Preparation and characterization of poly(methyltetradecylsiloxane) stationary phases immobilized by gamma radiation onto zirconized silica

The preparation of stationary phases with enhanced chemical stability in alkaline eluents has been the principal objective of many chromatographers. New and improved silica substrates and advanced chemical modification methods are among the possibilities being investigated to reach this objective. The present work has evaluated these two possibilities for new stationary phases. First, the silica surface was modified by reaction with zirconium tetrabutoxide to produce zirconized silica particles having about 21% (w/w) of zirconium. Then poly(methyltetradecylsiloxane) (PMTDS) was immobilized onto this surface using different doses (50-120 kGy) of gamma radiation. These new phases were characterized using elemental analysis and infrared and solid-state (29)Si-nuclear magnetic resonance (NMR) spectroscopies. These new stationary phases presented column efficiencies of about 68,000 plates m(-1), symmetric peaks for apolar compounds and retention factors that depend on the irradiation dose and show improved stability in high pH mobile phases. The separation of several pharmaceuticals at pH 11 is presented.