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This study investigates the plasma\u2010driven reaction pathways and synergistic effects in a microwave plasma\u2010catalytic system, designed for the degradation of representative odorous compounds including oxygenated volatile organic compounds (OVOCs), benzene derivatives, and sulfur compounds. An end\u2010face enhanced reactor design significantly improved plasma excitation efficiency and stability, enabling effective degradation (&gt;\u200990%) at low power (50\u201380\u2009W). Crucially, we report the first mechanistic study on the simultaneous degradation of mixed organic and inorganic sulfur compounds using microwave plasma catalysis. Real\u2010time online monitoring of reaction intermediates and products was achieved via a custom low\u2010pressure assisted microwave plasma time\u2010of\u2010flight mass spectrometry (LAMP\u2010TOFMS) instrument. Target compounds included butanal, ethyl acetate, benzene, toluene, dimethyl sulfide, dimethyl disulfide, methanethiol, and carbon disulfide. The system demonstrated not only high degradation efficiency but also a pronounced control over by\u2010product formation. The introduction of a catalyst was found to critically alter the reaction selectivity, suppressing the formation of undesirable oxygenates (e.g., formic acid) and nitrogen\u2010containing intermediates (e.g., nitromethane), thereby promoting the complete mineralization pathway. This work provides fundamental insights into the plasma\u2010catalytic reaction mechanisms governing the degradation of complex odorant mixtures, offering a novel molecular\u2010level perspective on nonthermal plasma chemistry relevant to environmental remediation.<\/jats:p>","DOI":"10.1002\/jms.70052","type":"journal-article","created":{"date-parts":[[2026,3,20]],"date-time":"2026-03-20T04:24:13Z","timestamp":1773980653000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":1,"title":["Synergistic Mechanisms Underlying Microwave Plasma\u2010Catalytic Degradation of Complex Odorous Mixtures: An In\u00a0Situ Mass Spectrometry Diagnostic Analysis"],"prefix":"10.1002","volume":"61","author":[{"given":"Jinxuan","family":"Zhang","sequence":"first","affiliation":[{"name":"School of Environmental and Chemical Engineering Shanghai University  Shanghai China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jixing","family":"Liu","sequence":"additional","affiliation":[{"name":"School of Environmental and Chemical Engineering Shanghai University  Shanghai China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Bin","family":"Jia","sequence":"additional","affiliation":[{"name":"School of Environmental and Chemical Engineering Shanghai University  Shanghai China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Gaosheng","family":"Zhao","sequence":"additional","affiliation":[{"name":"School of Environmental and Chemical Engineering Shanghai University  Shanghai China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Li","family":"Xu","sequence":"additional","affiliation":[{"name":"School of Environmental and Chemical Engineering Shanghai University  Shanghai China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-0962-8609","authenticated-orcid":false,"given":"Ping","family":"Cheng","sequence":"additional","affiliation":[{"name":"School of Environmental and Chemical Engineering Shanghai University  Shanghai China"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2026,3,19]]},"reference":[{"key":"e_1_2_9_2_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41467-022-32678-2"},{"key":"e_1_2_9_3_1","first-page":"173","article-title":"Recent Advances in the Catalytic Oxidation of Toluene on Mn\u2010Based Catalysts","volume":"71","author":"Wang X. 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