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In this study, we present a novel strategy for the in situ generation of imaging and radiosensitizing nanoprobes inside tumors, enabling responsive photoacoustic imaging and targeted radiotherapy. The designed organic\u2013inorganic hybrid nanoprobe is composed of a copper\u2010based layered double hydroxide (Cu\u2010LDH) intercalated with the near\u2010infrared organic dye IR\u2010806, serving as a photoacoustic imaging agent (designated as CAL\u2010IR). Upon exposure to hydrogen sulfide (H\n                    <jats:sub>2<\/jats:sub>\n                    S) in colorectal tumor microenvironments, the nanoprobe undergoes activation and transforms in situ into copper sulfide (Cu\n                    <jats:sub>2<\/jats:sub>\n                    <jats:sub>\u2212<\/jats:sub>\n                    <jats:sub>x<\/jats:sub>\n                    S) nanoparticles. The newly formed Cu\n                    <jats:sub>2<\/jats:sub>\n                    <jats:sub>\u2212<\/jats:sub>\n                    <jats:sub>x<\/jats:sub>\n                    S\/LDH heterojunction nanostructure exhibits significantly enhanced near\u2010infrared absorption, while concurrently promoting radiotherapy efficacy through multiple mechanisms: consumption of endogenous H\n                    <jats:sub>2<\/jats:sub>\n                    S, reduction of X\u2010ray attenuation, and intrinsic radiosensitization. This unique system allows high\u2010contrast photoacoustic imaging and, consequently, achieves improved radiotherapy outcomes in mouse models of colorectal cancer, with minimal off\u2010target effects. These results underscore the promising clinical potential of CAL\u2010IR for precision tumor imaging and enhanced radiotherapy.\n                  <\/jats:p>","DOI":"10.1002\/advs.202522370","type":"journal-article","created":{"date-parts":[[2026,1,25]],"date-time":"2026-01-25T08:42:51Z","timestamp":1769330571000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":3,"title":["In Situ Synthesis of a Tumor Microenvironment\u2010Activated Radiosensitizing Cu\n                    <sub>2\u2010x<\/sub>\n                    S\/LDH Probe for Photoacoustic Imaging\u2010Guided Radiotherapy"],"prefix":"10.1002","volume":"13","author":[{"given":"Kang","family":"Zhu","sequence":"first","affiliation":[{"name":"State Key Laboratory of Chemical Resource Engineering College of Chemistry Beijing University of Chemical Technology  Beijing P. R. 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