高速逆流色谱法从中药射干中制备分离和纯化黄酮类化合物
Preparative isolation and purification of flavonoids from the Chinese medicinal herb Belamcanda by high-speed countercurrent chromatography.
作者信息
Peng Cuilin, Liang Yong, Wang Xiaohong, Xie Huichun, Zhang Tianyou, Ito Yoichiro
机构信息
Institute of Analytical Chemistry, School of Chemistry and Environment, South China Normal University, Guangzhou, 510006.China.
出版信息
J Liq Chromatogr Relat Technol. 2009 Jan 1;32(16):2451-2461. doi: 10.1080/10826070903188245.
High-speed countercurrent chromatography (HSCCC) was applied for separation and purification of flavonoids from the extract of belamcanda. High efficiency of HSCCC separation was achieved on a two-phase solvent system of n-hexane-ethyl acetate-methanol-water (4:5:5:5, v/v) by eluting the lower mobile phase at a flow-rate of 1.2mL/min and a revolution speed of 800 rpm. Three well-separated peaks were obtained in the HSCCC chromatogram and their purities were determined by HPLC-UV absorption spectrometry. These peaks were characterized by ESI-MS(n) and NMR, and the data compared with the reference standards where three peaks were identified as isorhamnetin, irigenin and hispidulin. The purities of each peak were 94, 95 and 90% respectively. In HSCCC experiment, 100 mg of the crude extract were separated yielding 10 mg of isorhamnetin, 8 mg of irigenin and 7 mg of hispidulin. HSCCC thus provides a cost-effective alternative to preparative scale HPLC for the semi-preparative scale separation and purification of flavonoids from Belamcanda.
采用高速逆流色谱法（HSCCC）从射干提取物中分离纯化黄酮类化合物。在正己烷 - 乙酸乙酯 - 甲醇 - 水（4:5:5:5，v/v）的两相溶剂体系中，以1.2mL/min的流速洗脱下层流动相，转速为800 rpm，实现了HSCCC的高效分离。在HSCCC色谱图中获得了三个分离良好的峰，并通过HPLC - UV吸收光谱法测定了它们的纯度。通过电喷雾电离质谱（ESI - MS(n)）和核磁共振（NMR）对这些峰进行了表征，并将数据与参考标准进行比较，其中三个峰分别鉴定为异鼠李素、鸢尾黄素和木犀草素。每个峰的纯度分别为94%、95%和90%。在HSCCC实验中，100 mg粗提取物被分离，得到10 mg异鼠李素、8 mg鸢尾黄素和7 mg木犀草素。因此，对于从射干中进行半制备规模的黄酮类化合物分离纯化，HSCCC为制备规模的HPLC提供了一种经济高效的替代方法。
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