A scaled-up SRCCC apparatus equipped with a 40-L column was constructed on the basis of separations of crude broccoli seed extract and crude radish seed extract using a conventional SRCCC instrument. Scaled-up separation of 500 g of crude broccoli seed extract with n -butanol-acetonitrile-10% (NH 4 ) 2 SO 4 aqueous solution 1:0.5:2 (υ/υ) as solvent system yielded 61.5 g glucoraphanin product of purity 91.2%. Separation of 500 g crude radish seed extract with the same solvents in the ratio 0.5:1:2 (υ/υ) afforded 26.7 g glucoraphenin product of purity 94.5%. Recovery of glucoraphanin and glucoraphenin from the crude extracts was 98.3 and 98.9%, respectively. The results demonstrated that this SRCCC technology is useful for separation of glucosinolates from plant extracts.