Characterization and use of hydrophilic interaction liquid chromatography type stationary phases in supercritical fluid chromatography

• Published in: Journal of Chromatography A Vol. 1250; pp. 182 - 195
• Main Authors: West, Caroline, Khater, Syame, Lesellier, Eric
• Format: Journal Article
• Language: English
• Published: Netherlands Elsevier B.V 10.08.2012
• Subjects: barbiturates; benzodiazepines; Carbon Dioxide - chemistry; Chromatography, Supercritical Fluid - instrumentation; Chromatography, Supercritical Fluid - methods; Cluster Analysis; high performance liquid chromatography; hydrophilic interaction chromatography; Hydrophilic interaction liquid chromatography; Hydrophobic and Hydrophilic Interactions; Methanol - chemistry; Method development; molecular weight; Organic Chemicals - chemistry; Organic Chemicals - isolation & purification; Principal Component Analysis; propionic acid; Quantitative Structure-Activity Relationship; Quantitative structure–retention relationships; silica; Solvation parameter model; Stationary phases; Supercritical fluid chromatography; Hydrophilic interaction liquid chromatography; Quantitative structure–retention relationships; Stationary phases; Method development; Solvation parameter model; Supercritical fluid chromatography
• ISSN: 0021-9673; 1873-3778
• DOI: 10.1016/j.chroma.2012.05.008

► Eleven HILIC-type columns are characterized in SFC with over hundred test compounds. ► Three clusters of stationary phases are defined based on chemometric data treatment. ► Quantitative structure–retention relationships unravel retention mechanisms. All stationary phase chemistries are useful to achiral packed-column supercritical fluid chromatography (pSFC), but the majority of recent applications are based on polar stationary phases of the type used in normal-phase HPLC. Some manufacturers have recently introduced pSFC-tailored stationary phases, while others simply advocate the use of selected HPLC columns among their brands for SFC use. Indeed, any column developed for HPLC use can be used with supercritical fluids. Besides, hydrophilic interaction liquid chromatography (HILIC) is facing an increasing interest. Consequently, a number of HILIC-devoted stationary phases are now commercialized by most column manufacturers. As HILIC stationary phases are polar, their possible use in pSFC seems obvious, although literature examples are not numerous. However, whether they provide acceptable peak shapes in SFC conditions is a serious concern for them to find applicability. Indeed, columns optimized for HILIC mobile phases may not be optimum for SFC mobile phases. We present the characterization of eleven HILIC-type stationary phases used with carbon dioxide–methanol mobile phases in the isocratic mode. The columns are compared in terms of their retention and separation characteristics assessed by the solvation parameter model, and based on peak shapes. For this purpose, hundred and forty-six low molecular weight molecules, comprising neutral, basic and acidic compounds, were eluted on each column. Data analysis is carried out with hierarchical cluster analysis and principal component analysis in order to define three clusters of columns with similar selectivity: the first cluster comprises neutral stationary phases like amide and diol phases; the second one comprises basic stationary phases like aminopropyl-bonded silica; the last cluster comprises bare silica stationary phases. Sample applications with three different test mixtures relevant to pharmaceutical applications (barbiturates, benzodiazepines and propionic acids) are presented to assess the complementarity of some selected columns.