Mesoprous materials were successfully prepared in five choline chloride deep eutectic solvents by a triblock copolymertemplated hydrothermal synthesis.The mesoporous materials were characterized by thermal gravimetric analysis,scanning electron microscopy,and nitrogen sorption analysis.The mesoporous materials based choline chloride-ethylene glycol deep eutectic solvent,based choline chloride-glycerol,and based choline chloride-1,2-butanediol,shaped in flower-type,but the materials based choline chloride-urea and based choline chloride-acetic acid were mesoporous spheres.Application of the mesoporous materials in high-performance size exclusion chromatography column packing,the separation effect of dextrans was better from choline chloride-acetic acid deep eutectic solvent based mesoporous spheres packed in high-performance size exclusion chromatography column.The mesoporous spheres based deep eutectic solvents are a potential type of packing materials in high-performance size exclusion chromatography,and the separation conditions of more targets compounds will be explored in future works.