Mesoporous materials based on aluminophosphates and silicates have been synthesised and impregnated with different loadings of transition metals such as Ag, Cu and Ni. These materials have been characterised and tested as selective adsorbents for the desulphurization of light cycle oil (LCO) by liquid adsorption. The polarity of the adsorbent matrix showed a positive effect on desulphurization, leading the impregnated aluminophosphates to higher adsorption capacities than the silicates. Among the transition metals tested, Ag-impregnated materials showed the best results followed by Cu and Ni. The aluminophosphate synthesised using pluronic F-127 block copolymer impregnated with a 5% of Ag (MFAP-5Ag) presented the best adsorption results with a maximum adsorption capacity of 11.36 mg S/g of adsorbent (equilibrium experiments), and breakthrough and saturation capacities of 4.25 mgS/g and 7.06 mgS/g, respectively (dynamic experiments).