ABSTRACT
Objective: To isolate dehydrocorydaline and glaucine by high-speed counter-current chromatography (HSCCC) from the extraction of Corydalis Rhizoma (CR). Methods: A mixture of chloroform-n-butanol-methanol-water (4:1:2:5) was used as the two phase solvent system both in forward and reversal direction, with a flow rate of 10.0 mL/min and a rotary speed of 800 r/min eluting for 30 min. The detection wavelength was 282 nm and injection volume was 50 mg. The purity of the target product was analyzed by HPLC-UV and the structure was identified by ultra performance liquid chromatography-tandem quadrupole time-of- flight mass spectrometry (UPLC-Q-TOF-MS/MS). Results: Under optimized conditions, 7.1 mg and 3.4 mg of two compounds were obtained and their yields were 81.43% and 91.11% respectively. Their purities were 98.9% and 94.3% detected by HPLC. dehydrocorydaline and glaucine were identifiled through HPLC, ultraviolet absorbance, and UPLC-Q-TOF-MS/MS. Conclusion: The result indicate that HSCCC is a powerful technique for the purification of dehydrocorydaline and glaucine from CR.
ABSTRACT
Objective: To develop an effective and rapid method for the preparation of 23-acetate alisol B from Alisma orientalis. Methods: The SFE-CO2 extract from A. orientalis was injected into high speed counter current chromatography (HSCCC) directly, and eluted with difierent solvent systems. The crystalline purity was detected by HPLC. The structure of the target compound was identified by UV, IR, MS, and NMR. Results: The solvent system composed of n-hexane-ethylacetate- methanol-water (3∶2∶3∶2) was the best. The lower phase was used as the mobile phase and performed at a flow rate of 2 m/min, while the apparatus rotated at 800 r/min, and detected at 254 nm. The prepared alisol B 23-acetate was identified with infrared spectrometry (IR), mass spectrometry (MS), and nuclear magnetic resonance (NMR) detection, and its purity was 99.8% analyzed by HPLC. Conclusion: The established method is relatively simple, fast, and suitable for the fast isolation and separation of alisol B 23-acetate.
ABSTRACT
A high-speed counter-current chromatography (HSCCC) method was successfully developed for the preparative separation and purification of deoxyschizandrin from Schisandrae Sphenantherae Fructus in one step. The purity of deoxyschizandrin was 98.5%, and the structure was identified by MS, UV and NMR. This method was simple, fast, convenient and appropriate to prepare pure compound as reference substances for related research on Schisandrae Sphenantherae Fructus.
ABSTRACT
An efficient method for the isolation and purification of 12,13-dihydroxyeuparin from Radix Eupatorii Chinensis by high speed counter-current chromatography (HSCCC) was established in this paper.The ether extracts of Radix Eupatorii Chinensis were purified by HSCCC with a solvent system of hexyl hydride ethyl acetate-methanol-water (1∶2∶1∶2,v/v/v/v).The upper phase was used as the stationary phase and the lower phase as the mobile phase.About 8.4 mg of 12,13-dihydroxyeuparin was obtained from 200 mg of ether extracts from Radix Eupatorii Chinensis in one-step HSCCC separation,with the purity of 96.71％,as determined by HPLC.After methanolwater recrystallization,the purity of 12,13-dihydroxyeuparin reached 99.83％.Such a simple and effective method was fairly useful to prepare pure compound as reference substances for related study on Radix Eupatorii Chinensis.
ABSTRACT
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.
ABSTRACT
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.
ABSTRACT
In this article, the author reported the recent development in study on high-speed counter-current chromatography (HSCCC) and finger print, work principle and technology speciality of HSCCC, and noted that the prospect of HSCCC application in separation and analysis of Chinese medicines and herbal medicines is broad as rapid development of the pharmacentical industry of Chinese medicine, even though the application is still in its infancy at present.