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Use of a new pirkle‐type chiral stationary phase in analytical and preparative subcritical fluid chromatography of pharmaceutical compounds
Author(s) -
Blum Andrew M.,
Lynam Kenneth G.,
Nicolas Edgar C.
Publication year - 1994
Publication title -
chirality
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.43
H-Index - 77
eISSN - 1520-636X
pISSN - 0899-0042
DOI - 10.1002/chir.530060414
Subject(s) - chemistry , enantiomer , chromatography , supercritical fluid chromatography , chiral stationary phase , high performance liquid chromatography , chiral column chromatography , phase (matter) , stationary phase , organic chemistry
Good results have been obtained with use of the new bonded chiral stationary phase Whelk‐O 1 in analytical and preparative subcritical fluid chromatography. A wide variety of enantiomeric pairs of compounds with different functional groups that are of pharmaceutical and biological interest have been resolved. This Pirkle‐concept CSP appears to be more rugged than cellulosic phases (e.g., Chiralcel) with regards to solvents and pressure. In comparing the usefulness of the column for SFC versus HPLC chiral analysis, we have observed a clear superiority of SFC in terms of higher speed and efficiency of analysis, and faster method development. This is consistent with our experience with Chiralcel CSPs. With the Whelk‐O 1 we have shown that the effects of temperature and modifier on SFC separations are similar to what has been reported for most other CSPs. We also observed a unique selectivity advantage of SFC for verapamil. We had good success with using a 1‐in. diameter column packed with Whelk‐O 1 to perform preparative SFC separations of a number of enantiomeric mixtures. The advantages of preparative SFC over preparative HPLC will be discussed. The feasibility of preparative SFC is dependent on how well we meet the practical challenges such as sample introduction issues, special hardware requirements due to the high pressure, and fraction collection issues. © 1994 Wiley‐Liss, Inc.