In the current study, a new method was developed to synthesize the hybrid mesoporous material with metallic oxides, MCM-48 with TiO2, at an improved efficiency and reduced cost. The results have shown an over 95% adsorption efficiency for trace metals for the hybrid MCM-48 with TiO2 materials, and a significantly improved maximum adsorption capacity compared to pure MCM-48. Its unique hybrid structured allows the polluted water to pass through the strong yet highly permeable structure of mesoporous material, while gives enough time for the pollutants to react with the TiO2 infused on the porous structure so that the polluted water can be treated without introducing secondary pollutants. The microstructures of the MCM-48 with and without TiO2 are characterized using SEM with EDS and Porosimiter. The effectiveness of wastewater treatment is measured using Inductively Couple Plasma-Mass Spectrometer (ICP-MS). The significant improvements observed here is likely due to the infused TiO2 to the base MCM-48 structure, which also agree with the authors’ previous finding. It is noticed that, while the higher concentration of TiO2 has a positive impact on the adsorption of trace metals, the higher concentration of Ti source does not necessarily yield significantly higher concentration of TiO2 in the final product. Future study is needed to further explore this hybrid mesoporous material for other pollutants treatment, and to obtain a further understanding of its mechanisms.