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This issue is attributed to the absence of a separation unit prior to the sensor. Here, we report a new sensing medium, named porous fluorescent monolith, which can separate mixture and meanwhile be integrated into a sensor for discriminative detection. The fluorescent monoliths are prepared via polymerization of 4,4\u2032,4\u2033,4<jats:sup>\u2034<\/jats:sup>\u2010(ethene\u20101,1,2,2\u2010tetrayl)tetrabenzaldehyde with diamines. Their photophysical property and hierarchical porosity are systematically studied. On this basis, we set up a separation\u2010sensing platform and realize quantitative analysis for trace water in methanol, a sarin simulant, perfluoroalkyl compounds, and metal ions. The separation\u2010sensing platform furthermore demonstrates baseline separation for benzene, toluene, ethylbenzene, and xylene, with limit of detections of 86, 54, 19, and 58\u00a0ng, respectively. To our knowledge, this is the first time that a fluorescent monolith is used to realize a separation\u2010sensing tandem. We anticipate our findings will provide a promising strategy for producing portable devices with the on\u2010site discriminative sensing ability for real samples.<\/jats:p>","DOI":"10.1002\/anie.202502020","type":"journal-article","created":{"date-parts":[[2025,3,14]],"date-time":"2025-03-14T23:19:26Z","timestamp":1741994366000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":9,"title":["Miniaturized Separation\u2010Sensing Tandem Enabled by Fluorescent Monoliths"],"prefix":"10.1002","volume":"64","author":[{"given":"Jie","family":"Wang","sequence":"first","affiliation":[{"name":"Institute of New Concept Sensors and Molecular Materials Key Laboratory of Applied Surface and Colloid Chemistry (Ministry of Education) School of Chemistry and Chemical Engineering, Shaanxi Normal University  Xi'an 710119 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ruijuan","family":"Wen","sequence":"additional","affiliation":[{"name":"Institute of New Concept Sensors and Molecular Materials Key Laboratory of Applied Surface and Colloid Chemistry (Ministry of Education) School of Chemistry and Chemical Engineering, Shaanxi Normal University  Xi'an 710119 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jinglin","family":"Kong","sequence":"additional","affiliation":[{"name":"State Key Laboratory of NBC Protection for Civilian  Beijing 100049 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jing","family":"Liu","sequence":"additional","affiliation":[{"name":"Institute of New Concept Sensors and Molecular Materials Key Laboratory of Applied Surface and Colloid Chemistry (Ministry of Education) School of Chemistry and Chemical Engineering, Shaanxi Normal University  Xi'an 710119 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