SILICA XEROGEL AS A CONTINUOUS COLUMN SUPPORT FOR HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

摘要

A preliminary study of the chromatographic performance and permeability of a continuous silica xerogel column under reversed-phase HPLC conditions was performed, A porous chromatographic support was synthesized inside a 0.32 mm i.d. x 13 cm fused silica tube from potassium silicate solution and derivatized with dimethyloctadecylchlorosilane. The plate height at 0.01 cm/s (0.5 mu L/min), near the apparent optimum Linear velocity, was about 65 mu m. The column efficiencies in terms of numbers of plates per meter were 5000 and 13 000 for ethyl benzoate (k = 0.8) and naphthalene (k = 2.0), respectively, at 0.5 mu L/min. The major parameter affecting column efficiency was the heterogeneous morphology of the xerogel, modifications to which are expected to improve chromatographic performance. The column provided efficiencies comparable to those reported for continuous polymeric columns but less than that previously reported for a continuous silica column, Gradient elution mode was demonstrated with a mixture of polycyclic aromatic hydrocarbons. The column was highly permeable, exhibiting a linear dependence of pressure to now rate and a back pressure of only 632 psi at 10 mu L/min when a 95% aqueous mobile phase was used.