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高速逆流色谱法从紫茎泽兰中分离咖啡酸及咖啡酸插层水滑石的合成

ISOLATION OF CAFFEIC ACID FROM EUPATORIUM ADENOPHORUM SPRENG BY HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY AND SYNTHESIS OF CAFFEIC ACID-INTERCALATED LAYERED DOUBLE HYDROXIDE.

作者信息

Wei Yun, Gao Yali, Zhang Kai, Ito Yoichiro

机构信息

State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, 15 Beisanhuan East Road, Chaoyang District, Beijing 100029, China.

出版信息

J Liq Chromatogr Relat Technol. 2010 Jan 1;33(6):837-845. doi: 10.1080/10826071003684471.

Abstract

Preparative high-speed countercurrent chromatography (HSCCC) was successfully used for isolation and purification of caffeic acid from Eupatorium adenophorum Spreng with a solvent system composed of ethyl acetate-methanol-water at a volume ratio of 10:1:10, v/v. Using a preparative unit of the HSCCC centrifuge, about a 938 mg amount of the crude extract was separated, yielding 63.2 mg of caffeic acid at purity of 96.0%. Then, the anti-microbial and anti-virus drug caffeic acid (C(9)H(8)O(4)) was intercalated into layered double hydroxides for the first time by anion exchange under a nitrogen atmosphere. The product caffeic acid-LDH has been characterized by powder X-ray diffraction (XRD), Fourier transform-infrared (FT-IR), Scanning electron micrographs (SEM), indicating that the drug has been successfully intercalated into LDH.

摘要

制备型高速逆流色谱(HSCCC)成功用于从紫茎泽兰中分离纯化咖啡酸,所用溶剂系统为体积比10:1:10(v/v)的乙酸乙酯 - 甲醇 - 水。使用HSCCC离心机的制备单元,分离出约938 mg粗提取物,得到纯度为96.0%的咖啡酸63.2 mg。然后,首次在氮气气氛下通过阴离子交换将抗菌抗病毒药物咖啡酸(C(9)H(8)O(4))插入层状双氢氧化物中。产物咖啡酸 - LDH已通过粉末X射线衍射(XRD)、傅里叶变换红外光谱(FT - IR)、扫描电子显微镜(SEM)进行表征,表明该药物已成功插入LDH中。

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