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Here, the H2O2 degradation profiles of agar (FA) and agarose (TA) were systematically compared using HRMS\/MS and 2D NMR. FA products underwent extensive hydrolytic ring-opening at 3,6-anhydro bridges, whereas TA products predominantly retained intact anhydro skeletons. In LPS-induced RAW 264.7 macrophages, intact TA oligosaccharides potently inhibited TNF-\u03b1 and IL-6 secretion, whereas ring-opened FA oligosaccharides lost anti-inflammatory activity and triggered pro-inflammatory responses. This study elucidates the specific SAR of agar polysaccharides and identifies 3,6-anhydro-l-galactose as the essential anti-inflammatory pharmacophore, offering a robust theoretical basis for the targeted green preparation of bioactive marine oligosaccharides.<\/jats:p>","DOI":"10.1021\/acs.jafc.6c08751","type":"journal-article","created":{"date-parts":[[2026,9,23]],"date-time":"2026-09-23T08:02:12Z","timestamp":1790150532000},"page":"31180-31197","source":"Crossref","is-referenced-by-count":0,"title":["Degradation Behavior\nand Mechanism of Agar Polysaccharides\nInduced by Hydrogen Peroxide: Structure Evolution and Bioactivity\nof Oligosaccharides"],"prefix":"10.1021","volume":"74","author":[{"given":"Chao","family":"Yi","sequence":"first","affiliation":[{"name":"Ocean University of China , , ,","place":["Qingdao, P. R. China, 266404"]},{"name":"Qingdao Institute of Marine Bio-Manufacturing Industry , , ,","place":["Qingdao, P. R. China, 266071"]},{"name":"China National Light Industry , , ,","place":["Qingdao, P. R. China, 266404"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0008-6818-2177","authenticated-orcid":true,"given":"Jian","family":"Shi","sequence":"additional","affiliation":[{"name":"Ocean University of China , , ,","place":["Qingdao, P. R. China, 266404"]},{"name":"Qingdao Institute of Marine Bio-Manufacturing Industry , , ,","place":["Qingdao, P. R. China, 266071"]},{"name":"China National Light Industry , , ,","place":["Qingdao, P. R. China, 266404"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Bolun","family":"Li","sequence":"additional","affiliation":[{"name":"Ocean University of China , , ,","place":["Qingdao, P. R. China, 266404"]},{"name":"Qingdao Institute of Marine Bio-Manufacturing Industry , , ,","place":["Qingdao, P. R. China, 266071"]},{"name":"China National Light Industry , , ,","place":["Qingdao, P. R. China, 266404"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chunhui","family":"Liu","sequence":"additional","affiliation":[{"name":"Ocean University of China , , ,","place":["Qingdao, P. R. China, 266404"]},{"name":"Qingdao Institute of Marine Bio-Manufacturing Industry , , ,","place":["Qingdao, P. R. China, 266071"]},{"name":"China National Light Industry , , ,","place":["Qingdao, P. R. China, 266404"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-2939-2514","authenticated-orcid":true,"given":"Hong","family":"Jiang","sequence":"additional","affiliation":[{"name":"Ocean University of China , , ,","place":["Qingdao, P. R. China, 266404"]},{"name":"Qingdao Institute of Marine Bio-Manufacturing Industry , , ,","place":["Qingdao, P. R. China, 266071"]},{"name":"China National Light Industry , , ,","place":["Qingdao, P. R. China, 266404"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-4774-6873","authenticated-orcid":true,"given":"Jianan","family":"Sun","sequence":"additional","affiliation":[{"name":"Ocean University of China , , ,","place":["Qingdao, P. R. China, 266404"]},{"name":"Qingdao Institute of Marine Bio-Manufacturing Industry , , ,","place":["Qingdao, P. R. China, 266071"]},{"name":"China National Light Industry , , ,","place":["Qingdao, P. R. China, 266404"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6315-1338","authenticated-orcid":true,"given":"Xiangzhao","family":"Mao","sequence":"additional","affiliation":[{"name":"Ocean University of China , , ,","place":["Qingdao, P. R. China, 266404"]},{"name":"Qingdao Institute of Marine Bio-Manufacturing Industry , , ,","place":["Qingdao, P. R. China, 266071"]},{"name":"China National Light Industry , , ,","place":["Qingdao, P. R. China, 266404"]},{"name":"Qingdao Marine Science and Technology Center , , ,","place":["Qingdao, P. R. China, 266237"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,9,23]]},"reference":[{"issue":"28","key":"2026100711072563400_cit1","doi-asserted-by":"publisher","first-page":"7703","DOI":"10.1080\/10408398.2021.1916736","article-title":"Recent Advances in Marine Algae Oligosaccharides: Structure,\nAnalysis, and Potential Prebiotic Activities","volume":"62","author":"Xie","year":"2022","journal-title":"Crit. Rev. Food Sci. Nutr."},{"key":"2026100711072563400_cit2","doi-asserted-by":"publisher","first-page":"104132","DOI":"10.1016\/j.algal.2025.104132","article-title":"Cosmetic Potential\nof Agar Oligosaccharides: Anti-Melanogenesis\nand Photoprotective Effects","volume":"91","author":"Wang","year":"2025","journal-title":"Algal Res."},{"issue":"2","key":"2026100711072563400_cit3","doi-asserted-by":"publisher","first-page":"310","DOI":"10.1111\/jgh.12373","article-title":"Preventive\nEffect of Agaro-Oligosaccharides\non Non-Steroidal Anti-Inflammatory Drug-Induced Small Intestinal Injury\nin Mice","volume":"29","author":"Higashimura","year":"2014","journal-title":"J. Gastroenterol. Hepatol."},{"issue":"4","key":"2026100711072563400_cit4","doi-asserted-by":"publisher","first-page":"2547","DOI":"10.1007\/s10811-019-1740-2","article-title":"The Synergistic\nAnti-Inflammatory Activities of Agaro-Oligosaccharides\nwith Different Degrees of Polymerization","volume":"31","author":"Zou","year":"2019","journal-title":"J.\nAppl. Phycol."},{"issue":"10","key":"2026100711072563400_cit5","doi-asserted-by":"publisher","first-page":"321","DOI":"10.3390\/md15100321","article-title":"Different\nLevels of Skin Whitening Activity Among 3,6-Anhydro-L-galactose, Agarooligosaccharides,\nand Neoagarooligosaccharides","volume":"15","author":"Kim","year":"2017","journal-title":"Mar. Drugs"},{"issue":"4","key":"2026100711072563400_cit6","doi-asserted-by":"publisher","first-page":"489","DOI":"10.1007\/s12257-017-0049-8","article-title":"In Vitro and In Vivo Investigation for\nBiological Activities of Neoagarooligosaccharides\nPrepared by Hydrolyzing Agar with \u03b2-Agarase","volume":"22","author":"Hong","year":"2017","journal-title":"Biotechnol. Bioprocess Eng."},{"issue":"1","key":"2026100711072563400_cit7","doi-asserted-by":"publisher","first-page":"1","DOI":"10.1016\/j.anaerobe.2011.08.003","article-title":"In Vitro Fermentation and Prebiotic Potential of Novel Low Molecular\nWeight Polysaccharides Derived from Agar and Alginate Seaweeds","volume":"18","author":"Ramnani","year":"2012","journal-title":"Anaerobe"},{"issue":"5\u20136","key":"2026100711072563400_cit8","doi-asserted-by":"publisher","first-page":"260","DOI":"10.1016\/j.anaerobe.2006.07.005","article-title":"Prebiotic Effects\nof Neoagaro-Oligosaccharides Prepared by Enzymatic\nHydrolysis of Agarose","volume":"12","author":"Hu","year":"2006","journal-title":"Anaerobe"},{"key":"2026100711072563400_cit9","doi-asserted-by":"publisher","first-page":"110408","DOI":"10.1016\/j.foodres.2021.110408","article-title":"Advances in\nAgaro-Oligosaccharides Preparation and Bioactivities for Revealing\nthe Structure-Function Relationship","volume":"145","author":"Jiang","year":"2021","journal-title":"Food Res.\nInt."},{"key":"2026100711072563400_cit10","doi-asserted-by":"publisher","first-page":"118076","DOI":"10.1016\/j.carbpol.2021.118076","article-title":"Agar Oligosaccharides:\nA Review of Preparation, Structures, Bioactivities and Application","volume":"265","author":"Chen","year":"2021","journal-title":"Carbohydr. 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Polym."},{"issue":"3","key":"2026100711072563400_cit20","doi-asserted-by":"publisher","DOI":"10.1002\/cbdv.202402204","article-title":"Degradation Polysaccharides\nfrom Benincasa hispida var. chieh-qua How: Unveiling Bioactive Properties of Degraded Compounds","volume":"22","author":"Sheng","year":"2025","journal-title":"Chem. 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Macromol."},{"key":"2026100711072563400_cit25","doi-asserted-by":"publisher","DOI":"10.1590\/2675-2824069.21-010pbt","article-title":"Determination\nof Sulfate in Algal Polysaccharide Samples:\nA Step-by-Step Protocol Using Microplate Reader","volume":"69","author":"Torres","year":"2021","journal-title":"Ocean Coast. 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Polym."},{"issue":"10","key":"2026100711072563400_cit29","doi-asserted-by":"publisher","first-page":"5439","DOI":"10.1021\/acs.jafc.3c09344","article-title":"Degradation Mechanisms of Six Typical Glucosidic Bonds\nof Disaccharides Induced by Free Radicals","volume":"72","author":"Zhu","year":"2024","journal-title":"J.\nAgric. Food Chem."},{"key":"2026100711072563400_cit30","doi-asserted-by":"publisher","first-page":"112411","DOI":"10.1016\/j.foodhyd.2025.112411","article-title":"Optimized\nUltrasonication-Redox Process\nfor Controlled Production of Low Molecular Weight Carrageenan","volume":"174","author":"Baltrusch","year":"2026","journal-title":"Food Hydrocolloids"},{"key":"2026100711072563400_cit31","doi-asserted-by":"publisher","first-page":"277","DOI":"10.1016\/j.foodchem.2018.04.098","article-title":"Thermal Degradation of Agar: Mechanism and Toxicity of Products","volume":"264","author":"Ouyang","year":"2018","journal-title":"Food Chem."},{"key":"2026100711072563400_cit32","doi-asserted-by":"publisher","first-page":"107382","DOI":"10.1016\/j.foodhyd.2021.107382","article-title":"Antioxidant\nNeoagarooligosaccharides (NAOs) and Dietary Fiber Production from\nRed Algae Gracilariopsis lemaneiformis Using Enzyme-Assisted\nOne-Step Process","volume":"125","author":"Song","year":"2022","journal-title":"Food Hydrocolloids"},{"issue":"1","key":"2026100711072563400_cit33","first-page":"110","article-title":"Degradation\nof Porphyra haitanensis Polysaccharide by Ultrasonic-Assisted\nHydrogen Peroxide Method and\nIts Antioxidant Activity Analysis","volume":"16","author":"Huang","year":"2020","journal-title":"South China\nFish. Sci."},{"issue":"4","key":"2026100711072563400_cit34","first-page":"10","article-title":"Preparation of Low Molecular Weight Eucheuma striatum Sulfated Polysaccharides by Oxidative\nDegradation with H2O2 Under the Ultrasonic Wave","volume":"24","author":"Ma","year":"2005","journal-title":"Chin. J. Mar. Drugs"},{"issue":"10","key":"2026100711072563400_cit35","doi-asserted-by":"publisher","first-page":"6883","DOI":"10.1021\/acs.biomac.4c01125","article-title":"Scaling Laws in Polysaccharide Rheology:\nComparative Analysis of Water and Ionic Liquid Systems","volume":"25","author":"Mohamed Yunus","year":"2024","journal-title":"Biomacromolecules"},{"issue":"4","key":"2026100711072563400_cit36","doi-asserted-by":"publisher","first-page":"397","DOI":"10.1007\/BF01049915","article-title":"A Systematic Nomenclature\nfor Carbohydrate Fragmentations\nin FAB-MS\/MS Spectra of Glycoconjugates","volume":"5","author":"Domon","year":"1988","journal-title":"Glycoconjugate\nJ."},{"key":"2026100711072563400_cit37","doi-asserted-by":"publisher","first-page":"176","DOI":"10.1016\/j.foodchem.2018.09.074","article-title":"Identification and Structural Analysis of Cereal Arabinoxylan-Derived\nOligosaccharides by Negative Ionization HILIC-MS\/MS","volume":"275","author":"Juvonen","year":"2019","journal-title":"Food Chem."},{"key":"2026100711072563400_cit38","doi-asserted-by":"publisher","first-page":"124765","DOI":"10.1016\/j.carbpol.2025.124765","article-title":"Oligosaccharide\nMapping Analysis Through UPLC-Orbitrap-HRMS and Enzymatic Hydrolysis\nfrom Polygonatum odoratum (Mill.) 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An Investigation Using \u03b2-Agarase I from Pseudomonas atlantica and 13C-NMR Spectroscopy","volume":"133","author":"Morrice","year":"1983","journal-title":"Eur. J. Biochem."},{"issue":"1","key":"2026100711072563400_cit42","doi-asserted-by":"publisher","first-page":"277","DOI":"10.1016\/j.carbpol.2010.07.060","article-title":"Structural Analysis\nof the Degradation Products of Porphyran Digested by Zobellia galactanivorans \u03b2-Porphyranase A","volume":"83","author":"Correc","year":"2011","journal-title":"Carbohydr. Polym."},{"issue":"3","key":"2026100711072563400_cit43","doi-asserted-by":"publisher","first-page":"179","DOI":"10.1016\/S0162-0134(00)00235-X","article-title":"ESR Study of the\nNon-Enzymic Scission\nof Xyloglucan by an Ascorbate\u2013H2O2\u2013Copper\nSystem: The Involvement of the Hydroxyl Radical and the Degradation\nof Ascorbate","volume":"84","author":"Tabbi\u0300","year":"2001","journal-title":"J. Inorg. Biochem."},{"issue":"3","key":"2026100711072563400_cit44","doi-asserted-by":"publisher","first-page":"301","DOI":"10.1016\/S0268-005X(98)00018-6","article-title":"Structural\nAnalysis of Red Seaweed Galactans of Agar and Carrageenan Groups","volume":"12","author":"Usov","year":"1998","journal-title":"Food Hydrocolloids"},{"key":"2026100711072563400_cit45","doi-asserted-by":"publisher","first-page":"1370","DOI":"10.1016\/j.carbpol.2015.10.007","article-title":"Carrageenan and Agaran\nStructures from the Red Seaweed Gymnogongrus tenuis","volume":"136","author":"Perez Recalde","year":"2016","journal-title":"Carbohydr. Polym."},{"issue":"12","key":"2026100711072563400_cit46","doi-asserted-by":"publisher","DOI":"10.1111\/jfpp.16074","article-title":"Degradation\nby Vc-H2O2, Characterization\nand Antioxidant Activity of Polysaccharides from Passiflora edulis Peel","volume":"45","author":"Li","year":"2021","journal-title":"J. Food Process. 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