Sintered octadecylsilica as monolithic column packing in capillary electrochromatography and micro high-performance liquid chromatography

Fused-silica capillaries were packed with porous 6-mu m octadecylated silica microspheres and subjected to thermal treatment in order to obtain a column with porous silica based monolithic packing. After sintering, the monolithic packing was reoctadecylated in situ with dimethyloctadecylchlorosilane. The mechanical strength and stability of the monolithic column were significantly greater than those of conventional columns packed with particulate stationary phase. The performance of the columns was evaluated in both mu-HPLC and capillary electrochromatography (CEC) of small aromatic compounds and polycyclic aromatic hydrocarbons with 10 mM berate, pH 8.0, in acetonitrile-water mixtures as the mobile phase. Since no untoward bubble formation was observed, CEC could be performed in a CZE unit without the need for pressurizing the monolithic column. The plate efficiency of the monolithic column was similar to that of columns freshly packed with the same particles and was always higher in the CEC than in the mu-HPLC under otherwise identical conditions. The electrosmotic flow (EOF) velocity increased with the acetonitrile content of the eluent in open fused-silica capillaries with octadecylated innerwall and in columns packed with sintered octadecylsilica. In contradistinction, the EOF velocity decreased with the organic strength of the eluent in raw fused-silica capillaries. The opposite trend is attributed to the different effect of changing organic modifier concentration on the accessibility of silanol groups at the raw and octadecylated silica surfaces. (C) 1998 Elsevier Science B.V.