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色谱 2010
Separation and preparation of two rotenoids from the roots of Derris by high-speed counter-current chromatography
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Abstract:
Two rotenoids (rotenone and deguelin) were successfully isolated and purified from the roots of Derris by high-speed counter-current chromatography (HSCCC) with a two-phase solvent system composed of n-hexane-ethylacetate-methanol-water (7:0.25:5:3, v/v/v/v) on a preparative scale. The lower phase was used as the mobile phase and the upper phase was used as the stationary phase. The revolution speed was 850 r/min, the detection wavelength was set at 254 nm and the flow rate was 2.0 mL/min. Under the optimized conditions, within 2.5 h, 6.4 mg of rotenone with the purity of 96.60% and 23.4 mg of deguelin with the purity of 97.87% were obtained from 50 mg of the crude extract of the roots of Derris in a one-step elution. The results indicate that the rotenone and deguelin with high purities can be obtained by HSCCC, and the established method can provide the basic experimental material for the intensive study of rotenoids.