Preparative isolation and purification of three rotenoids and one isoflavone from the seeds of Millettia pachycarpa Benth by high-speed counter-current chromatography
2008
Ye, Haoyu | Chen, Lijuan | Li, Yanfang | Peng, Aihua | Fu, Afu | Song, Hang | Tang, Minghai | Luo, Houding | Luo, Youfu | Xu, Yongbin | Shi, Jianyou | Wei, Yuquan
Both analytical and preparative high-speed counter-current chromatography (HSCCC) were used to isolate and separate chemical bioactive constituents from the seeds of Millettia pachycarpa Benth, a famous traditional Chinese medicine. Three rotenoids and one isoflavone were successfully purified for the first time by HSCCC with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (HEMWat) (1:0.8:1:0.6, v/v/v/v). The separation parameters were first performed on the analytical HSCCC and optimized conditions were then scaled up to preparative HSCCC. The separation produced 160.2mg tephrosin, 14.6mg 4',5'-dimethoxy-6,6-dimethylpyranoisoflavone, 109.4mg deguelin, 6.7mg 6a,12a-dehydrodeguelin with respective purities of 95, 93, 95, 95%, in one single run from 400mg crude extract of the seeds of M. pachycarpa Benth. The purity of the isolated compounds was analyzed by high-performance liquid chromatography (HPLC) and their structures were identified by electrospray ionization mass spectrometry (ESI-MS); ¹H nuclear magnetic resonance (¹H NMR) and ¹³C nuclear magnetic resonance (¹³C NMR) analysis. This paper is an excellent example of the role that CCC is playing in isolating active compounds for pre-clinical trials of new chemical entities, even when scaling up between centrifuges from different manufacturers.
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