Utilize este identificador para referenciar este registo: http://hdl.handle.net/10198/8458
Título: Separation of nadolol stereoisomers by chiral liquid chromatography at analytical and preparative scales
Autor: Ribeiro, António E.
Rodrigues, A.E.
Pais, L.S.
Palavras-chave: Multicomponent chiral separations
Pharmaceutical intermediate;
Nadolol stereoisomers
Preparative chiral separation
Simulated moving bed chromatography
Data: 2013
Editora: Wiley
Citação: Ribeiro, A. E.; Rodrigues, A. E.; Pais, L. S. (2013) - Separation of nadolol stereoisomers by chiral liquid chromatography at analytical and preparative scales. Chirality. ISSN 1520-636X. 25:3, p. 197-205
Resumo: The separation of the four nadolol stereoisomers on ChiralpakW AD by chiral liquid chromatography was carried out at both analytical and preparative scales. A screening of possible mobile-phase compositions was performed using different alcohol–hydrocarbon mixtures. The results obtained confirm the use of 20:80:0.3 ethanol-hexane-diethylamine reported by McCarthy (1994) but introduce other possibilities for the complete resolution of the four nadolol stereoisomers at analytical scale, namely, the mixtures 30–40:70–60:0.3 ethanol-heptane-diethylamine. Additionally, this work describes how retention and resolution depend on the ethanol content in hexane and heptane mixtures. The separation of nadolol stereoisomers is also carried out at preparative scale and different alcohol–hydrocarbon compositions are proposed, depending on the target component to be obtained. Particularly, this work presents the experimental separation of the more retained nadolol stereoisomer (RSR-nadolol) by simulated moving bed (SMB) chromatography using an 80:20:0.3 ethanol-heptane-diethylamine mobile phase. For a 2 g/l feed concentration, RSR-nadolol is 100% recovered at the extract outlet stream, 100% pure, and with a system productivity of 0.65 gRSR-nadolol/(lbed . h) and a solvent consumption of 9.6 lsolvent/gRSR-nadolol.
Peer review: yes
URI: http://hdl.handle.net/10198/8458
Versão do Editor: http://onlinelibrary.wiley.com/doi/10.1002/chir.v25.3/issuetoc
Aparece nas colecções:CIMO - Artigos em Revistas Indexados ao WoS/Scopus

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