pelo processo cromatografico de leito movel simulado utilizando fase estacionaria quiral tris-(3,5-dimetilfenilcarbamato de celulose) suportada em silica

AUTOR(ES)

Caroline Vieira Gonçalves

DATA DE PUBLICAÇÃO

2005

RESUMO

Chiral stationary phases (CSPs) have shown efficiency in racemate purification. Rolipram, (mais ou menos)-4-(3-(cyclopentyloxy)-4-methoxyphenyl)- pyrrolidin-2-one, is an antidepressant with significant pharmacological properties. The main objective of this work was Rolipram purification in the Chiral Stationary Phase tris(3,5-dimethylphenylcarbamoyl) cellulose supported on silica by Simulated Moving Bed continuous chromatography. CSP was synthesized and its properties were determined by physical and chemical analysis. Kinetics and equilibrium parameters of the N-Boc-Rolipram, effect of the temperature on the separation factor (a) and competitive isotherms of the racemic mixture were evaluated by adsorption experiments with columns packed with the synthesized CSP. The experiments in the 5MB unit were carried out under diluted conditions at room temperature. The N-Boc-Rolipram racemate was separated on the synthesized CSP by the 5MB continuous chromatographic processoHenry constants are discussed and reveal Selectivity elose to 1,20. Purity and enantiomeric excess of extract and raffinate streams were determined. Chemicals and physicals analyses of the CSP obtained find good agreement with theoretical results. The effects of the temperature on the separation factor show that adsorption process is controlled by the enthalpy. Both enantiomers adsorb similarly on the synthesized CSP, but detailed studies need to be making for a good understanding of the adsorption processoKinetics and equilibrium parameters show good performance of the synthesized CSP to separate the enantiomers, mainly R-Boc-Rolipram racemate.

ASSUNTO(S)

antidepressants adsortions drogas quirais antidepressivos separation technology separação (tecnologia) adsorção chiral drugs

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