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Despite their relatively high molecular weights, many PFAS exhibit sufficient volatility to be analyzed by gas chromatography coupled with mass spectrometry (GC-MS). In this study, a novel analytical workflow was developed for extracting and analyzing (semi-)volatile PFAS in soil samples, combining dynamic headspace extraction (DHS) using thermal desorption (TD) tubes with both one-dimensional gas chromatography (1D-GC) and comprehensive two-dimensional gas chromatography (GC\u00d7GC), each coupled with time-of-flight mass spectrometry (TOFMS). Nine target PFAS compounds were selected, comprising fluorotelomer alcohols (FTOHs), fluorotelomer acrylates (FTAc), and sulfonamide-based derivatives (N-MeFOSA, N-EtFOSA, N-MeFOSE, and N-EtFOSE). Building on a prior aqueous-sample study, Tenax TA was identified as the optimal sorbent based on recovery and reproducibility. Extraction volumes of 1 L, 2 L, and 5 L were evaluated, with 1 L providing the best recovery-reproducibility balance. Three different conditions (no solvent, pure water, and 1:1 (\n                    <jats:italic>v\/v<\/jats:italic>\n                    ) water-methanol mixture) were tested to evaluate solvent effects. The water-methanol mixture yielded the highest recovery, ensuring consistent reproducibility. Detection limits as low as 7.02\u00a0pg\u00a0g\u207b\n                    <jats:sup>1<\/jats:sup>\n                    were achieved, demonstrating excellent sensitivity. In a soil case study, the use of GC\u00d7GC-TOFMS enabled the identification of 106 additional environmentally relevant compounds. Overall, the DHS-TD-GC\u00d7GC-TOFMS approach offers a sensitive, robust platform for quantifying (semi-)volatile PFAS and screening other trace contaminants, supporting comprehensive environmental monitoring.\n                  <\/jats:p>\n                  <jats:p>\n                    <jats:bold>Graphical Abstract<\/jats:bold>\n                  <\/jats:p>","DOI":"10.1007\/s00216-025-06266-4","type":"journal-article","created":{"date-parts":[[2025,12,16]],"date-time":"2025-12-16T02:19:29Z","timestamp":1765851569000},"page":"3137-3145","update-policy":"https:\/\/doi.org\/10.1007\/springer_crossmark_policy","source":"Crossref","is-referenced-by-count":2,"title":["Development and optimization of PFAS extraction in soil\u2019s headspace followed by multidimensional gas chromatography and mass spectrometry"],"prefix":"10.1007","volume":"418","author":[{"given":"Maria Chiara","family":"Corviseri","sequence":"first","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Allan","family":"Dos Santos Polidoro","sequence":"additional","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Claudia","family":"Stevanin","sequence":"additional","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Luisa","family":"Pasti","sequence":"additional","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7236-4266","authenticated-orcid":false,"given":"Flavio Antonio","family":"Franchina","sequence":"additional","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]}],"member":"297","published-online":{"date-parts":[[2025,12,16]]},"reference":[{"key":"6266_CR1","doi-asserted-by":"publisher","first-page":"513","DOI":"10.1002\/IEAM.258","volume":"7","author":"RC Buck","year":"2011","unstructured":"Buck RC, Franklin J, Berger U, Conder JM, Cousins IT, Voogt P, Jensen AA, Kannan K, Mabury SA, van Leeuwen SPJ. Perfluoroalkyl and polyfluoroalkyl substances in the environment: terminology, classification, and origins. Integr Environ Assess Manag. 2011;7:513\u201341. https:\/\/doi.org\/10.1002\/IEAM.258.","journal-title":"Integr Environ Assess Manag"},{"key":"6266_CR2","doi-asserted-by":"publisher","DOI":"10.1016\/J.ACA.2023.341206","volume":"1260","author":"AA Olomukoro","year":"2023","unstructured":"Olomukoro AA, DeRosa C, Gionfriddo E. Investigation of the adsorption\/desorption mechanism of perfluoroalkyl substances on HLB-WAX extraction phases for microextraction. Anal Chim Acta. 2023;1260: 341206. https:\/\/doi.org\/10.1016\/J.ACA.2023.341206.","journal-title":"Anal Chim Acta"},{"key":"6266_CR3","doi-asserted-by":"crossref","unstructured":"Kirsch P. Modern fluoroorganic chemistry. 2nd ed. Weinheim: Wiley; 2013.","DOI":"10.1002\/9783527651351"},{"key":"6266_CR4","unstructured":"Kissa E. Fluorinated surfactants and repellents. 2nd ed.\u00a0New York: Marcel Dekker, Inc.; 2001."},{"key":"6266_CR5","doi-asserted-by":"publisher","first-page":"13","DOI":"10.1071\/CH14165","volume":"68","author":"J Gardiner","year":"2015","unstructured":"Gardiner J. Fluoropolymers: origin, production, and industrial and commercial applications. Aust J Chem. 2015;68:13. https:\/\/doi.org\/10.1071\/CH14165.","journal-title":"Aust J Chem"},{"key":"6266_CR6","doi-asserted-by":"publisher","first-page":"24201","DOI":"10.1007\/s11356-017-0072-5","volume":"24","author":"X Wu","year":"2017","unstructured":"Wu X, Liang M, Yang Z, Su M, Yang B. Effect of acute exposure to PFOA on mouse liver cells in vivo and in vitro. 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