Synthesis and characterization of silica-based hyper-crosslinked sulfonate-modified reversed stationary phases

Hao Luo, Lianjia Ma, Yu Zhang, Peter W. Carr

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19 Scopus citations


A novel type of silica-based sulfonate-modified reversed phase (-SO3-HC-C8) has been synthesized; it is based on a newly developed acid stable "hyper-crosslinked" C8 derivatized reversed phase, denoted HC-C8. The -SO3-HC-C8 phases containing controlled amounts of sulfonyl groups were made by sulfonating the aromatic hyper-crosslinked network of the HC-C8 phase at different temperatures. The -SO3-HC-C8 phases are only slightly less hydrophobic than the parent HC-C8 phase. The added sulfonyl groups provide a unique strong cation-exchange selectivity to the hydrophobic hyper-crosslinked substrate as indicated by the very large C coefficient as shown through Snyder's hydrophobic subtraction reversed-phase characterization method. This cation-exchange activity clearly distinguishes the sulfonated phase from all other reversed phases as confirmed by the very high values of Snyder's column comparison function Fs. In addition, as was found in previous studies of silica-based and zirconia-based reversed phases, a strong correlation between the cation-exchange interaction and hydrophobic interaction was observed for these sulfonated phases in studies of the retention of cationic solutes. The overall chromatographic selectivity of these -SO3-HC-C8 phases is greatly enhanced by its high hydrophobicity through a "hydrophobically assisted" ion-exchange retention process.

Original languageEnglish (US)
Pages (from-to)41-55
Number of pages15
JournalJournal of Chromatography A
Issue number1
StatePublished - Feb 22 2008

Bibliographical note

Funding Information:
We thank the National Institutes of Health for the financial support. We also thank Agilent Technologies Inc. (Wilmington, DE, USA) for the donation of Zorbax silica and SB C 18 phases.


  • Basic analytes
  • Cation exchange
  • HPLC
  • Reversed phase
  • Selectivity
  • Stationary phase


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