*5.3. LC-MS*/*MS Analysis*

The mass spectrometer Thermo Q-Exactive Plus (Thermo Scientific, San Jose, CA, USA) was equipped with heated electrospray ionization (HESI) source. Capillary temperature and vaporizer temperature were set at 330 and 280 ◦C, respectively, while the electrospray voltage was adjusted at 3.50 kV (operating in both positive and negative mode). Sheath and auxiliary gas were 35 and 15 arbitrary units, with an S lens RF level of 60.

The mass spectrometer was controlled by the Xcalibur 3.0 software (Thermo Fisher Scientific, San Jose, CA, USA). The exact masses of the compounds were calculated using Qualbrowser in Xcalibur 3.0 software. The mass scan range was set in the range of *m*/*z* 100–1000.

The column was a Waters Acquity UPLC BEH C18 column (100 mm × 2.1 mm, 1.7 μm particle size). The mobile phases were (a) water with 0.1% (*v*/*v*) formic acid and (b) methanol with 0.1% (*v*/*v*) formic acid. The optimized elution conditions were as follows: holding at 10% B for 2 min, a linear gradient from 10% to 13% B (all *v*/*v*) (2 to 4 min), 13% to 15% B (4 to 10 min), 15% to 17% B (10 to 15 min), 17% to 21% B (15 to 19 min), 21% to 29% B (19 to 24 min), 29% to 53% B (24 to 29 min), 53% to 75% B (29 to 35 min), 75% to 100% B (35 to 36 min), isocratic 100% B for 1 min, and then back to 7% B in 1 min. The flow rate was 0.3 mL/min. The column temperature was 35 ◦C. The injection volume was 2 μL.
