Prediction of retention for pharmaceutical molecules in supercritical fluid chromatography : the synthesis and analysis of a library of sulfonamides
Prediction of retention for pharmaceutical molecules in supercritical fluid chromatography : the synthesis and analysis of a library of sulfonamides
A library of thirty-two sulfonamides was designed for analysis by supercritical fluid chromatography (SFC) with the aim of highlighting the relationship between properties of the test analytes and their chromatographic retention.
During a pilot study involving a restricted test set and using an isocratic approach with 20% methanol (MeOH) in carbon dioxide (CO2) as a mobile phase and three different stationary phase (2-ethyl-pyridyl, cyano and diol bonded silica), simple trends linking the retention time of the analytes to their structural features were identified.
Polycratic studies were undertaken on the test library using CO2-MeOH mobile phases (in the presence or absence of additive) and a 2-ethyl-pyridyl (2-EP) column.
Results obtained during the polycratic study showed a net improvement of peak shapes and a decrease in retention time when ammonium acetate was used as an additive in the mobile phase. The effects of increasing concentrations of ammonium acetate additive in supercritical fluid chromatography were studied on silica (Si), 2-ethyl-pyridine (2-EP) and endcapped 2-ethyl-pyridine (2-EP-C) stationary phases. The study involved the addition of increasing concentrations of ammonium acetate either in the mobile phase modifier (methanol) or in the sample solvent. The effects of ammonium acetate on the retention and the peak shape of the analyte were evaluated. Compounds that exhibited satisfactory chromatographic behaviour in the absence of the additive were virtually unaffected by its presence in mobile phase or sample solvent. Nevertheless, compounds that exhibited late elution and strongly tailing peak shapes when pure methanol was used showed dramatically improved chromatographic behaviour in the presence of the additive. Shorter retention was observed, not only when the modifier was introduced in the mobile phase but also when it was present in the sample solvent.
University of Southampton
Cazenave Gassiot, Amaury
f53d5438-9fad-4fd6-98f9-3e289205dcd7
2007
Cazenave Gassiot, Amaury
f53d5438-9fad-4fd6-98f9-3e289205dcd7
Cazenave Gassiot, Amaury
(2007)
Prediction of retention for pharmaceutical molecules in supercritical fluid chromatography : the synthesis and analysis of a library of sulfonamides.
University of Southampton, Doctoral Thesis.
Record type:
Thesis
(Doctoral)
Abstract
A library of thirty-two sulfonamides was designed for analysis by supercritical fluid chromatography (SFC) with the aim of highlighting the relationship between properties of the test analytes and their chromatographic retention.
During a pilot study involving a restricted test set and using an isocratic approach with 20% methanol (MeOH) in carbon dioxide (CO2) as a mobile phase and three different stationary phase (2-ethyl-pyridyl, cyano and diol bonded silica), simple trends linking the retention time of the analytes to their structural features were identified.
Polycratic studies were undertaken on the test library using CO2-MeOH mobile phases (in the presence or absence of additive) and a 2-ethyl-pyridyl (2-EP) column.
Results obtained during the polycratic study showed a net improvement of peak shapes and a decrease in retention time when ammonium acetate was used as an additive in the mobile phase. The effects of increasing concentrations of ammonium acetate additive in supercritical fluid chromatography were studied on silica (Si), 2-ethyl-pyridine (2-EP) and endcapped 2-ethyl-pyridine (2-EP-C) stationary phases. The study involved the addition of increasing concentrations of ammonium acetate either in the mobile phase modifier (methanol) or in the sample solvent. The effects of ammonium acetate on the retention and the peak shape of the analyte were evaluated. Compounds that exhibited satisfactory chromatographic behaviour in the absence of the additive were virtually unaffected by its presence in mobile phase or sample solvent. Nevertheless, compounds that exhibited late elution and strongly tailing peak shapes when pure methanol was used showed dramatically improved chromatographic behaviour in the presence of the additive. Shorter retention was observed, not only when the modifier was introduced in the mobile phase but also when it was present in the sample solvent.
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Published date: 2007
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Local EPrints ID: 466472
URI: http://eprints.soton.ac.uk/id/eprint/466472
PURE UUID: 307187d2-8ffc-4701-8f3c-635970f3992c
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Date deposited: 05 Jul 2022 05:18
Last modified: 16 Mar 2024 20:43
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Author:
Amaury Cazenave Gassiot
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