Preparative Separation of Fruit Extract of Silybum Marianum Using a High-Speed Countercurrent Chromatograph With Scale-Up Columns

A crude extract (12 g) of fruits of Silybum marianum was separated with a two-phase solvent system composed of water/ methanol/ethyl acetate/n-hexane (4 : 3 : 4 : 1, v/v/v/v) by high speed countercurrent chromatography. Using a set of three large multilayer coil separation columns with a total capacity of 2460 mL, the separation yielded 1.37 g of silycristin at 93.1% purity, 3.47 g of silybin at 95.7% purity, and 0.93 g of isosilybin at 89.7% purity.