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Thermal decomposition gold amalgamation atomic absorption spectrophotometry (TDA-AAS) is an efficient and cost-effective technique for measuring low levels of total mercury requiring no sample preparation. Measuring methylmercury with TDA-AAS requires isolating methylmercury from the matrix and other mercury species prior to detection. We developed a method that uses ethyl acetate instead of a legacy non-polar solvent, toluene. Toluene is a potentially hazardous and problematic solvent whereas ethyl acetate is greener and safer. Additionally, the salting-out assisted liquid\u2013liquid extraction (SALLE) approach with ethyl acetate avoids emulsion formation throughout extraction. We describe method development and validation of a SALLE and TDA-AAS detection for methylmercury in finfish. From 10 reference materials, our method recovered 80\u2013118% of total or methylmercury with\n                    <jats:italic>Z<\/jats:italic>\n                    scores ranging from\u2009\u22121.98 to 2.75 (\n                    <jats:italic>n<\/jats:italic>\n                    \u2009=\u2009184). The LOD and LOQ of the method for methylmercury were 3.8 and 27\u00a0ng\/g, respectively. From extraction to detection, accurate results were obtained from a sample in less than 2\u00a0h for both total mercury and methylmercury.\n                  <\/jats:p>\n                  <jats:p>\n                    <jats:bold>Graphical Abstract<\/jats:bold>\n                  <\/jats:p>","DOI":"10.1007\/s00216-025-05989-8","type":"journal-article","created":{"date-parts":[[2025,7,16]],"date-time":"2025-07-16T21:58:18Z","timestamp":1752703098000},"page":"4723-4738","update-policy":"https:\/\/doi.org\/10.1007\/springer_crossmark_policy","source":"Crossref","is-referenced-by-count":8,"title":["Development and validation of a non-chromatographic method for mercury and methylmercury in finfish using thermal decomposition gold amalgamation atomic absorption spectrophotometry (TDA-AAS) and salting-out assisted liquid\u2013liquid extraction (SALLE)"],"prefix":"10.1007","volume":"417","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-1818-5704","authenticated-orcid":false,"given":"Jake A.","family":"Carter","sequence":"first","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-4968-7486","authenticated-orcid":false,"given":"Charles A.","family":"Barber","sequence":"additional","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-5586-6643","authenticated-orcid":false,"given":"Mesay M.","family":"Wolle","sequence":"additional","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8248-2749","authenticated-orcid":false,"given":"Patrick J.","family":"Gray","sequence":"additional","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"297","published-online":{"date-parts":[[2025,7,16]]},"reference":[{"key":"5989_CR1","unstructured":"U.S. Food & Drug Administration (2024) Mercury in food. https:\/\/www.fda.gov\/food\/environmental-contaminants-food\/mercury-food. 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