Extraction and Isolation.
The air-dried sample (3.6 kg) was extracted with CH2Cl2 at room temperature (×3).
The resulting syrup CH2Cl2 extract (43.7 g) was separated by silica gel column (1.0 kg) and developed by gradient elution with CHCl3 and increasing concentrations of acetone to afford 25 fractions (F1−F25, each 1000 mL).
The active fractions F5 and F6 (2.4 g) were combined and subjected to passage over a C18 reversed-phase (RP-18, 75 g) column.
Elution of this column with 500 mL of MeOH−H2O (9:1) yielded F26, which was then subjected to flash column chromatography on another C18 reversed-phase (RP-18, 130 g) column.