Effect of reaction solvent on the preparation of thermo-responsive stationary phase through a surface initiated atom transfer radical polymerization

Kenichi Nagase, Aya Mizutani Akimoto, Jun Kobayashi, Akihiko Kikuchi, Yoshikatsu Akiyama, Hideko Kanazawa, Teruo Okano

Research output: Contribution to journalArticle

32 Citations (Scopus)

Abstract

Poly(N-isopropylacrylamide) (PIPAAm) brush grafted silica beads, a thermo-responsive chromatographic stationary phase, were prepared through a surface-initiated atom transfer radical polymerization (ATRP) using 2-propanol, N,N-dimethylformamide (DMF), and water as reaction solvents. The rate of grafting PIPAAm on silica bead surfaces was different and found to be dependent on the reactivity of reaction solvent. Temperature-dependent elution profiles of hydrophobic steroids from the prepared-beads-packed columns were found to be different, although the graft amounts of PIPAAm were similar on silica bead surfaces. Especially, prepared beads using 2-propanol exhibited a higher resolution than those using DMF. Calibration curves using glucose and pullulan suggested that beads prepared using DMF prohibited analytes to diffuse into the pores. On the contrary, beads prepared using 2-propanol allowed analytes to diffuse into the pores. The pore diameter of the prepared beads, measured by N 2 adsorption-desorption measurement, suggested that beads using 2-propanol has relatively larger pore diameter than those using DMF. Thus, the reaction solvent in surfaces-initiated ATRP affected the grafting configuration of PIPAAm on porous silica-bead surfaces, leading to the different separation efficiency of stationary phase for bioactive compounds.

Original languageEnglish
Pages (from-to)8617-8628
Number of pages12
JournalJournal of Chromatography A
Volume1218
Issue number48
DOIs
Publication statusPublished - 2011 Dec 2

Keywords

  • Atom transfer radical polymerization
  • Poly(N-isopropylacrylamide)
  • Polymer brush
  • Reaction solvent
  • Thermo-responsive polymer

ASJC Scopus subject areas

  • Analytical Chemistry
  • Biochemistry
  • Organic Chemistry

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