CHROMATOGRAPHY

CHROMATOGRAPHY, Vol. 21 (2000), No. 3, pp. 209-216
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Original Paper
Preparation of Packing Materials for Temperature-Responsive Chromatography
Modification of Silica Surface with Poly (N-isopropylacrylamide)
Kazuo Yamamoto1), Hideko Kanazawa1)*, Yoshikazu Matsushima1),
Nobuharu Takai2), Akihiko Kikuchi3) and Teruo Okano3)
1) Kyoritsu College of Pharmacy, 1-5-30 Shibakoen, Minato-ku, Tokyo 105-8512, Japan
2) Faculty of Science and Engineering, Tokyo Denki University, Saitama 350-0394, Japan
3) Institute of Biomedical Engineering, Tokyo Women's Medical University,
8-1 Kawadacho, Shinju-ku, Tokyo 162-8666, Japan

Abstract:
Poly (N-isopropylacrylamide) (PIPAAm) with a carboxyl terminal was coupled with aminopropylsilica for preparation of packing materials of temperature-responsive chromatography. Several coupling methods were examined. The best results were obtained by the method, in which an active ester of the terminal carboxyl with succinimide was coupled in 1,4-dioxane. Scanning electron micrographs showed similar external appearances for both PIPAAm modified and unmodified silica, indicating the particle and pore sizes were essentially the same. With the packing material, five steroids and benzene were well separated with water as a sole mobile phase at a column temperature of 50, while they were poorly separated at 15, which is lower than the lower critical solution temperature of PIPAAm (32).
Keywords: Poly (N-isopropylacrylamide); temperature-responsive chromatography; packing material


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