Purification of high-throughput organic synthesis libraries by counter-current chromatography
| Autor: | Philip A. Searle, Jeffrey Y. Pan, Noah P. Tu, Jill E. Hochlowski, Frank L. Wagenaar |
|---|---|
| Rok vydání: | 2009 |
| Předmět: |
medicine.drug_class
Acylation Ibuprofen Carboxamide Biochemistry Chemical synthesis Analytical Chemistry Small Molecule Libraries chemistry.chemical_compound Countercurrent chromatography medicine Organic chemistry Dimethyl Sulfoxide Organic Chemicals Countercurrent Distribution Chromatography High Pressure Liquid Chromatography Dimethyl sulfoxide Elution Methanol Organic Chemistry Equipment Design General Medicine Solvent Solubility chemistry Ketoprofen Solvents Supercritical fluid chromatography Organic synthesis |
| Zdroj: | Journal of Chromatography A. 1216:4154-4160 |
| ISSN: | 0021-9673 |
| Popis: | Experiments were performed to evaluate whether counter-current chromatography (CCC) could function as an alternative purification method to reversed-phase high-performance liquid chromatography (RP-HPLC) and normal-phase supercritical fluid chromatography (SFC). RP-HPLC and SFC are the routine methods currently used in our high-throughput purification (HTP) facility for the purification of high-throughput organic synthesis (HTOS) libraries and medicinal chemistry reaction mixtures. Pre-equilibration of the solvent mixture layers was not mandatory for effective chromatography when hexanes–ethyl acetate–methanol–water (HEMW) solvent mixtures were used. Key to the use of CCC for high-throughput applications is the ability to effectively select a solvent system appropriate to each library member. Pilot-scale CCC elution time was used to estimate a starting solvent ratio and RP-HPLC retention time was then used to adjust solvent ratios within a particular library. It was also found that dimethyl sulfoxide (DMSO) and DMSO–methanol were suitable as sample injection solvents when using the HEMW solvent systems. |
| Databáze: | OpenAIRE |
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