*3.4. UHPLC/HRMS/MS*

Crude extract was analyzed on an Ultimate 3000 UHPLC system (Dionex, Germering, Germany) hyphenated with Impact II high resolution quadrupole time-of-flight (QqTOF) equipped with an electrospray ionization (ESI) source (Bruker Daltonics, Bremen, Germany). Separation of extract was achieved on a Luna C18 column (150 mm × 2.1 mm, 1.6 μm) with an injection volume of 2 μL. A binary solvent system was used as mobile phase, solvent A consisting of water with 0.1% (*v*/*v*) formic acid and solvent B consisting of acetonitrile with 0.1% (*v*/*v*) formic acid. The flow rate was 0.6 mL min−1, and a gradient was applied: from 10% to 100% of B in 15min. The acquisition was carried out in ESI positive ionization mode with a range of 50–1200 Da. The capillary voltage was maintained at 3 kV, the gas flow to the nebulizer was set at 3.5 bars, the drying temperature was 200 ◦C, and the drying gas flow was 4 L min−1. The collision-induced dissociated (CID) energy was applied from 20 to 40 eV.

Data were analyzed using Bruker Data Analysis 4.4 software. The data were processed using MetaboScape 4.0 (Bruker Daltonics, Bremen, Germany). A mgf file was submitted to the GNPS (Global Natural Product Social Networking) web-based platform for generating MS based molecular network [33]. The following parameters were applied to create the molecular network. The mass tolerance was 0.01 Da for precursor and fragment ions. Minimum score was 0.6 between two MS/MS spectra to be connected. The minimum number of common fragment ions between two MS/MS spectra was 3. The nearly identical MS/MS spectra were not merged into consensus MS/MS spectrum. A node was allowed to connect to a maximum of 10 nodes. A cluster can have a maximum of 100 nodes. The spectra in the network were then compared with GNPS spectral libraries [31]. Each MS<sup>2</sup> spectrum of the seven isolated compounds was assigned an individual accession number on the GNPS (Supplementary Materials). The molecular networking was visualized using Cytoscape (ver. 3.6.0). The obtained molecular network can be accessed at: https://gnps. ucsd.edu/ProteoSAFe/status.jsp?task=527472b15d4247dfad0534aa80f7ebfa, accessed on 8 October 2022.
