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Purification method development for chiral separation in supercritical fluid chromatography with the solubilities in supercritical fluid chromatographic mobile phases

Purification method development for chiral separation in supercritical fluid chromatography with the solubilities in supercritical fluid chromatograph

Purification method development for chiral separation in supercritical fluid chromatography with the solubilities in supercritical fluid chromatographic mobile phases   (Citations: 2)
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A comprehensive approach was applied to develop a chiral purification method for an analyte that was found to be unusually difficult to scale-up in supercritical fluid chromatography (SFC). This was performed by studying major factors such as the solubility of an analyte in SFC mobile phases, impurity profiles, and cycle time. For this case study, the solubility in SFC mobile phase was measured by a packed column technique, coupled with a novel trapping mechanism to enhance measurement precision in SFC conditions. The solubility studies in SFC mobile phases suggested a couple of possible SFC mobile phases, in which the analyte would potentially be most soluble. The SFC methods were developed to purify a sample containing 15% of an impurity, after considering impurity profiles and cycle times of several potential methods in addition to SFC mobile phase solubility. An equal volume mixture of acetonitrile and ethanol was chosen for the final purification method, since this mixture demonstrated the relatively high SFC solubility among all solvent combinations with enhanced resolution between the analyte and the impurity as well as the shortest run time. The solubility of the compound was also determined in various organic solvents using a high throughput solubility screening system to better understand relative change of solubility from neat solution to SFC mobile phases.
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    • ...Recently, packed column supercritical Xuid chromatography (pSFC) becomes increasingly important in the enantiomeric separation since it oVers several advantages over HPLC such as higher eYciency, much less solvents consumed, ease of disposal and solute recovery in preparative separation [12, 13]...
    • ...Again -C 11 and -C 12 gave no resolution whether MeOH, EtOH or MeCN used, while in comparison IPA proved the best for the resolution of -C7–-C10 [13, 16, 18], as illustrated in Table 1 on -C 8 ...
    • ...These observations were similar to what had been reported previously [13, 19, 20]...

    Jian-Chun Xieet al. Resolution of racemic δ-lactone flavors on Chiralcel OB by packed colu...

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