利用高速逆流色谱法从玉米须中制备分离异鼠李素
PREPARATIVE ISOLATION OF ISORHAMNETIN FROM STIGMA MAYDIS USING HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY.
作者信息
Cao Xiaoying, Wei Yun, Ito Yoichiro
机构信息
Applied Chemistry Department, Faculty of Sciences, Beijing University of Chemical Technology, 15 Beisanhuan East Road, Chaoyang District, Beijing 100029, China.
出版信息
J Liq Chromatogr Relat Technol. 2009 Jan 1;32(2):273-280. doi: 10.1080/10826070802603369.
Abstract
Preparative high-speed countercurrent chromatography (HSCCC) has been successfully used for the isolation and purification of isorhamnetin from Stigma maydis. This was achieved in two stages: the first separation was performed with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (HEMW) at a volume ratio of 5:5:5:5, yielding isorhamnetinat 65.6 %, which is followed by the second run using a two-phase solvent system composed of HEMW 5:5:6:4, v/v. From 700 mg of the crude extract 11.8 mg of isorhamnetin was obtained at a high purity of 98%. The final identification was performed by MS, (1)H-NMR and (13)C-NMR spectra.
摘要
制备型高速逆流色谱法（HSCCC）已成功用于从玉米须中分离纯化异鼠李素。这一过程分两个阶段完成：第一次分离采用正己烷 - 乙酸乙酯 - 甲醇 - 水（HEMW）体积比为5:5:5:5的两相溶剂系统，异鼠李素得率为65.6%，随后进行第二次分离，采用体积比为5:5:6:4（v/v）的HEMW两相溶剂系统。从700毫克粗提物中获得了11.8毫克高纯度（98%）的异鼠李素。最终通过质谱、氢核磁共振谱（¹H-NMR）和碳核磁共振谱（¹³C-NMR）进行鉴定。
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