Tags

Type your tag names separated by a space and hit enter

Preparative isolation and purification of three rotenoids and one isoflavone from the seeds of Millettia pachycarpa Benth by high-speed counter-current chromatography.
J Chromatogr A. 2008 Jan 18; 1178(1-2):101-7.JC

Abstract

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 160.2 mg tephrosin, 14.6 mg 4',5'-dimethoxy-6,6-dimethylpyranoisoflavone, 109.4 mg deguelin, 6.7 mg 6a,12a-dehydrodeguelin with respective purities of 95, 93, 95, 95%, in one single run from 400 mg 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); (1)H nuclear magnetic resonance ((1)H NMR) and (13)C nuclear magnetic resonance ((13)C 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.

Authors+Show Affiliations

State Key Laboratory of Biotherapy, West China Hospital and College of Chemical Engineering, Sichuan University, Chengdu 610041, China.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

18082754

Citation

Ye, Haoyu, et al. "Preparative Isolation and Purification of Three Rotenoids and One Isoflavone From the Seeds of Millettia Pachycarpa Benth By High-speed Counter-current Chromatography." Journal of Chromatography. A, vol. 1178, no. 1-2, 2008, pp. 101-7.
Ye H, Chen L, Li Y, et al. Preparative isolation and purification of three rotenoids and one isoflavone from the seeds of Millettia pachycarpa Benth by high-speed counter-current chromatography. J Chromatogr A. 2008;1178(1-2):101-7.
Ye, H., Chen, L., Li, Y., Peng, A., Fu, A., Song, H., Tang, M., Luo, H., Luo, Y., Xu, Y., Shi, J., & Wei, Y. (2008). Preparative isolation and purification of three rotenoids and one isoflavone from the seeds of Millettia pachycarpa Benth by high-speed counter-current chromatography. Journal of Chromatography. A, 1178(1-2), 101-7.
Ye H, et al. Preparative Isolation and Purification of Three Rotenoids and One Isoflavone From the Seeds of Millettia Pachycarpa Benth By High-speed Counter-current Chromatography. J Chromatogr A. 2008 Jan 18;1178(1-2):101-7. PubMed PMID: 18082754.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Preparative isolation and purification of three rotenoids and one isoflavone from the seeds of Millettia pachycarpa Benth by high-speed counter-current chromatography. AU - Ye,Haoyu, AU - Chen,Lijuan, AU - Li,Yanfang, AU - Peng,Aihua, AU - Fu,Afu, AU - Song,Hang, AU - Tang,Minghai, AU - Luo,Houding, AU - Luo,Youfu, AU - Xu,Yongbin, AU - Shi,Jianyou, AU - Wei,Yuquan, Y1 - 2007/11/28/ PY - 2007/09/26/received PY - 2007/11/13/revised PY - 2007/11/15/accepted PY - 2007/12/18/pubmed PY - 2008/4/23/medline PY - 2007/12/18/entrez SP - 101 EP - 7 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1178 IS - 1-2 N2 - 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 160.2 mg tephrosin, 14.6 mg 4',5'-dimethoxy-6,6-dimethylpyranoisoflavone, 109.4 mg deguelin, 6.7 mg 6a,12a-dehydrodeguelin with respective purities of 95, 93, 95, 95%, in one single run from 400 mg 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); (1)H nuclear magnetic resonance ((1)H NMR) and (13)C nuclear magnetic resonance ((13)C 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. SN - 0021-9673 UR - https://www.unboundmedicine.com/medline/citation/18082754/Preparative_isolation_and_purification_of_three_rotenoids_and_one_isoflavone_from_the_seeds_of_Millettia_pachycarpa_Benth_by_high_speed_counter_current_chromatography_ DB - PRIME DP - Unbound Medicine ER -