GB1257956A - - Google Patents

Abstract

1,257,956. Preparing polyhydroxyphenylchromones. DR MADAUS & CO. 30 May, 1969 [1 June, 1968; 6 May, 1969], No. 27545/ 69. Heading A5B. In a process for obtaining polyhydroxyphenylchromones (e.g. silymarin), the dried fruit of Silybum marianum Gaertn is subjected to mechanical pressure in order substantially to free it from the fatty oil present therein, the press residue, which contains residual oil in an amount of 5-10% by weight, is exhaustively extracted with ethyl acetate, the extract is evaporated, the oily-greasy, partially lumpy dried residue, which contains about 20-30% by weight of active material, is dissolved, to give an approximately 2% by weight solution, in the lower phase of a ternary solvent system (i.e. water/methanol/pet. ether), centrifuged until clear for the removal of flocculant solid material particles, subjected in this solvent system to a multiplicative partition in countercurrent and the lower phase separated and either (A) evaporated under reduced pressure to give a brownish powder containing 70-80% by weight of polyhydroxyphenyl-chromones, or (B) mixed with about 0.5% by weight of active charcoal, concentrated under a pressure of about 20 mm. Hg. to about one third of the initial volume, the still hot solution clarified through a filter press and further concentrated to one sixth to one tenth of the initial volume, in which concentration range a white to ochre-coloured crystallisate of silymarin I separates out and is separated off. The products may be admixed with a solid or liquid pharmaceutical carrier or diluent.