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The\u00a0optimization and application of the developed assay\u00a0is presented\u00a0 showing the: (i) exploration of different methods for LTG separation from human serum; (ii) implementation of a molecular adsorption step on an ordered Au nanopillar SERS substrate; (iii) adaptation of a fast scanning of the SERS substrate, performed with a custom-built compact Raman spectrometer; and (iv) development of LTG quantification methods with univariate and multivariate spectral data analysis. Our results showed, for the first time, the SERS-based characterization of LTG and its label-free identification in human serum. We found that combining a miniaturized solid phase extraction, as sample pre-treatment with the SERS assay, and using a multivariate model is an optimal strategy for LTG quantification in human serum in a linear range from 9.5 to 75\u00a0\u03bcM, with LoD and LoQ of 3.2\u00a0\u03bcM and 9.5\u00a0\u03bcM, respectively, covering the suggested clinical therapeutic window. We also showed that the developed assay allowed for quantifying LTG from human serum in the presence of other drugs, thereby demonstrating the robustness of label-free SERS. The sensing approach and instrumentation can be further automated and integrated in devices that can advance the drug monitoring in real clinical settings.<\/jats:p>\n                <jats:p><jats:bold>Graphical abstract<\/jats:bold><\/jats:p>","DOI":"10.1007\/s00604-023-06085-3","type":"journal-article","created":{"date-parts":[[2023,12,1]],"date-time":"2023-12-01T04:36:25Z","timestamp":1701405385000},"update-policy":"https:\/\/doi.org\/10.1007\/springer_crossmark_policy","source":"Crossref","is-referenced-by-count":17,"title":["Label-free SERS assay combined with multivariate spectral data analysis for lamotrigine quantification in human serum"],"prefix":"10.1007","volume":"190","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-9153-7158","authenticated-orcid":false,"given":"Isidro","family":"Badillo-Ram\u00edrez","sequence":"first","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Selina A. 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