期刊
JOURNAL OF CHROMATOGRAPHY A
卷 1156, 期 1-2, 页码 35-44出版社
ELSEVIER
DOI: 10.1016/j.chroma.2006.12.028
关键词
monolithic silica capillary columns; reversed-phase; polymerization; HPLC
High efficiency and highly retentive monolithic silica capillary columns were obtained by polymerization of octaclecyl methacrylate using alpha,alpha '-azobis-isobutyronitrile (AIBN) as a free radical initiator. Hybrid type monolithic silica columns (25 cm total length x 200 mu m I.D.) prepared from a mixture of tetramethoxysilane and methyltrimetboxysilane were used as a support. The effects of the monomer and the radical initiator concentrations in the reaction mixture were examined. The performance of the columns was tested in terms of column efficiency and retention behavior by using alkylbenzenes and a few other compounds as solutes and compared with that of hybrid monolithic silica columns modified with octadecylsilyl-N,N-diethylamino)silane (ODS-DEA). Highly retentive monolithic silica columns were obtained by polymerization at high monomer concentrations. Although a decrease in column efficiency was observed with the increase in the monomer concentration in a feed mixture, an improvement in efficiency was achieved (a plate height value lower than 10 mu m) by increasing an initiator concentration without significant variations in column retention properties. Results obtained by polymerization using other monomers are also presented to demonstrate the applicability of the preparation method. (c) 2006 Elsevier B.V. All rights reserved.
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