Design of experiments for enantiomeric separation in supercritical fluid chromatography

Journal of Pharmaceutical and Biomedical Analysis
Elodie LandagarayEmmanuelle Lipka

Abstract

A new chiral melatoninergic ligand, potentially successor of Valdoxan(®), presenting an improved pharmacological profile with regard to agomelatine, was chosen as a probe for a supercritical fluid chromatographic separation carried-out on an amylose tris[(S)-1-α-methylbenzylcarbamate] based stationary phase. The goal of this work was to optimize simultaneously three factors identified to have a significant influence to obtain the best resolution in the shortest analysis time (i.e., retention time of the second eluting enantiomer) for this chiral compound. For this purpose a central circumscribed composite (CCC) design was developed with three factors: the flow-rate, the pressure outlet and the percentage of ethanol to optimize of two responses: shortest analysis time and best resolution. The optimal conditions obtained via the optimizer mode of the software (using the Nelder-Mead method) i.e., CO2/EtOH 86:14 (v:v), 104bar, 3.2mLmin(-1) at 35°C lead to a resolution of 3.27 in less than 6min. These conditions were transposed to a preparative scale where a concentrated methanolic solution of 40mM was injected with a sample loop of 100μL. This step allowed to separate an amount of around 65mg of racemic melatonin ligand in only 3h ...Continue Reading

References

Apr 11, 2008·Journal of Separation Science·Debby Mangelings, Yvan Vander Heyden
Jul 22, 2008·Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences·Larry Miller, Matt Potter
Nov 11, 2008·Journal of Chromatography. a·E Lesellier
Aug 4, 2009·Electrophoresis·Babak JamaliSteen Honoré Hansen
May 26, 2010·Analytical Chemistry·Timothy J Ward, Karen D Ward
Jan 29, 2011·Journal of Chromatography. a·Georges Guiochon, Abhijit Tarafder
Jun 5, 2012·Journal of Chromatography. a·Larry Miller
Jun 19, 2012·Journal of Chromatography. a·Arvind Rajendran
Dec 19, 2012·Journal of Pharmaceutical and Biomedical Analysis·Iolanda NistorEric Rozet
Apr 8, 2014·Analytica Chimica Acta·Květa KalíkováEva Tesařová
Mar 31, 2015·Journal of Pharmaceutical and Biomedical Analysis·Vincent DesfontaineLucie Nováková

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Citations

Aug 16, 2016·Journal of Chromatography. a·David Speybrouck, Emmanuelle Lipka
Mar 25, 2019·Journal of Pharmaceutical and Biomedical Analysis·Angéline NoireauCaroline West

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