Analytical Sciences

Enhancement of Retentivity and Selectivity for PAHs in NP-HPLC by High-density Immobilization of Poly(4-vinylpyridine) as an Organic Phase on Silica

Usha GHIMIRE GAUTAM, Mani P. GAUTAM, Tsuyoshi SAWADA, Makoto TAKAFUJI, and Hirotaka IHARA

Department of Applied Chemistry and Biochemistry, Kumamoto University, 2-39-1 Kurokami, Kumamoto 860-8555, Japan

Poly(4-vinylpyridine)-modified silica with high grafting density have been prepared by a grafting-from (g-from) approach through radical chain-transfer reactions. The widely used silane coupling agent 3-mercaptopropyltrimethoxysilane was used to prepare thiol-terminated silica. Chain-transfer reaction and polymerization of 4-vinylpyridine was carried out using α,α′-azobisisobutyronitrile as an initiator. Thiol-terminated silica and polymer-modified silica were both characterized qualitatively and quantitatively. The quantification of the organic phase has been done by thermogravimetric analysis and elemental analysis. Thus, the modified silica was used as a packing material and the retention behavior of polycyclic aromatic hydrocarbons (PAHs) was studied in normal-phase high-performance liquid chromatography. Results were compared with those of poly(4-vinylpyridine)-modified silica prepared by a grafting-to (g-to) approach. Commercially available aminopropyl-bonded silica and bare silica columns were also used as reference columns. The column of poly(4-vinylpyridine)-grafted silica prepared by the g-from method, having higher grafting density, provided the better retentivity and selectivity for PAHs compared to the other reference columns.

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