采用中压液相色谱（MPLC）、高速逆流色谱（HSCCC）和制备型高效液相色谱（Prep-HPLC）对射干化学成分进行制备分离与纯化
PREPARATIVE ISOLATION AND PURIFICATION OF CHEMICAL CONSTITUENTS OF BELAMCANDA BY MPLC, HSCCC AND PREP-HPLC.
作者信息
Wang Xiaohong, Liang Yong, Peng Cuilin, Xie Huichun, Pan Man, 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. 2011;34(4):241-257. doi: 10.1080/10826076.2011.547058.
Combined with medium-pressure liquid chromatography (MPLC) and preparative high-pressure liquid chromatography (Prep-HPLC), high-speed countercurrent chromatography (HSCCC) was successfully applied for separation and purification of isoflavonoids from the extract of belamcanda. HSCCC separation was performed on a two-phase solvent system composed of methyl tert-butyl ether -ethyl acetate - n-butyl alcohol - acetonitrile -0.1% aqueous trifluoroacetic acid at a volume radio of 1:2:1:1:5. Semi-purified peak fractions from HSCCC separation were further purified by Prep-HPLC. Nine well-separated fractions were analyzed by HPLC-UV absorption spectrometry to determine their purities and characterized with ESI-MS(n). Except for peaksland VII (unknown) seven compounds were identified as apocynin (peak II), mangiferin (peak III), 7-O-methylmangiferin (peak IV), hispidulin (peak V), 3'-hydroxyltectoridin (peak VI), iristectorin B (peak VII), isoiridin (peak IX).
高速逆流色谱（HSCCC）与中压液相色谱（MPLC）和制备型高压液相色谱（Prep-HPLC）相结合，成功应用于射干提取物中异黄酮类化合物的分离与纯化。HSCCC分离在由甲基叔丁基醚 - 乙酸乙酯 - 正丁醇 - 乙腈 - 0.1% 三氟乙酸水溶液组成的两相溶剂体系中进行，体积比为1:2:1:1:5。HSCCC分离得到的半纯化峰馏分通过Prep-HPLC进一步纯化。通过HPLC-UV吸收光谱法分析九个分离良好的馏分以确定其纯度，并采用电喷雾电离质谱（ESI-MS(n)）进行表征。除峰I和VII（未知）外，七种化合物被鉴定为穿心莲内酯（峰II）、芒果苷（峰III）、7-O-甲基芒果苷（峰IV）、滨蓟黄素（峰V）、3'-羟基鸢尾苷（峰VI）、鸢尾黄酮B（峰VII）、异鸢尾苷（峰IX）。
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