Ion-pair supercritical fluid chromatography of metoprolol and related amino alcohols on diol silica
| Autor: | Olle Gyllenhaal, Bengt-Arne Persson, Lena Edström |
|---|---|
| Rok vydání: | 2006 |
| Předmět: |
Fluorocarbons
Chromatography organic chemicals Organic Chemistry Diol Temperature Diastereomer Chromatography Supercritical Fluid Stereoisomerism General Medicine Silicon Dioxide Biochemistry Analytical Chemistry chemistry.chemical_compound chemistry Phase (matter) Carbon dioxide Supercritical fluid chromatography Organic chemistry Methanol Sulfonic Acids Selectivity Triethylamine Metoprolol |
| Zdroj: | Journal of Chromatography A. 1134:305-310 |
| ISSN: | 0021-9673 |
| DOI: | 10.1016/j.chroma.2006.08.051 |
| Popis: | In this paper, a chromatographic system based on carbon dioxide with methanol as mobile phase, and diol silica as stationary phase has been investigated for metoprolol and related amino alcohols by addition of strong acids to systems with triethylamine base as primary additive. Standard conditions used were 10% of methanol, containing 24 mM of acid and 18 mM of triethylamine, in carbon dioxide with a flow rate of 1.5 ml min(-1). The column dimensions were 125 mm x 4 mm I.D. and kept at 40 degrees C with a back pressure of 150 bar. Effects on selectivity were stronger with trifluoroacetic acid than with ethanesulfonic acid. From a large set of related analytes, it was shown that selectivity changes were significant when the structure close to the nitrogen of the amino alcohol analyte differed. The stability of the column in the short time perspective was examined and it showed negligible changes. For a diastereoisomeric pair, not resolved in a basic system with triethylamine nor by addition of ethanesulfonic acid, resolution improved to about 2.1 with trifluoroacetic acid. The described approach offers a way to tune the selectivity of SFC systems when amines are analyzed without the need to change stationary phase for the chromatographic separation. |
| Databáze: | OpenAIRE |
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