The aim of this work was the preparation and characterization of a new sorbent material for solid phase extraction (SPE) from silica metallization with Ti and thermal immobilization of poly(methyloctadecylsiloxane)(PMODS) under three experimental conditions: 80 ºC for 8 h, 100 ºC for 17.36 h and 120 ºC for 16 h. The results of physicochemical characterization showed that Ti was incorporated at silica support with 33.2% (w/w), and the efficiency of immobilization of PMODS onto the surface of the metallized support in all three conditions (Figure 1). The determination of breakthrough volume (Vb), using aqueous media fortified with the pesticides methomyl, imidacloprid, carbofuran, diuron, tebuconazole, carbosulfan, by the construction of the Vb curves, showed a good sorptive capacity for solid phase extraction of the analytes, with good retentivity, especially in the condition 100 ºC for 17.36 h (Figure 2), where the Si-Ti(PMODS) phase shows adequate recovery for most analytes studied according to ANVISA criteria (ANVISA, 2017).