Two-dimensional counter-current chromatography for the preparative separation of prenylflavonoids from Artocarpus altilis.
A two-dimensional counter-current chromatographic system (2D-CCC) for preparative isolation and purification of three prenylflavonoids from Artocarpus altilis is presented. An upright CCC instrument (CCC1, total capacity: 1600 ml) was used as the first dimension. Effluent of interest from CCC1 was collected on-line into a 30 ml sample loop by a laboratory-prepared column-switching interface and introduced into a high-speed CCC instrument (CCC2, total capacity: 210 ml) for the second dimension separation. With this 2D-CCC system and a pair of two-phase solvent systems composed of n-hexane-ethyl acetate-methanol-water (5:5:7:3 and 5:5:6.5:3.5, v/v/v/v), which had been selected by high-speed CCC, about a 500 mg amount of the crude extract was separated, yielding 9 mg of compound 1, 28 mg of compound 2 and 78 mg of compound 3. The purities of the three prenylflavonoids were 98.7 (1), 98.3 (2) and 97.2% (3), respectively, as determined by HPLC analysis. Their chemical structures were identified by electrospray ionization MS, (1)H NMR and (13)C NMR.
Lu
Yanbin
Y
Department of Chemistry, Zhejiang University, Hangzhou, Zhejiang Province 310027, China.
Sun
Cuirong
C
Wang
Yu
Y
Pan
Yuanjiang
Y
D031622:Artocarpus / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid; D003377:Countercurrent Distribution / Q000295:instrumentation / Q000379:methods*; D005419:Flavonoids / Q000737:chemistry / Q000302:isolation & purification*; D015394:Molecular Structure; D021241:Spectrometry, Mass, Electrospray Ionization
D005419:Flavonoids