T. Loughlin et al., USE OF SUBCRITICAL FLUID CHROMATOGRAPHY FOR THE SEPARATION OF ENANTIOMERS USING PACKED CELLULOSE-BASED STATIONARY-PHASE, Chirality, 8(1), 1996, pp. 157-162
Investigations into the parameters affecting the enantiomeric separati
on of an intermediate in the synthesis of a drug targeted for cardiac
arrhythmia is presented. The separation was achieved under subcritical
fluid chromatography using CO2 modified with methanol and co-modifier
s isopropyl amine and methylene chloride. The stationary phase was a c
ellulose based stationary phase manufactured under the trade name Chir
acel OB. The results showed the addition of methylene chloride had a n
oticeable effect on resolution while the separation factor, alpha, rem
ained constant. The co-modifier, isopropyl amine, did not considerably
influence the resolution, or separation factor. Temperature studies w
ere performed in order to establish the thermodynamic parameters of th
e interaction between the enantiomers and the stationary phase. Plots
of ln k' vs. 1/T proved to be curved, while plots of ln or vs. 1/T wer
e linear. (C) 1996 Wiley-Liss, Inc.