Zirconia layer coated mesoporous silica microspheres with mesostructured cellular foams (MCFs) were prepared by NH(3)/water vapor-induced internal hydrolysis method. Zirconia layer coated MCF microspheres were characterized by SEM, XRD, N(2) sorption, UV, and chromatographic analysis, and explored for enrichment of phosphopeptides. ZrO(2)/MCF microspheres in solid-phase extraction (SPE) mode demonstrated much higher selectivity and higher efficiency towards phosphopeptide enrichment than bulk ZrO(2) particles. In particular, the selectivities of ZrO(2)/MCF microspheres towards multi-phosphopeptides are even higher than that of the widely used commercial TiO(2) microparticles. The ZrO(2)/MCF microspheres were also applied to enrich endogenous phosphopeptides from human serum, and twelve endogenous phosphorylated peptides could be specifically enriched.
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