Optimization of the synthesis of a hyper-crosslinked stationary phases: A new generation of highly efficient, acid-stable hyper-crosslinked materials for HPLC

Yu Zhang, Yuming Huang, Peter W. Carr

Research output: Contribution to journalArticlepeer-review

8 Scopus citations

Abstract

A new family of hyper-crosslinked (HC) phases was recently developed for use under very aggressive conditions including those encountered in ultra-fast, high-temperature two-dimensional liquid chromatography (2-DLC). This type of stationary phase has improved acid stability compared with the most acid-stable, commercial RPLC phases. Kinetic studies are here reported that allow optimization of reaction time and crosslinking reagent concentrations used to prepare such HC phases. We have determined that the Friedel-Crafts chemistry used to prepare HC phases is nearly complete within about 15 min. Thus, reaction time for each step of the synthesis was greatly reduced from the multihour reactions used previously without sacrificing the stationary phases' acid stability and separation performance. Results from elemental analysis of the finished particles were combined with LC data to provide insights regarding the properties of these HC phases. This new generation of acid stable HC phases, with their attractive chromatographic properties, should be very useful in the separations of bases or biological analytes in acidic media, especially at elevated temperatures.

Original languageEnglish (US)
Pages (from-to)1407-1422
Number of pages16
JournalJournal of Separation Science
Volume34
Issue number12
DOIs
StatePublished - Jun 2011

Keywords

  • Acid stable
  • LC
  • RPLC
  • Stationary phase
  • Two dimensional

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