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Methods: The oleo-gum resins of F. tadshikorum (OGRFT) and F. foetida (OGRFF) were analyzed using HS-GC-MS, UHPLC-MS, and NMR. Results: A total of 40 compounds were detected by HS-GC-MS, representing 94% and 97% of the volatiles in F. foetida and F. tadshikorum, respectively. The major volatile constituents of the resins were disulfides. RP-UHPLC-ESI-QqTOF-MS\/MS tentatively identified 51 compounds, including sesquiterpene coumarins, sesquiterpenes, sulfides, phenolics and fatty acids in both OGRFT and OGRFF. NMR (1D and 2D) confirmed the identity of five major compounds and provided complete signal assignments for their potential quantification. UHPLC-MS revealed that OGRFF was rich in foetisulfide A, followed by daucane sesquiterpenes and esters of sesquiterpenes and fatty acids, while OGRFT was dominated by galbanic acid and 8-acetoxy-5-hydroxyumbelliprenin, as confirmed by both UHPLC-MS and NMR. Anthelmintic, antifungal, and cytotoxic assays demonstrated that the oleo-gum resins were non-toxic, at least in the in vitro test systems addressed. Conclusions: This study provides the first comprehensive metabolite profiling of oleo-gum resins from F. foetida and F. tadshikorum, revealing distinct chemical compositions and supporting the preferential use of F. tadshikorum in food applications. Advanced analytical approaches (HS-GC-MS, UHPLC-MS\/MS, and NMR) identified key marker compounds, particularly sesquiterpene coumarins, enabling reliable differentiation, standardization and quality control.<\/jats:p>","DOI":"10.3390\/plants15182781","type":"journal-article","created":{"date-parts":[[2026,9,11]],"date-time":"2026-09-11T08:17:42Z","timestamp":1789114662000},"page":"2781","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Combination of GC-MS, UHPLC-MS, and NMR Reveals Metabolic Differences Between the Oleo-Gum Resins of Ferula tadshikorum Pimenov and F. foetida (Bunge) Regel"],"prefix":"10.3390","volume":"15","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-1756-3638","authenticated-orcid":false,"given":"Nilufar Z.","family":"Mamadalieva","sequence":"first","affiliation":[{"name":"Institute of the Chemistry of Plant Substances, Uzbekistan Academy of Sciences, M. Ulugbek Str 77, Tashkent 100170, Uzbekistan"},{"name":"Department of Pharmacy and Chemistry, Faculty of Dentistry and Pharmacy, Alfraganus University, Yuqori Qoraqamish Str. 2a, Tashkent 100190, Uzbekistan"},{"name":"Department of Bioorganic Chemistry, Leibniz Institute of Plant Biochemistry, Weinberg 3, 06120 Halle (Saale), Germany"}],"role":[{"vocabulary":"crossref","role":"author"},{"role":"conceptualization","vocabulary":"credit"},{"role":"software","vocabulary":"credit"},{"role":"validation","vocabulary":"credit"},{"role":"formal-analysis","vocabulary":"credit"},{"role":"resources","vocabulary":"credit"},{"role":"data-curation","vocabulary":"credit"},{"role":"writing-original-draft","vocabulary":"credit"},{"role":"writing-review-editing","vocabulary":"credit"},{"role":"visualization","vocabulary":"credit"},{"role":"supervision","vocabulary":"credit"},{"role":"project-administration","vocabulary":"credit"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-4537-7173","authenticated-orcid":false,"given":"Michal","family":"\u0160oral","sequence":"additional","affiliation":[{"name":"Analytical Department, Institute of Chemistry, Slovak Academy of Sciences, D\u00fabravsk\u00e1 cesta 9, SK-845 38 Bratislava, Slovakia"}],"role":[{"vocabulary":"crossref","role":"author"},{"role":"software","vocabulary":"credit"},{"role":"writing-review-editing","vocabulary":"credit"},{"role":"methodology","vocabulary":"credit"},{"role":"validation","vocabulary":"credit"},{"role":"formal-analysis","vocabulary":"credit"},{"role":"data-curation","vocabulary":"credit"},{"role":"visualization","vocabulary":"credit"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1631-8841","authenticated-orcid":false,"given":"Olim K.","family":"Khojimatov","sequence":"additional","affiliation":[{"name":"Institute of Botany, Uzbekistan Academy of Sciences, Durmon Yuli Str 32, Tashkent 100125, Uzbekistan"}],"role":[{"vocabulary":"crossref","role":"author"},{"role":"investigation","vocabulary":"credit"}]},{"given":"Davlat K.","family":"Akramov","sequence":"additional","affiliation":[{"name":"Institute of the Chemistry of Plant Substances, Uzbekistan Academy of Sciences, M. Ulugbek Str 77, Tashkent 100170, Uzbekistan"}],"role":[{"vocabulary":"crossref","role":"author"},{"role":"investigation","vocabulary":"credit"},{"role":"data-curation","vocabulary":"credit"},{"role":"writing-original-draft","vocabulary":"credit"}]},{"given":"Andrej","family":"Frolov","sequence":"additional","affiliation":[{"name":"Department of Bioorganic Chemistry, Leibniz Institute of Plant Biochemistry, Weinberg 3, 06120 Halle (Saale), Germany"},{"name":"Laboratory of Analytical Biochemistry and Biotechnology, K.A. Timiryazev Institute of Plant Physiology of Russian Academy of Science, Botanicheskaya street 35, 127276 Moscow, Russia"}],"role":[{"vocabulary":"crossref","role":"author"},{"role":"software","vocabulary":"credit"},{"role":"validation","vocabulary":"credit"},{"role":"formal-analysis","vocabulary":"credit"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-2060-8235","authenticated-orcid":false,"given":"Ludger A.","family":"Wessjohann","sequence":"additional","affiliation":[{"name":"Department of Bioorganic Chemistry, Leibniz Institute of Plant Biochemistry, Weinberg 3, 06120 Halle (Saale), Germany"}],"role":[{"vocabulary":"crossref","role":"author"},{"role":"conceptualization","vocabulary":"credit"},{"role":"data-curation","vocabulary":"credit"},{"role":"resources","vocabulary":"credit"},{"role":"writing-review-editing","vocabulary":"credit"},{"role":"writing-original-draft","vocabulary":"credit"},{"role":"supervision","vocabulary":"credit"},{"role":"project-administration","vocabulary":"credit"},{"role":"funding-acquisition","vocabulary":"credit"}]}],"member":"1968","published-online":{"date-parts":[[2026,9,11]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","first-page":"350","DOI":"10.1016\/j.indcrop.2018.12.012","article-title":"The genus Ferula: Ethnobotany, phytochemistry and bioactivities\u2014A review","volume":"129","author":"Mohammadhosseini","year":"2019","journal-title":"Ind. 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