Synthesis, characterisation and chromatographic evaluation of pentafluorophenyl and phenyl bonded silica phases prepared using supercritical carbon dioxide as a reaction solvent

Ashu-Arrah, Benjamin A.; Glennon, Jeremy D.; Albert, Klaus

doi:10.1016/j.chroma.2012.11.041

Cited by 17 publications

(9 citation statements)

References 71 publications

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“…3). These results are consistent with previous results reported by AshuArrah et al [22,23,29,30]. Moreover, the slope of the TGA curve of Table 4 Zeta-potentials of thin-shell particles dispersed in methanol.…”

Section: Thermogravimetric Analysis (Tga)supporting

confidence: 95%

“…The three regions correspond to (a) a monolayer-multilayer adsorption on the pore walls, (b) followed by capillary condensation, and (c) multilayer adsorption on the outer surface. These findings are in good agreement with cited results in literature [9,[21][22][23]. The linear increase at low pressure is significantly larger compared to increase at higher pressures, thus indicating a larger surface area of pores compared with the outer layer, and in good agreement with previous results cited in literature [22,24].…”

Section: Bet Analysissupporting

confidence: 95%

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Sub-2-μm seeded growth mesoporous thin shell particles for high-performance liquid chromatography: Synthesis, functionalisation and characterisation

Langsi

Ashu-Arrah

Glennon

2015

Journal of Chromatography A

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Section: Thermogravimetric Analysis (Tga)supporting

confidence: 95%

Section: Bet Analysissupporting

confidence: 95%

Sub-2-μm seeded growth mesoporous thin shell particles for high-performance liquid chromatography: Synthesis, functionalisation and characterisation

Langsi

Ashu-Arrah

Glennon

2015

Journal of Chromatography A

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“…When fluorine is incorporated into bonded phases, it can promote ion-exchange type interactions with electron-deficient analytes. In the PFPP phase, five fluorines provide additional electrons, and as a result, the phase has the ability to polarize analytes [32,33]. With our model analyte set, it was clear that analytes containing protonated amines were retained longer on the PFPP phase compared to the aqueous C 18 phase.…”

Section: Pentafluorophenyl Propyl Phase Selectivitymentioning

confidence: 85%

Automated screening of reversed-phase stationary phases for small-molecule separations using liquid chromatography with mass spectrometry

et al. 2016

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There are various reversed-phase stationary phases that offer significant differences in selectivity and retention. To investigate different reversed-phase stationary phases (aqueous stable C18 , biphenyl, pentafluorophenyl propyl, and polar-embedded alkyl) in an automated fashion, commercial software and associated hardware for mobile phase and column selection were used in conjunction with liquid chromatography and a triple quadrupole mass spectrometer detector. A model analyte mixture was prepared using a combination of standards from varying classes of analytes (including drugs, drugs of abuse, amino acids, nicotine, and nicotine-like compounds). Chromatographic results revealed diverse variations in selectivity and peak shape. Differences in the elution order of analytes on the polar-embedded alkyl phase for several analytes showed distinct selectivity differences compared to the aqueous C18 phase. The electron-rich pentafluorophenyl propyl phase showed unique selectivity toward protonated amines. The biphenyl phase provided further changes in selectivity relative to C18 with a methanolic phase, but it behaved very similarly to a C18 when an acetonitrile-based mobile phase was evaluated. This study shows the value of rapid column screening as an alternative to excessive mobile phase variation to obtain suitable chromatographic settings for analyte separation.

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“…These values and the analogous quantities estimated by elemental analysis can be compared, as carbon content was determined before and after end-capping of both silicas. [63][64][65] Simple calculations based on C content [63] show that for the PFP cap -SP 698 mmol of silanol groups per gram of native silica were end-capped as opposed to 968 mmol g À1 for native silica during the anchoring of perfluoroaryl groups. Therefore, the ratio between end-capped silanol groups and PFP-siloxane silicon atoms estimated by elemental analysis is 0.7 [cf.…”

Section: Quantitative Analysis Of Reacted Silanol Groupsmentioning

confidence: 99%

Revealing the Fine Details of Functionalized Silica Surfaces by Solid‐State NMR and Adsorption Isotherm Measurements: The Case of Fluorinated Stationary Phases for Liquid Chromatography

Ciogli

Simone

Villani

et al. 2014

Chemistry A European J

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The structural and chromatographic characterization of two novel fluorinated mesoporous materials prepared by covalent reaction of 3-(pentafluorophenyl)propyldimethylchlorosilane and perfluorohexylethyltrichlorosilane with 2.5 μm fully porous silica particles is reported. The adsorbents were characterized by solid state (29)Si, (13)C, and (19)F NMR spectroscopy, low-temperature nitrogen adsorption, elemental analysis (C and F), and various chromatographic measurements, including the determination of adsorption isotherms. The structure and abundance of the different organic surface species, as well as the different silanol types, were determined. In particular, the degree of so-called horizontal polymerization, that is, Si-O-Si bridging parallel to the silica surface due to the reaction, under "quasi-dry" conditions, of trifunctional silanizing agents with the silica surface was quantified. Significant agreement was found between the information provided by solid-state NMR, elemental analysis, and excess isotherms regarding the amount of surface residual silanol groups, on the one hand, and the degree of surface functionalization, on the other. Finally, the kinetic performance of the fluorinated materials as separation media for applications in near-ultrahigh-performance liquid chromatography was evaluated. At reduced velocities of about 5.5 (ca. 600 bar backpressure at room temperature) with 3 mm diameter columns and toluene as test compound, reduced plate heights on the order of 2 were obtained on columns of both adsorbents.

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Synthesis, characterisation and chromatographic evaluation of pentafluorophenyl and phenyl bonded silica phases prepared using supercritical carbon dioxide as a reaction solvent

Cited by 17 publications

References 71 publications

Sub-2-μm seeded growth mesoporous thin shell particles for high-performance liquid chromatography: Synthesis, functionalisation and characterisation

Sub-2-μm seeded growth mesoporous thin shell particles for high-performance liquid chromatography: Synthesis, functionalisation and characterisation

Automated screening of reversed-phase stationary phases for small-molecule separations using liquid chromatography with mass spectrometry

Revealing the Fine Details of Functionalized Silica Surfaces by Solid‐State NMR and Adsorption Isotherm Measurements: The Case of Fluorinated Stationary Phases for Liquid Chromatography

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