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Selective capture of phosphopeptides prior to mass spectrometry analysis is necessary due to their low abundance and low ionization efficiency in complex biological samples.The design,synthesis and applications of novel materials are attracting our attention for improving the phosphopeptides enrichment specificity and recovery.In this study,hierarchical Ti-aluminophosphate-5 materials (TiAPO-5H,micropore diameter 7.3×7.3 (A)) with mesoporous structure were successfully synthesized and utilized to selectively capture phosphopeptides from complex peptide mixtures prior to matrix-assisted laser desorption/ionization time of flight mass spectrometry (MALDI-TOF MS) analysis.We found that additional mesopores were obtained by using glucose as a template agent,thereby enhancing the capacity of the materials,while improving the content of titanium could improve the efficiency for phosphopeptides enrichment.The hierarchical Ti-aluminophosphate-5 materials have great potential in the design and development of high performance separation and adsorption molecular sieve materials.We expect that further development of this type of material in optimized pore structure and composition will make progress in the application of bioanalysis.