Journal
JOURNAL OF CHROMATOGRAPHY A
Volume 1218, Issue 48, Pages 8617-8628Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2011.09.082
Keywords
Thermo-responsive polymer; Poly(N-isopropylacrylamide); Atom transfer radical polymerization; Polymer brush; Reaction solvent
Funding
- National Institute of Environmental Science (NIES)
- Japan Society for the Promotion of Science [20300169]
- Grants-in-Aid for Scientific Research [21390012, 20300169] Funding Source: KAKEN
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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. (C) 2011 Elsevier B.V. All rights reserved.
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