Separation and purification of tanshinone from Salvia miltiorrhiza by combination of silica gel and high-speed counter-current chromatography / 中草药

Objective: To develop a method for separation and purification of tanshinone from Salvia miltiorrhiza by combination of silica gel and high-speed counter-current chromatography (HSCCC). Methods: The crude extract of S. miltiorrhiza was separated by silica gel chromatography and F1 and F2 were obtained. Then, F1 and F2 were separated by HSCCC with a two-phase solvent system composed of petroleum ether-methanol-water (4:3:4:2 and 8:5:8:3), respectively. The lower phase was used as the mobile phase with a flow rate of 2.0 mL/min, while the apparatus rotated at 850 r/min and the eluates were detected at 254 nm. The structures of the target compounds were identified by ESI-MS and NMR. Results: From 80 mg of F1, three compounds with tanshinone I (14 mg), dihydrotanshinone I (22 mg), and tanshinone IIA (26 mg) were obtained. And from 80 mg of F2, dihydrotanshinone (11 mg), trijuganone B (15 mg), and cryptotanshinone (30 mg) were obtained. The purities of these six compounds determined by HPLC were all over 96%, respectively. Conclusion: Combination of silica gel and HSCCC is an efficient method for separation of tanshinone from S. miltiorrhiza.

Isolation and purification of alpinetin and cardamomin from Alpinia katsumadai by high speed counter-current chromatography / 中草药

Objective: The aim of the study was to establish a high speed counter-current chromatography (HSCCC) method for the isolation and purification of alpinetin and cardamomin from Alpinia katsumadai. Methods: Two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (5 : 5 : 7 : 3) was used. The flow rate of the mobile phase was 2.0 mL/min, the revolution speed was 800 r/min, the separation temperature was controlled at 25 °C, the reservation ratio of the stationary phase was 50%, and the detection wavelength was 300 nm. Results: Alpinetin (17.2 mg) and cardamomin (25.1 mg) could be obtained from 100 mg of the crude extract in one-step separation by the method. The purities of them were 98.1% and 99.2%, respectively, as determined by HPLC and their chemical structures were identified by 1H-NMR and 13C-NMR. Conclusion: The traditional method, column elution, could not eliminate irreversible adsorption, while the HSCCC method used for the isolation and purification of alpinetin and cardamomin from A. katsumadai has many advantages, such as facility, high efficiency, and high recovery as well.