This work describes the preparation and characterization of two stationary phases based on the immobilization of poly(methyltetradecylsiloxane) onto doubly titanized silica particles. Chromatographic tests indicate that these metallized silica-based stationary phases present similar chromatographic performance for apolar and polar compounds to those obtained for their bare silica-based counterparts. Spectroscopic characterizations indicate high residual silanol quantities on titanized silica-based stationary phases; however, this fact does not contribute to a high asymmetry factor for basic compounds as is usually found with titania-based stationary phases. These stationary phases may be useful for analysis of pharmaceuticals.6741795357363