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A\u03b2 peptides are present at trace levels in cerebrospinal fluid, therefore, developing a\u00a0new selective extraction procedure is essential for isolating targeted biomarkers from the matrix interferents, ensuring accurate identification and quantification. In this study, a hybrid organic-silica monolith was synthesized in a 530\u00a0\u00b5m inner diameter-capillary and used for the covalent grafting of beta amyloid peptide aptamers. The resulting miniaturized oligosorbent (mOS) was applied to selectively extract A\u03b2 peptides 40 and 42 from artificial\u00a0cerebrospinal fluid (CSF) samples. The immobilization procedure achieved grafting yields higher than 90% leading to a dense coverage of A\u03b2 aptamers (655\u2009+\u200915\u00a0pmol.\u00b5L<jats:sup>\u22121<\/jats:sup> of oligosorbent, n\u2009=\u20093, RSD\u2009=\u20092.3), and in a capacity exceeding 50\u00a0pmol.\u00b5L<jats:sup>\u22121<\/jats:sup> of mOS. After optimization in pure media, an extraction recovery of 74% and 31% for A\u03b240 and A\u03b242 peptides, respectively was reached on this mOS. The developed method including extraction on mOS and LC\u2013MS analysis achieved LLOQ values of 0.1\u00a0ng.mL<jats:sup>\u22121<\/jats:sup>, precision and accuracy with CV and RSD values ranging from 1.0% to 12.9% and\u2009\u22124.7% to 11.1%, respectively. This method was successfully applied to selectively extract A\u03b2 peptides from artificial CSF samples, effectively isolating the two A\u03b2 targeted peptides from this complex biological fluid and enhancing trace-level analysis reliability.<\/jats:p>\n          <jats:p>\n            <jats:bold>Graphical Abstract<\/jats:bold>\n          <\/jats:p>","DOI":"10.1007\/s00216-025-06085-7","type":"journal-article","created":{"date-parts":[[2025,9,1]],"date-time":"2025-09-01T01:54:00Z","timestamp":1756691640000},"page":"5907-5918","update-policy":"https:\/\/doi.org\/10.1007\/springer_crossmark_policy","source":"Crossref","is-referenced-by-count":2,"title":["Synthesis and characterization of miniaturized aptamer-based monolithic sorbent for selective extraction of \u03b2-amyloid peptides from cerebrospinal fluid"],"prefix":"10.1007","volume":"417","author":[{"given":"Israel Donizeti","family":"de Souza","sequence":"first","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Caroline","family":"Fernandes Grecco","sequence":"additional","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Maria Eug\u00eania","family":"Costa Queiroz","sequence":"additional","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Valerie","family":"Pichon","sequence":"additional","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3318-7230","authenticated-orcid":false,"given":"Audrey","family":"Comb\u00e8s","sequence":"additional","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"297","published-online":{"date-parts":[[2025,9,1]]},"reference":[{"key":"6085_CR1","unstructured":"Evans-Lacko S, Aguzzoli E, Read S, Comas-Herrera A, Farina N. 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All other authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.","order":2,"name":"Ethics","group":{"name":"EthicsHeading","label":"Competing interest"}}]}}