Selective extraction of low molecular weight ( LMW) proteins and peptides from complex biological samples plays an important role in the discovery of useful biomarkers and signaling molecules. It is demonstrated that the unique pore structure of mesoporous material makes it efficient to enrich LMW proteins and peptides from complex matrixes. In this study, a mesoporous material, alkyl-diol@ phenyl-SiO2 , with modified exterior ( alkyl-diol group) and interior ( phenyl group) surfaces, was synthesized by co-condensation and post-grafting, and its characteristic was evaluated by FTIR and MS. The LMW proteins and peptides enriched by the alkyl-diol@phenyl-SiO2 mesoporous material could be easily eluted by organic solvents, which was compatible with the following detection by mass spectrometry ( MS ) . This new mesoporous material exhibited good selectivity for the extraction of LMW proteins and peptides ( less than 10 kDa) from complex biological samples.