As previously described by Tu et al. (2010) (link), preparative HPLC separations were performed on a Gemini 5-μm C18 110A column (30 mm × 50 mm, 5 μm, Phenomenex, Inc., Torrance, CA, United States). A Shimadzu LC-8A binary preparative pump with a Shimadzu SCL-10A VP system controller was connected to the Gilson 215 auto sampler and Gilson 215 fraction collector (Gilson, Inc., Middleton, WI, United States). Detections were performed by a Shimadzu SPD-M20A diode-array detector and a Shimadzu ELSD-LT II evaporative light-scattering detector (Shimadzu Corp., Kyoto, Japan). The mobile phase consisted of water (A) and Acetonitrile (B): 0 min, 98:2; 0.5 min, 98:2; 6.5 min, 0:100; 12.3 min, 0:100; 12.5 min, 98:2; 12.95 min, stop. The flow rate was 25 mL/min. Briefly, fractions (A – fractions 1–6, B – fractions 7–9, C – fractions 10–17, D – fractions 18–31, E – fractions 32–41, F – fractions 42–100) were collected and combined based on mass spectra data; their TLC profiles and biological properties were evaluated (Supplementary Figure S1).
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