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In this study, corncob, an agricultural by-product rich in cellulose and hemicellulose, was subjected to acid pretreatment to remove hemicellulose and subsequently delignified using two deep eutectic solvent (DES) systems: choline chloride:urea and choline chloride:glycerol. The effect of temperature and reaction time was evaluated for both systems; ChCl:U was selected for optimization due to its superior lignin removal performance under the conditions evaluated. Temperature, time, and solid\u2013liquid ratio (SLR) were optimized using a Box\u2013Behnken design to maximize lignin removal. Under optimal conditions (113 \u00b0C, 5.7 h, 1:16.2 g\/mL), 59.086% lignin removal was achieved. Temperature and reaction time significantly influenced delignification, whereas the solid\u2013liquid ratio had a minimal effect. Structural changes in biomass throughout the process were characterized by compositional analysis, Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM), confirming effective delignification. To the best of our knowledge, there are few studies that comprehensively characterize DES-treated corncob using FTIR and SEM analysis. These findings demonstrate that choline chloride:urea has potential as a sustainable and effective pretreatment system for lignocellulosic biorefineries based on agricultural residues.<\/jats:p>","DOI":"10.3390\/molecules31183202","type":"journal-article","created":{"date-parts":[[2026,9,11]],"date-time":"2026-09-11T08:17:42Z","timestamp":1789114662000},"page":"3202","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Towards Efficient Lignin Removal: A Box\u2013Behnken Design Approach to Corncob Delignification Using Deep Eutectic Solvents"],"prefix":"10.3390","volume":"31","author":[{"ORCID":"https:\/\/orcid.org\/0009-0003-5963-9474","authenticated-orcid":false,"given":"Rebeca","family":"Astorga-Trejo","sequence":"first","affiliation":[{"name":"Laboratorio de Bioenerg\u00e9ticos, Centro Interdisciplinario de Investigaci\u00f3n para el Desarrollo Integral Regional-Unidad Sinaloa, Instituto Polit\u00e9cnico Nacional, Boulevard Juan de Dios B\u00e1tiz Paredes 250, Guasave 81101, Sinaloa, Mexico"}],"role":[{"vocabulary":"crossref","role":"author"},{"role":"methodology","vocabulary":"credit"},{"role":"data-curation","vocabulary":"credit"},{"role":"writing-original-draft","vocabulary":"credit"},{"role":"validation","vocabulary":"credit"},{"role":"formal-analysis","vocabulary":"credit"},{"role":"investigation","vocabulary":"credit"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-4605-3170","authenticated-orcid":false,"given":"Luis Ramiro","family":"Caso-Vargas","sequence":"additional","affiliation":[{"name":"Facultad de Ciencias Biol\u00f3gicas, Benem\u00e9rita Universidad Aut\u00f3noma de Puebla, Puebla 72570, Puebla, Mexico"}],"role":[{"vocabulary":"crossref","role":"author"},{"role":"methodology","vocabulary":"credit"},{"role":"writing-review-editing","vocabulary":"credit"},{"role":"data-curation","vocabulary":"credit"}]},{"given":"Efra\u00edn","family":"Rubio-Rosas","sequence":"additional","affiliation":[{"name":"Direcci\u00f3n de Innovaci\u00f3n y Transferencia del Conocimiento, Centro Universitario de Vinculaci\u00f3n y Transferencia de Tecnolog\u00eda, Benem\u00e9rita Universidad Aut\u00f3noma de Puebla, Puebla 72592, Puebla, Mexico"}],"role":[{"vocabulary":"crossref","role":"author"},{"role":"methodology","vocabulary":"credit"}]},{"given":"Leslie Susana","family":"Arcila-Lozano","sequence":"additional","affiliation":[{"name":"Centro de Investigaci\u00f3n en Biotecnolog\u00eda Aplicada (CIBA Tlaxcala), Instituto Polit\u00e9cnico Nacional, Investigadoras e Investigadores por M\u00e9xico, Secretar\u00eda de Ciencia, Humanidades, Tecnolog\u00eda e Innovaci\u00f3n, Ex-Hacienda San Juan Molino, Carretera Estatal Manzana Tepetitla Km 1.5, Santa In\u00e9s Tecuexcomac 90700, Tlaxcala, Mexico"}],"role":[{"vocabulary":"crossref","role":"author"},{"role":"writing-review-editing","vocabulary":"credit"},{"role":"methodology","vocabulary":"credit"},{"role":"data-curation","vocabulary":"credit"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-3875-7928","authenticated-orcid":false,"given":"Mar\u00eda Guadalupe","family":"Aguilar-Uscanga","sequence":"additional","affiliation":[{"name":"Laboratorio de Bioingenier\u00eda y Planta Piloto, Instituto Tecnol\u00f3gico de Veracruz, Av. 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