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2 Acta Chromatographica

2 2008

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Scale-up of slow rotary countercurrent chromatographic isolation of glucoraphanin and glucoraphenin from broccoli seeds and radish seeds

Fu Y., Du Q., Wang K.

Acta Chromatographica

2008

Vol. 20, no. 4

697-707

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.

Isolation of glucosinolates from broccoli seeds by use of high-speed countercurrent chromatography

Du Q., Zhang L., Cui H., Wang K., Xiu L., Sheng L.

Acta Chromatographica

2008

Vol. 20, no. 3

489-496

Cleavage of glucosinolates with myrosinase yields thioglycosidic compounds which have cancer chemoprevention activity. In this paper, glucosinolates in an extract (2.0 g) of broccoli seeds ( Brassica oleracea var. italica ) were separated by high-speed countercurrent chromatography (HSCCC) with the solvent system n -butanol-acetonitrile-10% ammonium sulfate solution 1:0.5:2.2 (v/v) to yield five glucosinolate compounds after desalting and decolorizing by MCI column chromatography. The five compounds, 7-methylsulfinylheptyl glucosinolate (22.4 mg), 4-pentenyl glucosinolate (33.6 mg), 3-butenyl glucosinolate (24.0 mg), 4-methylsulfinylbutyl glucosinolate (161.4 mg), and 3-methylsulfinylpropyl glucosinolate (29.6 mg), were identified by ESI-MS, 1 H NMR and 13 C NMR. The purity of the products was >98%, and 7-methylsulfinylheptyl glucosinolate was obtained from broccoli seeds for the first time.