We have developed a smart nanodevice for the highly efficient and selective detection of glycoproteins. This polyfunctional device is fabricated through the rational functionalization of macroporous silica foam (MOSF) materials with a boron species (B-MOSF) and amino groups (NH(2)-MOSF), and then the integration of MOSF, B-MOSF and NH(2)-MOSF materials. In such a device, a macroporous structure with very large-pore sizes (diameters approximately 100 nm) and high-pore volumes (>0.65 cm(3) g(-1)) is advantageous to efficiently fasten the enzymatic reaction. The targeted specific glycopeptides of the products can be selectively isolated and enriched in B-MOSF through the chemo-affinity between boronic acid and glycol groups, while the non-specific peptides are released to the solutions, or further purified by MOSF and NH(2)-MOSF, which have opposite charges. As a result, the protein digestion and glycol-peptide isolation can be simultaneously achieved in the functionalized macroporous materials in one step, which is a great advantage compared to conventional multi-procedure and time-consuming techniques.