Continuously　promoting　new　curriculum　standards　is　a　key　aim　of　the　Ministry　of　Education　of　China.　With　this　in　mind,　this　paper　introduces　a　comprehensive　teaching　experiment　for　undergraduate　instrumental　analysis　courses　that　aims　to　improve　students＇　material-preparation　and　instrumental-analysis　skills　through　practice.　Herein,　a　covalent　organic　framework-based　core-shell　stationary　phase　material　(SiO2@COFTTA-DHTA)　is　prepared　via　a　one-pot　method　and　characterized　in　detail,　after　which　its　chromatographic　properties　are　evaluated　by　high　performance　liquid　chromatography　(HPLC).　The　experimental　process　includes　material　synthesis　and　characterization,　as　well　as　studying　the　chromatographic-retention　behavior　and　chromatographic-separation　performance　of　the　material.　By　the　combining　theoretical　science　and　experimental　teaching,　this　experiment　not　only　deepens　students＇　understanding　of　the　properties　of　functional　materials　and　their　applications,　but　also　improves　their　experimental-design　and　critical-thinking　skills.　This　experiment　not　only　cultivates　students＇　interests　in　scientific　research,　but　also　exercises　their　experimental,　operational,　innovative-thinking,　and　practical　abilities,　while　concurrently　enhancing　their　sense　of　social　responsibility　and　historical　mission,　thereby　delivering　the　all-round　educational　goals　of　experimental　teaching.