*4.1. General*

The NMR spectra were recorded on a Bruker FT-400 MHz NMR spectrometer and samples were dissolved in deuterated acetone-*d6*. Mass data were acquired on aXevoTM G2 XS-ESI-QTof mass spectrometer (Waters Corp., Manchester, UK). For thin layer chromatography (TLC) analysis, precoated Merck plates (silica gel 60 F254) were utilized. Silica gel (100–200 mesh) (Qing-dao Marine Chemical, Inc., Qingdao, China) was chosen for column chromatographic separation. Semi-preparative chromatography was performed on a Gilson HPLC (Middleton, WI, USA) instrument equipped with a 321 binary pump, GX-281 liquid handler, and UV-155 detector with X Select HSS T3 (250 mm × 100 mm, 5 μm) (Waters Corp., Drinagh, Ireland) as a stationary phase using a Trilution LC v2.1 platform. Formic acid (OptimaTM Mass spec grade) (Thermo Fisher Scientific, Geel, Belgium), HPLC-grade acetonitrile, LiChrosolv (Merck, Darmstadt, Germany), and ultra-pure water (Millipore System, Randolph, MA, USA) were used.

#### *4.2. Instrumental UPLC Conditions*

The instrumental conditions were set-up as per our recent report (Reddy et al., 2019) with slight modifications. Chromatographic separation was performed on an Acquity H Class UPLC system (Waters, Milford, MA, USA) with a conditioned auto sampler using an ACQUITY UPLC CSH Phenyl-Hexyl column (100 mm × 2.1 mm id., 1.7 μm particle size) (Waters, Milford, MA, USA). Column temperature was maintained at 40 ◦C. Highresolution masses of secondary metabolites were measured after UPLC separation. A mobile phase consisting of water with 0.1% formic acid in water (solvent A) and acetonitrile with 0.1% formic acid (solvent B) was pumped at a flow rate of 0.4 mL/min. The gradient elution program was as follows: 0 min, 5% B; 3.00 min, 20% B; 5.00min, 35% B; 7.50 min, 50% B; 10.00 min, 70% B; 12.50 min, 95% B; 17.00 min 95% B; and 21.00 min 5% B. The equilibration time was 4.0 min and the injection volume was 2 μL. The LC-QTof-MS<sup>E</sup> mode was applied to analyze the samples in both TIC as well as the MS/MS mode, where the collision energy was ramped at 15–45 eV. Eluted compounds were detected from *m*/*z* 50 to 1200 using a Xevo G2-XS Q-Tof mass spectrometer (Waters, Manchester, UK), which was connected to Electro-spray ionization (ESI) interface with a negative ion mode using the following instrument settings: capillary voltage, 2.0 KV; sample cone, 40 V; source temperature, 120 ◦C; desolvation temperature 350 ◦C; cone gas flow rate 50 L/h; desolvation gas (N2) flow rate 850 L/h, argon as CID gas for MS/MS experiments. All analyses were performed using lock spray, which ensured accuracy and reproducibility. Leucine–Enkephalin (5 ng/mL) was used as a lock mass, generating a reference ion in the negative mode at *m*/*z* 554.2615, and was introduced by a lock spray at 10 μL/min for accurate mass acquisition. Data acquisition was achieved using MassLynx ver. 4.1. Acquiring data in this manner provided information on intact precursor ions as well as fragment ions.
