Preparative separation of alkaloids from Gelsemium elegans Benth. using pH-zone-refining counter-current chromatography

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• 作者：Yan-Ping Su^a ; ^b ; Jie Shen^a ; Ying Xu^a ; Mi Zheng^a ; Chang-Xi Yu^a ; ^{changxiyu@mail.fjmu.edu.cn"" rel=""nofollow}
• 关键词：Gelsemium elegans ; pH-zone-refining counter-current chromatography ; Alkaloids ; Gelsemine ; Koumine ; Gelsevirine
• 刊名：Journal of Chromatography A
• 出版年：2011
• 出版时间：10 June 2011
• 年：2011
• 卷：1218
• 期：23
• 页码：3695-3698
• 全文大小：361 K

文摘

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.