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Advisor(s)
Abstract(s)
Chiralpak IA adsorbent is used for both analytical and preparative chromatographic
separation of nadolol stereoisomers. The results include a complete screening of the
mobile phase composition for both the baseline resolution of all four nadolol stereoisomers
(analytical separation) and the simulated moving bed (SMB) pseudo-binary separation of the
most retained stereoisomer. The experimental results show that analytical baseline resolution
of nadolol stereoisomers can be achieved using alcohol/hydrocarbon and alcohol/acetonitrile
solvent mixtures. The 10%ethanol/90%acetonitrile mixture is presented as the one that presents
baseline resolution with lower retention. For the preparative pseudo-binary separation, pure
ethanol, pure methanol, alcohol/acetonitrile, and alcohol/tetrahydrofuran mixtures proved to
allow good separation results. The 100%methanol/0.1%diethylamine solvent composition was
selected to perform the experimental SMB separation. Using a 10 g/L total feed concentration,
the more retained stereoisomer was recovered at the extract outlet stream with 99.5% purity,
obtaining a system productivity of 1.98 gL-1 h-1 and requiring a solvent consumption of
3.13 L/g of product. Comparing these results with the ones recently presented by Ribeiro et al.
(2013), this work shows that the Chiralpak IA chiral adsorbent is an interesting alternative to
Chiralpak AD for the separation of nadolol stereoisomers at both analytical and preparative
scales.
Description
Keywords
Chiral liquid chromatography Immobilized chiral stationary phase Nadolol stereoisomers Screening of solvents
Citation
Arafah, Rami; Ribeiro, António E.; Rodrigues, A.E.; Pais, L.S. (2016). Separation of Nadolol Stereoisomers Using Chiralpak IA Chiral Stationary Phase. Chirality. ISSN 0899-0042. 28:5, p. 399-408
Publisher
Wiley