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Layered double hydroxide (LDH) transition metal containing are widely assumed to be biologically inert despite their tunable metal composition, high surface reactivity, and potential to interact directly with biological systems. Here, we evaluated the acute and sublethal toxicity of LDH nanoparticles containing transition metals (Al\u2013Ni, Al\u2013Co, or Al\u2013Cu) on Spodoptera frugiperda larvae. Laboratory bioassays were performed by incorporating nanoparticles into the larval artificial diet to quantify dose\u2013mortality relationships, estimate LC50 values, and assess impacts on larval and pupal development. All LDH formulations exhibited dose-dependent toxicity, with Al\u2013Cu LDH showing the highest potency and the lowest LC50 (19.1\u201337.3 mg mL\u20131). Furthermore, a significant reduction in pupation rate and larval weight was observed, suggesting relevant sublethal effects. These findings provide evidence that metallic LDHs possess bioactivity against an agriculturally important pest, challenging the assumption of LDH inertness and revealing their potential as dual-function materials that combine inherent biological effects with delivery capabilities. This work establishes a new foundation for evaluating LDHs within pest-management frameworks and underscores the need to assess selectivity, environmental fate, and impacts on nontarget organisms before field deployment.<\/jats:p>","DOI":"10.1021\/acsomega.6c06039","type":"journal-article","created":{"date-parts":[[2026,9,23]],"date-time":"2026-09-23T08:02:00Z","timestamp":1790150520000},"page":"59593-59600","source":"Crossref","is-referenced-by-count":0,"title":["Novel Insights\ninto the Acute and Sublethal Toxicity\nof Layered Double Hydroxide Nanoparticles in\n                    <i>Spodoptera frugiperda<\/i>\n                    Larvae"],"prefix":"10.1021","volume":"11","author":[{"given":"Andre\u0301","family":"Lopes Ferreira","sequence":"first","affiliation":[{"name":"Universidade Estadual de Campinas - UNICAMP , , , ,","place":["Campinas, Sa\u0303o Paulo, Brazil, 13083-872"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Kelly Cristina","family":"Gonc\u0327alves","sequence":"additional","affiliation":[{"name":"Universidade Estadual Paulista Julio de Mesquita Filho - UNESP , , , ,","place":["Sa\u0303o Paulo, Sa\u0303o Paulo, Brazil, 14884-900"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Sofia Cristina","family":"Picotte","sequence":"additional","affiliation":[{"name":"Universidade Estadual Paulista Julio de Mesquita Filho - UNESP , , , ,","place":["Sa\u0303o Paulo, Sa\u0303o Paulo, Brazil, 14884-900"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Raqueli","family":"Viana","sequence":"additional","affiliation":[{"name":"Universidade Estadual Paulista Julio de Mesquita Filho - UNESP , , , ,","place":["Sa\u0303o Paulo, Sa\u0303o Paulo, Brazil, 14884-900"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0769-9902","authenticated-orcid":true,"given":"Ricardo Antonio","family":"Polanczyk","sequence":"additional","affiliation":[{"name":"Universidade Estadual Paulista Julio de Mesquita Filho - UNESP , , , ,","place":["Sa\u0303o Paulo, Sa\u0303o Paulo, Brazil, 14884-900"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0812-1491","authenticated-orcid":true,"given":"Marcelo Bispo","family":"de Jesus","sequence":"additional","affiliation":[{"name":"Universidade Estadual de Campinas - UNICAMP , , , ,","place":["Campinas, Sa\u0303o Paulo, Brazil, 13083-872"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,9,23]]},"reference":[{"issue":"5","key":"2026100610464562500_cit1","doi-asserted-by":"publisher","first-page":"1131","DOI":"10.3390\/agronomy15051131","article-title":"Nanoparticles for Sustainable Agriculture: Assessment\nof Benefits and Risks","volume":"15","author":"Bouhadi","year":"2025","journal-title":"Agronomy"},{"key":"2026100610464562500_cit2","doi-asserted-by":"publisher","first-page":"45","DOI":"10.1007\/978-981-10-6056-4_2","article-title":"Insect Pests and Crop Losses","volume-title":"Breeding\nInsect Resistant Crops for Sustainable Agriculture","author":"Sharma","year":"2017"},{"issue":"2","key":"2026100610464562500_cit3","doi-asserted-by":"publisher","first-page":"342","DOI":"10.3390\/agriculture13020342","article-title":"Control of Spodoptera Frugiperda\non Fresh Corn via Pesticide Application before Transplanting","volume":"13","author":"Han","year":"2023","journal-title":"Agriculture"},{"key":"2026100610464562500_cit4","doi-asserted-by":"publisher","first-page":"106743","DOI":"10.1016\/j.cropro.2024.106743","article-title":"Level of Damage and Yield Losses Associated with the Fall Armyworm\n(Spodoptera Frugiperda) on Maize (Zea Mays), Millet (Pennisetum Glaucum) and Sorghum (Sorghum Bicolor) on Station in Burkina Faso","volume":"182","author":"Yame\u0301ogo","year":"2024","journal-title":"Crop Prot."},{"issue":"1","key":"2026100610464562500_cit5","doi-asserted-by":"publisher","first-page":"133","DOI":"10.1007\/s44279-025-00316-2","article-title":"The Impact of Fall Armyworm on Subsistence Farmers\nin the Limpopo Province of South Africa","volume":"3","author":"Raphela","year":"2025","journal-title":"Discover\nAgric."},{"key":"2026100610464562500_cit6","doi-asserted-by":"publisher","first-page":"3","DOI":"10.3389\/fchem.2015.00064","article-title":"Nanopesticides\nand Nanofertilizers: Emerging Contaminants or Opportunities for Risk\nMitigation?","volume":"3","author":"Kah","year":"2015","journal-title":"Front. Chem."},{"key":"2026100610464562500_cit7","doi-asserted-by":"publisher","first-page":"305","DOI":"10.1016\/B978-0-323-95721-2.00012-9","article-title":"Chapter Fourteen -Application of Nanoparticles\nin Agriculture: Nano-Based Fertilizers, Pesticides, Herbicides, and\nNanobiosensors","volume-title":"Molecular Impacts of Nanoparticles\non Plants and Algae","author":"Pathak","year":"2024"},{"key":"2026100610464562500_cit8","doi-asserted-by":"publisher","first-page":"122","DOI":"10.1016\/j.pestbp.2014.11.014","article-title":"IRAC: Mode of Action Classification\nand Insecticide Resistance Management","volume":"121","author":"Sparks","year":"2015","journal-title":"Pestic.\nBiochem. Physiol."},{"issue":"5","key":"2026100610464562500_cit9","doi-asserted-by":"publisher","first-page":"528","DOI":"10.3390\/insects16050528","article-title":"Insect Pest\nControl from Chemical to Biotechnological Approach: Constrains and\nChallenges","volume":"16","author":"Civolani","year":"2025","journal-title":"Insects"},{"issue":"40","key":"2026100610464562500_cit10","doi-asserted-by":"publisher","first-page":"41130","DOI":"10.1021\/acsomega.4c06628","article-title":"Integrated Pest\nManagement: An Update on the Sustainability\nApproach to Crop Protection","volume":"9","author":"Zhou","year":"2024","journal-title":"ACS Omega"},{"issue":"18","key":"2026100610464562500_cit11","doi-asserted-by":"publisher","first-page":"2939","DOI":"10.3390\/plants14182939","article-title":"Advancements in Agricultural Nanotechnology: An Updated\nReview","volume":"14","author":"Pagano","year":"2025","journal-title":"Plants"},{"issue":"10","key":"2026100610464562500_cit12","doi-asserted-by":"publisher","first-page":"686","DOI":"10.1016\/j.scib.2017.04.004","article-title":"Delaminated Layered\nDouble Hydroxide Delivers DNA Molecules as Sandwich Nanostructure\ninto Cells via a Non-Endocytic Pathway","volume":"62","author":"Li","year":"2017","journal-title":"Sci.\nBull."},{"issue":"10","key":"2026100610464562500_cit13","doi-asserted-by":"publisher","first-page":"2544","DOI":"10.1021\/acs.bioconjchem.9b00434","article-title":"Layered Double\nHydroxide\nNanoparticles for Efficient Gene Delivery for Cancer Treatment","volume":"30","author":"Senapati","year":"2019","journal-title":"Bioconjugate Chem."},{"key":"2026100610464562500_cit14","article-title":"Layered\nDouble Hydroxide Nanoparticles Induce Composition-Dependent Cytotoxic\nand Phenotypic Effects in Mammalian Cells","author":"Ferreira","year":"2026","journal-title":"bioRxiv"},{"issue":"4","key":"2026100610464562500_cit15","doi-asserted-by":"publisher","first-page":"487","DOI":"10.1093\/jee\/69.4.487","article-title":"Velvetbean Caterpillar: A Rearing\nProcedure and Artificial Medium123","volume":"69","author":"Greene","year":"1976","journal-title":"J. Econ.\nEntomol."},{"key":"2026100610464562500_cit16","doi-asserted-by":"publisher","first-page":"105460","DOI":"10.1016\/j.biocontrol.2024.105460","article-title":"Global\nScientific Progress and Shortfalls in Biological Control of the Fall\nArmyworm Spodoptera Frugiperda","volume":"191","author":"Wyckhuys","year":"2024","journal-title":"Biol. Control"},{"issue":"23","key":"2026100610464562500_cit17","doi-asserted-by":"publisher","first-page":"3227","DOI":"10.1007\/s11434-007-0480-x","article-title":"Metallothionein Expression Induced by Nickel Accumulation in the\nMidgut of Spodoptera Litura Fabricius Larvae Exposed to Nickel","volume":"52","author":"Sun","year":"2007","journal-title":"Chin. Sci. Bull."},{"key":"2026100610464562500_cit18","doi-asserted-by":"publisher","first-page":"106314","DOI":"10.1016\/j.pestbp.2025.106314","article-title":"Toxicological\nInvestigations of Biosynthesized\nNickel Ferrites Nanoparticles on Midgut Epithelium of Blaps Polychresta as Nanopesticides: Structural Damages and Oxidative\nStress","volume":"208","author":"Arafat","year":"2025","journal-title":"Pestic. Biochem. Physiol."},{"issue":"4","key":"2026100610464562500_cit19","doi-asserted-by":"publisher","first-page":"812","DOI":"10.1002\/etc.4663","article-title":"Bioaccumulation\nand Toxicity of Cadmium, Copper, Nickel, and Zinc and Their Mixtures\nto Aquatic Insect Communities","volume":"39","author":"Mebane","year":"2020","journal-title":"Environ. Toxicol.\nChem."},{"issue":"10","key":"2026100610464562500_cit20","doi-asserted-by":"publisher","first-page":"1861","DOI":"10.1002\/etc.4812","article-title":"Toxicity of Nanoparticulate Nickel to Aquatic Organisms:\nReview and Recommendations for Improvement of Toxicity Tests","volume":"39","author":"Meyer","year":"2020","journal-title":"Environ. Toxicol. Chem."},{"issue":"2","key":"2026100610464562500_cit21","doi-asserted-by":"publisher","first-page":"610","DOI":"10.1039\/C9EN00690G","article-title":"In Vivo Evaluation\nof the Toxic and\nGenotoxic Effects of Exposure to Cobalt Nanoparticles Using Drosophila\nMelanogaster","volume":"7","author":"Alaraby","year":"2020","journal-title":"Environ. Sci.: Nano"},{"key":"2026100610464562500_cit22","doi-asserted-by":"publisher","first-page":"111","DOI":"10.1007\/978-94-017-8739-0_7","article-title":"Intracellular Signal Modulation by Nanomaterials","volume":"811","author":"Hussain","year":"2014","journal-title":"Adv. Exp. Med. Biol."},{"issue":"5","key":"2026100610464562500_cit23","doi-asserted-by":"publisher","DOI":"10.1016\/j.heliyon.2023.e16133","article-title":"Insecticidal\nEfficacy of Nanoparticles against Spodoptera Frugiperda (J.E. Smith)\nLarvae and Their Impact in the Soil","volume":"9","author":"Pittarate","year":"2023","journal-title":"Heliyon"},{"issue":"11","key":"2026100610464562500_cit24","doi-asserted-by":"publisher","first-page":"1030","DOI":"10.3390\/insects13111030","article-title":"Larvicidal and Antifeedant Effects\nof Copper Nano-Pesticides against Spodoptera Frugiperda (J.E. Smith)\nand Its Immunological Response","volume":"13","author":"Rahman","year":"2022","journal-title":"Insects"},{"issue":"3","key":"2026100610464562500_cit25","doi-asserted-by":"publisher","first-page":"1163","DOI":"10.3390\/nano5031163","article-title":"Nanotoxicity: An Interplay of Oxidative\nStress, Inflammation and Cell Death","volume":"5","author":"Khanna","year":"2015","journal-title":"Nanomaterials"},{"issue":"1","key":"2026100610464562500_cit26","doi-asserted-by":"publisher","first-page":"2220","DOI":"10.1038\/s41598-025-85691-y","article-title":"Cobalt Oxide\nNanoparticles Induce Cytotoxicity and Excessive ROS Mediated Mitochondrial\nDysfunction and P53-Independent Apoptosis in Melanoma Cells","volume":"15","author":"Mohamed","year":"2025","journal-title":"Sci. Rep."},{"issue":"10","key":"2026100610464562500_cit27","doi-asserted-by":"publisher","first-page":"5262","DOI":"10.1007\/s12011-025-04562-9","article-title":"Toxicological\nAlterations Induced by Subacute Exposure of Cobalt Oxide Nanoparticles\nin Aged Rats: Behavioral, Biochemical, Molecular, and Histopathological\nEvidence","volume":"203","author":"Boukholda","year":"2025","journal-title":"Biol. Trace Elem. Res."},{"key":"2026100610464562500_cit28","doi-asserted-by":"publisher","first-page":"115165","DOI":"10.1016\/j.watres.2019.115165","article-title":"Exposure to Heavy Metal-Contaminated Sediments Disrupts\nGene Expression, Lipid Profile, and Life History Traits in the Midge\nChironomus Riparius","volume":"168","author":"Arambourou","year":"2020","journal-title":"Water Res."},{"issue":"14","key":"2026100610464562500_cit29","doi-asserted-by":"publisher","first-page":"14426","DOI":"10.1007\/s11356-019-04792-0","article-title":"Heavy Metal Exposure\nthrough Artificial Diet Reduces Growth and Survival of Spodoptera\nLitura (Lepidoptera: Noctuidae)","volume":"26","author":"Ali","year":"2019","journal-title":"Environ. Sci.\nPollut. Res. Int."},{"issue":"2","key":"2026100610464562500_cit30","doi-asserted-by":"publisher","first-page":"144","DOI":"10.1007\/s00244-024-01076-8","article-title":"Impact\nof Exposure to Leaves From\nMetal-Polluted Sites on the Developmental Parameters of Larvae of\nthe Dark Sword-Grass, Agrotis Ipsilon (Lepidoptera: Noctuidae)","volume":"87","author":"Rasmy","year":"2024","journal-title":"Arch. Environ. Contam. Toxicol."},{"key":"2026100610464562500_cit31","doi-asserted-by":"publisher","first-page":"189","DOI":"10.1094\/MPMI-19-0189","article-title":"Ethylene\nSignaling Mediates a Maize Defense Response to Insect Herbivory","volume":"19","author":"Harfouche","year":"2006","journal-title":"MPMI"},{"issue":"21","key":"2026100610464562500_cit32","doi-asserted-by":"publisher","first-page":"12112","DOI":"10.1021\/es3022182","article-title":"Upon Exposure to Cu\nNanoparticles, Accumulation of Copper in the\nIsopod Porcellio Scaber Is Due to the Dissolved Cu Ions Inside the\nDigestive Tract","volume":"46","author":"Golobic\u030c","year":"2012","journal-title":"Environ. Sci. Technol."}],"container-title":["ACS Omega"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/pubs.acs.org\/doi\/pdf\/10.1021\/acsomega.6c06039","content-type":"application\/pdf","content-version":"vor","intended-application":"unspecified"},{"URL":"https:\/\/pubs.acs.org\/acsodf\/article-pdf\/11\/39\/59593\/68612699\/acsomega.6c06039.pdf","content-type":"application\/pdf","content-version":"vor","intended-application":"syndication"},{"URL":"https:\/\/pubs.acs.org\/acsodf\/article-pdf\/11\/39\/59593\/68612699\/acsomega.6c06039.pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2026,10,6]],"date-time":"2026-10-06T15:30:50Z","timestamp":1791300650000},"score":1,"resource":{"primary":{"URL":"https:\/\/pubs.acs.org\/acsodf\/article\/11\/39\/59593\/5436114\/Novel-Insights-into-the-Acute-and-Sublethal"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2026,9,23]]},"references-count":32,"journal-issue":{"issue":"39","published-online":{"date-parts":[[2026,9,23]]},"published-print":{"date-parts":[[2026,10,6]]}},"URL":"https:\/\/doi.org\/10.1021\/acsomega.6c06039","relation":{},"ISSN":["2470-1343"],"issn-type":[{"value":"2470-1343","type":"electronic"}],"subject":[],"published":{"date-parts":[[2026,9,23]]}}}