performed on a Hypersil GOLD aQ (ThermoFisher Scientific) column (100
mm × 2.1 mm, 1.9 μm) using a solvent system consisting
of A: H2O with 0.02% AcOH and B: MeCN with 0.02% AcOH (linear
gradient from 0 to 100% B in 30 min) at a flow rate of 0.2 mL/min
at 30 °C and UV detection at 254 nm. Fractions detected using
low-resolution mass spectra (HRMS) were obtained on a LC QTOF mass
spectrometer.
on a Q Exactive mass spectrometer (Thermo Fisher Scientific), equipped
with an electrospray ionization source (H-ESI II probe) coupled with
an Accela 1250 Pump (Thermo Fisher Scientific). Samples were injected
onto a Thermo Fisher Hypersil GOLD aQ chromatography column (100 mm
× 2.1 mm, 1.9 μm particle size). The flow rate was set
at 0.3 mL/min, and the mobile phase consisted of water containing
0.02% acetic acid (solvent A) and acetonitrile containing 0.02% acetic
acid (solvent B). The gradient program was as follows: 0 to 5 min,
2% B; 5 to 20 min, up to 70% B; 20 to 30 min, came back to 98% B and
2 min of equilibration. The column temperature was maintained at 30
°C, and the temperature of the autosampler was set at 4 °C.
MS analyses were performed in a full scan negative ion mode with a
scan range from 200 to 1500 m/z.