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Nevertheless, constructing membrane pores with subnanometer precision and resolving structurally similar molecular mixtures remain major challenges. Herein, we report an isoreticular contraction strategy to construct a series of kgd\u2010topology COF membranes with progressively narrowed apertures in situ on polyacrylonitrile (PAN) substrates through contra\u2010diffusion interfacial polymerization between hexa(4\u2010formylphenyl)benzene (HFPB) and three triamine monomers of decreasing size. Systematic framework contraction decreased the aperture from 12.1 to 10.2 \u00c5 and then to 6.5 \u00c5, giving molecular weight cut\u2010offs of 500, 380, and 290\u00a0Da, respectively. Notably, membranes with different contraction degrees were further integrated into a cascade separation system with well\u2010separated molecular\u2010weight rejection thresholds, enabling the purification of a four\u2010component mixture of camptothecin\u2010related compounds with equal mass concentrations, achieving a maximum fraction purity of 96.6%. This work establishes isoreticular contraction as an effective strategy for programming transport\u2010relevant pores in COF membranes and highlights the potential of kgd\u2010topology COF membranes for cascade pharmaceutical purification.<\/jats:p>","DOI":"10.1002\/smll.76356","type":"journal-article","created":{"date-parts":[[2026,10,18]],"date-time":"2026-10-18T19:38:30Z","timestamp":1792352310000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Isoreticular Contraction of kgd\u2010Topology Covalent Organic Framework Membranes for Precise Pharmaceutical Separation"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-3955-8437","authenticated-orcid":false,"given":"Baodong","family":"Tian","sequence":"first","affiliation":[{"name":"MOE Key Laboratory of Macromolecular Synthesis and Functionalization Department of Polymer Science and Engineering Zhejiang University Hangzhou P. R. 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China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-2542-3176","authenticated-orcid":false,"given":"Chuanjie","family":"Fang","sequence":"additional","affiliation":[{"name":"Center for Healthcare Materials Shaoxing Institute Zhejiang University Shaoxing P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Li","family":"Xu","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Chemical Engineering and Low\u2010carbon Technology College of Chemical and Biological Engineering Zhejiang University  Hangzhou 310058 P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-1553-4190","authenticated-orcid":false,"given":"Liping","family":"Zhu","sequence":"additional","affiliation":[{"name":"MOE Key Laboratory of Macromolecular Synthesis and Functionalization Department of Polymer Science and Engineering Zhejiang University Hangzhou P. R. 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