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

Background: Central Asia is a key center of diversity for Ferula species, including Ferula foetida and Ferula tadshikorum, which are important but insufficiently characterized sources of oleo-gum resins. 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.