title: Preparative separation of alkaloids from Gelsemium elegans Benth. using pH-zone-refining counter-current chromatography.
abstract: Alkaloids in Gelsemium elegans possess a variety of therapeutic properties, including tumor suppression, analgesic and anti-inflammatory effects. In China, G. elegans has been used for centuries to treat a variety of medical conditions, including chronic pain and skin ulcer. Methods currently used to separate the active components of G. elegans are time-consuming and have low recovery. In the present study, we used pH-zone-refining counter-current chromatography to separate major alkaloids from a crude extract of G. elegans. The two-phase solvent system was methyl tert-butyl ether (MtBE)/acetonitrile/water (3:1.5:4, v/v). Triethylamine (20 mM) was added to the upper organic stationary phase as a retainer. Hydrochloric acid (10 mM) was added to the lower aqueous phase as an eluter. From 1.5 g of crude extract, we obtained 312 mg gelsemine, 420 mg koumine and 195 mg gelsevirine, with purities at 94.8%, 95.9% and 96.7%, respectively, which were determined by HPLC at 256 nm. The chemical identity of the isolated compounds was verified by electrospray ionization-mass spectrometry (ESI-MS), ¹H NMR and ¹³C NMR. These results demonstrated that pH-zone-refining counter-current chromatography is an effective method to separate and purify major alkaloids from G. elegans.
authors.affiliation: Department of Pharmacology, College of Pharmacy, Fujian Medical University, Fuzhou 350004, Fujian, China.
authors.forename: Yan-Ping
authors.initials: YP
authors.lastname: Su
authors.forename: Jie
authors.initials: J
authors.lastname: Shen
authors.forename: Ying
authors.initials: Y
authors.lastname: Xu
authors.forename: Mi
authors.initials: M
authors.lastname: Zheng
authors.forename: Chang-Xi
authors.initials: CX
authors.lastname: Yu
mesh_terms: D000470:Alkaloids / Q000032:analysis / Q000302:isolation & purification*; D003377:Countercurrent Distribution / Q000379:methods*; D004365:Drugs, Chinese Herbal / Q000737:chemistry*; D031450:Gelsemium / Q000737:chemistry*; D006863:Hydrogen-Ion Concentration; D026121:Indole Alkaloids / Q000032:analysis / Q000302:isolation & purification*
chemical_list: D000470:Alkaloids; D004365:Drugs, Chinese Herbal; D026121:Indole Alkaloids; C515085:koumine; C063230:gelsemine