Abstract:Within this review, we thoroughly explored supercritical fluid chromatography (SFC) columns used across > 3000 papers published from the first study carried out under SFC conditions in 1962 to the end of 2022. We focused on the open tubular capillary, packed capillary, and packed columns, their chemistries, dimensions, and trends in used stationary phases with correlation to their specific interactions, advantages, drawbacks, used instrumentation, and application field. Since the 1990s, packed columns with … Show more
“…Therefore, a small percentage of water in the organic modifier, i.e., 2–5%, could shift the equilibrium toward the free silanols and mitigate the SEF. Thus, the process of regeneration, where the column is washed with a large volume of water, is suggested to reverse the SEF. − However, the SEF phenomenon is still not well understood, and more detailed studies are necessary. Furthermore, organic acids, ammonia, water, and/or buffers can be added to the mobile phase, affecting the separation of acidic/basic analytes and their peak shapes.…”
mentioning
confidence: 99%
“…Polar stationary phases with predominant –OH functionalities have been used in more than 35% of published works . At the same time, the –OH functionalities of these phases are more prone to SEF .…”
mentioning
confidence: 99%
“…Polar stationary phases with predominant –OH functionalities have been used in more than 35% of published works . At the same time, the –OH functionalities of these phases are more prone to SEF . The well-established linear solvation energy relationship (LSER) classification sorts these columns among the polar stationary phases in two clusters (Supporting Information Figure S1): (i) nonbonded silica and hybrid silica and (ii) polar ligands bonded to the silica surface.…”
The retention behavior in supercritical fluid chromatography and its stability over time are still unsatisfactorily explained phenomena despite many important contributions in recent years, especially focusing on linear solvation energy relationship modeling. We studied polar stationary phases with predominant −OH functionalities, i.e., silica, hybrid silica, and diol columns, and their retention behavior over time. We correlated molecular descriptors of analytes with their retention using three organic modifiers of the CO 2 -based mobile phase. The differences in retention behavior caused by using additives, namely, 10 mmol/L NH 3 and 2% H 2 O in methanol, were described in correlation to analyte properties and compared with the CO 2 /methanol mobile phase. The structure of >100 molecules included in this study was optimized by semiempirical AM1 quantum mechanical calculations and subsequently described by 226 molecular descriptors including topological, constitutional, hybrid, electronic, and geometric descriptors. An artificial neural networks simulator with deep learning toolbox was trained on this extensive set of experimental data and subsequently used to determine key molecular descriptors affecting the retention by the highest extent. After comprehensive statistical analysis of the experimental data collected during one year of column use, the retention on different stationary phases was fundamentally described. The changes in the retention behavior during one year of column use were described and their explanation with a proposed interpretation of changes on the stationary phase surface was suggested. The effect of the regeneration procedure on the retention was also evaluated. This fundamental understanding of interactions responsible for retention in SFC can be used for the evidence-based selection of stationary phases suitable for the separation of particular analytes based on their specific physicochemical properties.
“…Therefore, a small percentage of water in the organic modifier, i.e., 2–5%, could shift the equilibrium toward the free silanols and mitigate the SEF. Thus, the process of regeneration, where the column is washed with a large volume of water, is suggested to reverse the SEF. − However, the SEF phenomenon is still not well understood, and more detailed studies are necessary. Furthermore, organic acids, ammonia, water, and/or buffers can be added to the mobile phase, affecting the separation of acidic/basic analytes and their peak shapes.…”
mentioning
confidence: 99%
“…Polar stationary phases with predominant –OH functionalities have been used in more than 35% of published works . At the same time, the –OH functionalities of these phases are more prone to SEF .…”
mentioning
confidence: 99%
“…Polar stationary phases with predominant –OH functionalities have been used in more than 35% of published works . At the same time, the –OH functionalities of these phases are more prone to SEF . The well-established linear solvation energy relationship (LSER) classification sorts these columns among the polar stationary phases in two clusters (Supporting Information Figure S1): (i) nonbonded silica and hybrid silica and (ii) polar ligands bonded to the silica surface.…”
The retention behavior in supercritical fluid chromatography and its stability over time are still unsatisfactorily explained phenomena despite many important contributions in recent years, especially focusing on linear solvation energy relationship modeling. We studied polar stationary phases with predominant −OH functionalities, i.e., silica, hybrid silica, and diol columns, and their retention behavior over time. We correlated molecular descriptors of analytes with their retention using three organic modifiers of the CO 2 -based mobile phase. The differences in retention behavior caused by using additives, namely, 10 mmol/L NH 3 and 2% H 2 O in methanol, were described in correlation to analyte properties and compared with the CO 2 /methanol mobile phase. The structure of >100 molecules included in this study was optimized by semiempirical AM1 quantum mechanical calculations and subsequently described by 226 molecular descriptors including topological, constitutional, hybrid, electronic, and geometric descriptors. An artificial neural networks simulator with deep learning toolbox was trained on this extensive set of experimental data and subsequently used to determine key molecular descriptors affecting the retention by the highest extent. After comprehensive statistical analysis of the experimental data collected during one year of column use, the retention on different stationary phases was fundamentally described. The changes in the retention behavior during one year of column use were described and their explanation with a proposed interpretation of changes on the stationary phase surface was suggested. The effect of the regeneration procedure on the retention was also evaluated. This fundamental understanding of interactions responsible for retention in SFC can be used for the evidence-based selection of stationary phases suitable for the separation of particular analytes based on their specific physicochemical properties.
scite is a Brooklyn-based organization that helps researchers better discover and understand research articles through Smart Citations–citations that display the context of the citation and describe whether the article provides supporting or contrasting evidence. scite is used by students and researchers from around the world and is funded in part by the National Science Foundation and the National Institute on Drug Abuse of the National Institutes of Health.