Wang Xiao, Li Fuwei, Sun Qinglei, Yuan Jingpeng, Jiang Ting, Zheng Chengchao
Test Center, Shandong Academy of Sciences, Jinan, Shandong 250014, China.
J Chromatogr A. 2005 Jan 21;1063(1-2):247-51. doi: 10.1016/j.chroma.2004.11.077.
Following an initial clean-up step on the AB-8 resin (polystyrene resin, 0.3-1.25 mm: NanKai Chemical Factory, Tianjin, China), high-speed counter-current chromatography (HSCCC) was used to purify an arctiin from an extract of the fruits of the Arctium lappa L. Arctiin is a major lignan compound in the traditional Chinese medicinal herb A. lappa L. The two-phase solvent system used was composed of ethyl acetate-n-butanol-ethanol-water at an optimized volume ratio of 5:0.5:1:5 (v/v/v/v). The upper phase was used as the mobile phase in the head to tail elution mode. A total amount of 159 mg of arctiin at 98% purity was obtained from 350 mg of the crude extract (containing 49% arctiin) with 91% recovery. The preparative isolation and purification of arctiin by HSCCC was completed in 5 h in a separation. Identification of the target compound was performed by LC-electrospray ionization MS and 13C-NMR. The structure of the product was further confirmed by comparison with authentic sample (National Institute of the Control of Pharmaceutical and Biological Products, Beijing, China).
在对AB - 8树脂(聚苯乙烯树脂,0.3 - 1.25毫米:中国天津南开化工厂)进行初步清理步骤后,采用高速逆流色谱法(HSCCC)从牛蒡果实提取物中纯化牛蒡子苷。牛蒡子苷是传统中药材牛蒡中的主要木脂素类化合物。所使用的两相溶剂系统由乙酸乙酯 - 正丁醇 - 乙醇 - 水组成,优化体积比为5:0.5:1:5(v/v/v/v)。上层相用作流动相,采用头对尾洗脱模式。从350毫克粗提取物(含49%牛蒡子苷)中获得了159毫克纯度为98%的牛蒡子苷,回收率为91%。HSCCC对牛蒡子苷的制备分离和纯化在一次分离中于5小时内完成。通过液相色谱 - 电喷雾电离质谱和13C - NMR对目标化合物进行鉴定。通过与标准品(中国北京国家药品生物制品检定所)比较进一步确认了产物的结构。