利用高速逆流色谱法从金钱松根皮中制备分离出伪土荆皮酸A和B及其糖苷。

Preparative isolation of pseudolaric acids A and B, and their glucosides from the root bark of Pseudolarix kaempferi using high-speed counter-current chromatography.

作者信息

Han Quan-Bin, Wong Lina, Lai Fanny, Yang Nian-Yun, Song Jing-Zheng, Qiao Chun-Feng, Xu Hong-Xi

机构信息

Chinese Medicine Laboratory, Hong Kong Jockey Club Institute of Chinese Medicine, ShaTin N. T., Hong Kong, China.

出版信息

J Sep Sci. 2009 Jan;32(2):309-13. doi: 10.1002/jssc.200800547.

DOI:10.1002/jssc.200800547

PMID:19072902

Abstract

In order to provide the chemical markers for the quality control of herbal medicines, four diterpenoids, pseudolaric acids A and B (PAA and PAB), and their glucosides were isolated from the methanol extract of the Chinese herb Pseudolarix kaempferi using high-speed counter-current chromatography (HSCCC). The diphase solvent system was n-hexane/EtOAc/MeOH/H(2)O which was used at two ratios (5:5:5:5 and 1:9:4:6 by volume) in the separation of pseudolaric acids and their glycosides, respectively. As a result, PAA (14 mg), PAB (129 mg), PAA-O-beta-D-glucopyranoside (8 mg, PAAG), and PAB-O-beta-D-glucopyranoside (42 mg, PABG) were obtained from 0.5 g of the crude extract. Their purities were determined to be above 97% by HPLC analysis. Their chemical structures were confirmed by( 1)H and( 13)C NMR analysis or HPLC comparison with the reference compounds.

摘要

为了提供中药材质量控制的化学标志物，采用高速逆流色谱法（HSCCC）从中国草药金钱松的甲醇提取物中分离出四种二萜类化合物，即土荆酸A和B（PAA和PAB）及其糖苷。双相溶剂体系为正己烷/乙酸乙酯/甲醇/水，分别以两种比例（体积比5:5:5:5和1:9:4:6）用于分离土荆酸及其糖苷。结果，从0.5 g粗提取物中获得了PAA（14 mg）、PAB（129 mg）、PAA-O-β-D-吡喃葡萄糖苷（8 mg，PAAG）和PAB-O-β-D-吡喃葡萄糖苷（42 mg，PABG）。通过HPLC分析确定它们的纯度高于97%。通过¹H和¹³C NMR分析或与参考化合物的HPLC比较确认了它们的化学结构。