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Laser exposure on electrospun polyimide nanofibers, embedded with Pt and Ni precursors, facilitated not only the formation of LCNFs but also the generation of Pt\/Ni nanoparticles with a radius of approximately 2\u00a0nm and a distinctive crystalline structure. X-ray photoelectron spectroscopy revealed the oxidation states of the laser-generated Pt\/Ni and confirmed the formation of the Pt\/Ni alloy nanocatalysts. Additionally, small-angle X-ray scattering has shown that the graphitic structures of the LCNFs strongly depend on the metal salt concentrations and molar ratio. Pt\/Ni-LCNFs were exploited as enzyme-free electrodes for glucose sensing at physiological pH. The presence of Pt in the alloy enabled a low potential (\u22120.9 V for 20 s) in situ generation of highly localized OH<jats:sup>\u2212<\/jats:sup> which facilitated glucose electrooxidation by Ni. Under optimized conditions, Pt\/Ni-LCNFs achieved reliable glucose detection in physiological conditions (pH 7.4), with detection limit of 0.3 mM, linearity from 0.1 to 4\u00a0mM, and minimal interference from other electroactive species. Self-calibrated data acquisition strategy provided an excellent recovery rate (95 \u00b1\u200910%) in diluted human serum. Furthermore, unlike enzyme-based sensors, the catalytic activity of Pt\/Ni LCNFs was maintained after sterilization, highlighting their robustness and potential in biomedical applications and bioprocess monitoring.<\/jats:p>\n          <jats:p>\n            <jats:bold>Graphical Abstract<\/jats:bold>\n          <\/jats:p>","DOI":"10.1007\/s00216-025-05869-1","type":"journal-article","created":{"date-parts":[[2025,4,11]],"date-time":"2025-04-11T01:21:06Z","timestamp":1744334466000},"page":"3337-3351","update-policy":"https:\/\/doi.org\/10.1007\/springer_crossmark_policy","source":"Crossref","is-referenced-by-count":3,"title":["Laser-generated Pt\/Ni nanocatalysts-carbon nanofibers enabling self-calibrated enzyme-free glucose detection at physiological pH"],"prefix":"10.1007","volume":"417","author":[{"given":"Christoph","family":"Bruckschlegel","sequence":"first","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Vivien","family":"Fleischmann","sequence":"additional","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Aladin","family":"Ullrich","sequence":"additional","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Luc","family":"Girard","sequence":"additional","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Pierre","family":"Bauduin","sequence":"additional","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Antje J.","family":"Baeumner","sequence":"additional","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6118-6182","authenticated-orcid":false,"given":"Nongnoot","family":"Wongkaew","sequence":"additional","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"297","published-online":{"date-parts":[[2025,4,11]]},"reference":[{"key":"5869_CR1","doi-asserted-by":"publisher","DOI":"10.1016\/j.microc.2020.105910","volume":"163","author":"R Rajeev","year":"2021","unstructured":"Rajeev R, Datta R, Varghese A, Sudhakar YN, George L. 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