Citation: LIU Yongling, CHEN Tao, CHEN Chen, ZOU Denglang, LI Yulin. Isolation and preparation of an imidazole alkaloid from radix of Aconitum pendulum Busch by semi-preparative high-speed counter-current chromatography[J]. Chinese Journal of Chromatography, ;2014, 32(5): 543-546. doi: 10.3724/SP.J.1123.2013.12007 shu

Isolation and preparation of an imidazole alkaloid from radix of Aconitum pendulum Busch by semi-preparative high-speed counter-current chromatography

LIU Yongling ^1,2 ,
CHEN Tao ¹ ,
CHEN Chen ¹ ,
ZOU Denglang ^1,2 ,
LI Yulin ^1,,

1.
1. Northwest Institute of Plateau Biology, Chinese Academy of Sciences, Xining 810008, China;

Corresponding author: LI Yulin,
Received Date: 10 December 2013
Available Online: 23 January 2014
Fund Project: 中国科学院知识创新工程重要方向项目(KSCX2-EW-J-26). (KSCX2-EW-J-26)

Aconitum pendulum Busch is rich C₁₉ diterpenoid alkaloids, but there is no report of imidazole alkaloid in Aconitum pendulum Busch. In this study, an imidazole alkaloid named 1H-imidazole-2-carboxylic acid, butyl ester (ICABE) was successfully separated from Aconitum pendulum Busch with semi-preparative high-speed counter-current chromatography (HSCCC). The partition coefficient was measured by HPLC to select the solvent systems for ICABE separation by HSCCC. The separation was performed with a two-phase solvent system composed of n-hexane-chloroform-ethanol-water (10:1:13:2, v/v/v/v). The upper phase was used as the stationary phase and the lower phase as the mobile phase. It was operated at a flow rate of 1.8 mL/min. The apparatus was rotated at 850 r/min, and the detection wavelength was set at 230 nm. Under the selected conditions, a high efficiency separation of HSCCC was achieved, and 7.5 mg of ICABE was obtained from 100 mg of the crude sample of Aconitum pendulum in one-step separation within 350 min. The HPLC analysis showed that the purity of the compound was over 98%. The chemical structure was confirmed by UV, ¹H-NMR and ¹³C-NMR. The established method is simple, highly efficient and suitable for large scale separation of ICABE from radix of Aconitum pendulum Busch.
- semi-preparation,
- high-speed counter-current chromatography (HSCCC),
- imidazole alkaloid,
- Aconitum pendulum Busch
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