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Complete separation of nadolol stereoisomers by fixed-bed and simulated moving bed chromatography

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Resumo:This work deals with the identification of main experimental strategy for the complete separation of nadolol quaternary mixture into its pure four stereoisomers. Different chiral and achiral adsorbents, with different particle size diameters (5, 10 and 20 m) as well as several solvents and solvent mixtures (aqueous and organic) are used. The selected global strategy is based on two main steps. The first step is the achiral separation of nadolol racemates (two pairs of enantiomers) by high pH reversed-phase preparative chromatography using C18 adsorbents. Then, the second step is based on two parallel binary chiral separations using Chiralpak IA adsorbents. It is important to notice that both first and second steps can be accomplished by fixed-bed and simulated moving bed (SMB) technologies. The theoretical and experimental results show that SMB technology presents higher preparati performance when compared to the "equivalent" preparative fixed-bed operation.
Autores principais:Arafah, Rami
Outros Autores:Ribeiro, António E.; Rodrigues, Alírio; Pais, Luís S.
Assunto:Chromatography Nadolol Stereoisomers
Ano:2023
País:Portugal
Tipo de documento:documento de conferência
Tipo de acesso:acesso aberto
Instituição associada:Instituto Politécnico de Bragança
Idioma:inglês
Origem:Biblioteca Digital do IPB
Descrição
Resumo:This work deals with the identification of main experimental strategy for the complete separation of nadolol quaternary mixture into its pure four stereoisomers. Different chiral and achiral adsorbents, with different particle size diameters (5, 10 and 20 m) as well as several solvents and solvent mixtures (aqueous and organic) are used. The selected global strategy is based on two main steps. The first step is the achiral separation of nadolol racemates (two pairs of enantiomers) by high pH reversed-phase preparative chromatography using C18 adsorbents. Then, the second step is based on two parallel binary chiral separations using Chiralpak IA adsorbents. It is important to notice that both first and second steps can be accomplished by fixed-bed and simulated moving bed (SMB) technologies. The theoretical and experimental results show that SMB technology presents higher preparati performance when compared to the "equivalent" preparative fixed-bed operation.

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