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Herein, we report a broadly applicable strategy driven by clinical ultrasound for the reductive deoxygenation of N-oxides, enabling externally controlled prodrug activation via a riboflavin tetrabutyrate (TBR)\/NADPH redox-relay system. Under mild, clinically translatable ultrasound (1 MHz, 2.0 W\/cm2, 50% duty cycle), this platform promotes efficient N\u2013O bond cleavage through single-electron transfer and hydrogen-atom transfer. Density functional theory calculations support that all ground-state steps are thermodynamically favorable with negative Gibbs free-energy changes (\u0394G), supporting the feasibility of sonochemical N-oxide reduction. This method exhibits broad substrate generality toward diverse N-oxide compounds, including the clinically investigated hypoxia-activated prodrug banoxantrone (AQ4N), quinoline N-oxide, 8-hydroxyquinoline N-oxide, clozapine N-oxide, and olanzapine N-oxide. In hypoxic tumor cells, the ultrasound\/TBR system enhances intracellular AQ4 formation significantly and reduces the IC50 of AQ4N from 35.0 to 2.8 mg\/L. In vivo, the combination of AQ4N, TBR, and ultrasound increased intratumoral AQ4 formation by approximately 24.1-fold and achieved a tumor inhibition rate of 113.7%, outperforming AQ4N monotherapy (82.3%). This sonochemically triggered activation platform bypasses the heterogeneity of tumor-microenvironment stimuli and offers a versatile, externally controlled framework for precision prodrug chemotherapy with deep tissue penetration and clinical translatability.<\/jats:p>","DOI":"10.1021\/jacs.6c07122","type":"journal-article","created":{"date-parts":[[2026,8,6]],"date-time":"2026-08-06T16:02:03Z","timestamp":1786032123000},"page":"34231-34243","source":"Crossref","is-referenced-by-count":0,"title":["Ultrasound-Driven Reductive\nDeoxygenation of\n                    <i>N<\/i>\n                    -Oxides for Spatiotemporally\nControlled Prodrug\nActivation"],"prefix":"10.1021","volume":"148","author":[{"given":"Jingxuan","family":"Zhang","sequence":"first","affiliation":[{"name":"Jilin University , , , ,","place":["Changchun, Jilin, China, 130021"]},{"name":"Chinese Academy of Sciences , , , ,","place":["Changchun, Jilin, China, 130022"]},{"name":"Jilin Biomedical Polymers Engineering Laboratory , , ,","place":["Changchun, Jilin, China, 130022"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hongyu","family":"Chu","sequence":"additional","affiliation":[{"name":"China-Japan Union Hospital of Jilin University , , , ,","place":["Changchun, Jilin, China, 130033"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Weidong","family":"Zhao","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , , ,","place":["Changchun, Jilin, China, 130022"]},{"name":"Jilin Biomedical Polymers Engineering Laboratory , , ,","place":["Changchun, Jilin, China, 130022"]},{"name":"University of Science and Technology of China , , , ,","place":["Hefei, Anhui, China, 230026"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chaoying","family":"Kong","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , , ,","place":["Changchun, Jilin, China, 130022"]},{"name":"Jilin Biomedical Polymers Engineering Laboratory , , ,","place":["Changchun, Jilin, China, 130022"]},{"name":"University of Science and Technology of China , , , ,","place":["Hefei, Anhui, China, 230026"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hang","family":"Xu","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , , ,","place":["Changchun, Jilin, China, 130022"]},{"name":"Jilin Biomedical Polymers Engineering Laboratory , , ,","place":["Changchun, Jilin, China, 130022"]},{"name":"University of Science and Technology of China , , , ,","place":["Hefei, Anhui, China, 230026"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Haiyang","family":"Yu","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , , ,","place":["Changchun, Jilin, China, 130022"]},{"name":"Jilin Biomedical Polymers Engineering Laboratory , , ,","place":["Changchun, Jilin, China, 130022"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ming","family":"Yang","sequence":"additional","affiliation":[{"name":"Jilin University , , , ,","place":["Changchun, Jilin, China, 130021"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1557-1060","authenticated-orcid":true,"given":"Na","family":"Shen","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , , ,","place":["Changchun, Jilin, China, 130022"]},{"name":"Jilin Biomedical Polymers Engineering Laboratory , , ,","place":["Changchun, Jilin, China, 130022"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-9326-3755","authenticated-orcid":true,"given":"Guoqing","family":"Wang","sequence":"additional","affiliation":[{"name":"Jilin University , , , ,","place":["Changchun, Jilin, China, 130021"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-4726-4305","authenticated-orcid":true,"given":"Zhaohui","family":"Tang","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , , ,","place":["Changchun, Jilin, China, 130022"]},{"name":"Jilin Biomedical Polymers Engineering Laboratory , , ,","place":["Changchun, Jilin, China, 130022"]},{"name":"University of Science and Technology of China , , , ,","place":["Hefei, Anhui, China, 230026"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,8,6]]},"reference":[{"issue":"38","key":"2026081910233938200_cit1","doi-asserted-by":"publisher","first-page":"34425","DOI":"10.1021\/jacs.5c08152","article-title":"Development of Cyclooctyne-Nitrone Based Click Release Chemistry\nfor Bioorthogonal Prodrug Activation both In Vitro and In Vivo","volume":"147","author":"Xu","year":"2025","journal-title":"J. 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