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This study examined how rational formulation design influences physicochemical properties, extraction performance, energy efficiency, thermal behavior, and cytocompatibility during bioactive recovery from Nigella sativa seeds. Twelve formulations spanning malic acid\u2013polyol, citric acid\u2013polyol, binary polyol, and ternary acid\u2013polyol families were evaluated under standardized ultrasound-assisted conditions and compared with ethanolic ultrasound-assisted extraction, Soxhlet extraction, and cold-pressed oils. Selected NADES formulations outperformed the conventional systems. E1 (malic acid:glycerol:water) achieved the highest total phenolic content and lowest specific energy consumption (40.00 kJ mg\u22121 GAE), below the Soxhlet benchmark (55.17 kJ mg\u22121 GAE), whereas E9 (glycerol:xylitol:water) exhibited the greatest ABTS activity. Neat-NADES apparent pH and viscosity were inversely associated with total phenolic content, while viscosity and density were inversely associated with ABTS activity. ATR-FTIR showed stable, solvent-dominated fingerprints over 15 days, whereas DSC better differentiated neat NADES from their extracts. Most systems remained cytocompatible at 10,000\u00d7 dilution, while acid\u2013polyol formulations reduced viability at 500\u00d7; partial neutralization of N5\/E5 restored viability. NADES performance was formulation- and application-dependent, requiring joint optimization of composition, acidity, viscosity, energy efficiency, and biologically compatible concentration.<\/jats:p>","DOI":"10.3390\/molecules31162854","type":"journal-article","created":{"date-parts":[[2026,8,17]],"date-time":"2026-08-17T10:04:36Z","timestamp":1786961076000},"page":"2854","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["From Solvent Design to Biological Response: Structure\u2013Property Relationships of Edible Natural Deep Eutectic Solvents for the Extraction of Nigella sativa Bioactives"],"prefix":"10.3390","volume":"31","author":[{"ORCID":"https:\/\/orcid.org\/0009-0002-8616-0525","authenticated-orcid":false,"given":"Emina","family":"Mehmedovi\u0107","sequence":"first","affiliation":[{"name":"Faculty of Technology and Faculty of Natural Sciences and Mathematics, University of Tuzla, 75000 Tuzla, Bosnia and Herzegovina"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-9356-0813","authenticated-orcid":false,"given":"Vesna B.","family":"Jovanovi\u0107","sequence":"additional","affiliation":[{"name":"CoE for Molecular Food Sciences, Department of Biochemistry, University of Belgrade\u2014Faculty of Chemistry, Studentski Trg 12-16, 11158 Belgrade, Serbia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8794-9408","authenticated-orcid":false,"given":"Maja","family":"Krsti\u0107 Ristivojevi\u0107","sequence":"additional","affiliation":[{"name":"CoE for Molecular Food Sciences, Department of Biochemistry, University of Belgrade\u2014Faculty of Chemistry, Studentski Trg 12-16, 11158 Belgrade, Serbia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-9264-4406","authenticated-orcid":false,"given":"Smilja","family":"Markovi\u0107","sequence":"additional","affiliation":[{"name":"Institute of Technical Sciences of SASA, Knez Mihailova 35\/IV, 11000 Belgrade, Serbia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0604-9246","authenticated-orcid":false,"given":"Ivana","family":"Prodi\u0107","sequence":"additional","affiliation":[{"name":"Institute of Virology, Vaccines and Sera \u201cTorlak\u201d, Vojvode Stepe 458, 11152 Belgrade, Serbia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0005-8133-0574","authenticated-orcid":false,"given":"Husejin","family":"Keran","sequence":"additional","affiliation":[{"name":"Faculty of Technology, University of Tuzla, 75000 Tuzla, Bosnia and Herzegovina"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-4774-8895","authenticated-orcid":false,"given":"Katarina","family":"Smiljani\u0107","sequence":"additional","affiliation":[{"name":"CoE for Molecular Food Sciences, Department of Biochemistry, University of Belgrade\u2014Faculty of Chemistry, Studentski Trg 12-16, 11158 Belgrade, Serbia"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"1968","published-online":{"date-parts":[[2026,8,15]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","unstructured":"Hannan, M.A., Rahman, M.A., Sohag, A.A.M., Uddin, M.J., Dash, R., Sikder, M.H., Rahman, M.S., Timalsina, B., Munni, Y.A., and Sarker, P.P. 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