Analytical RP-HPLC was performed on a LC Dionex UltiMate 3000 (ThermoFisher Scientific, Waltham, MA, USA), using a Kinetex Reversed Phase C18 column (100 × 4.6 mm). Gradients of 0.1% TFA in H2O (B) and 0.1% TFA in CH3CN (A) were used, at a flow rate 0.4 mL/min with UV detection at 220 and 254 nm. Preparative HPLC was done on a CombiFlash, EZPrep, Teledyne ISCO (Lincoln, NE, USA) using a Supelco Discovery BIO Wide Pore C18 column (25 cm × 21.2 mm, 10 mm; Sigma-Aldrich) flow rate 5 mL/min, detection wavelengths 220 and 254 nm, gradient ratio A (0.1% TFA in CH3CN) and B (0.1% TFA in H2O) 0:100 to 18:82 in 30 min, followed by an isocratic run for 5 min.
Mass Spectrometry analysis was performed on a Bruker microOTOF-QIII (Bruker Corporation, Billerica, MA, USA).