Wei Yun, Zhang Kai, Zhang Guoliang, Ito Yoichiro
State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, 15 Beisanhuan East Road, Chaoyang District, Beijing 100029, P. R. China.
J Liq Chromatogr Relat Technol. 2011 Dec 1;34(20):2505-2515. doi: 10.1080/10826076.2011.591030.
Semi-preparative high-speed counter-current chromatography (HSCCC) was successfully performed for isolation and purification of caffeic acid 4 bioactive flavonoids from Eupatorium adenophorum Spreng using stepwise elution with a pair of two-phase solvent systems composed of ethyl acetate-methanol-water at the volume ratios of 10: 1: 10 and 5: 1: 5 (v/v). From 378.5 mg of crude extract 24.1 mg of caffeic acid, 6.7 mg of 4'-methyl quercetagetin 7-O-(6"-O-E-caffeoylglucopyranoside), 6.5 mg of quercetagetin 7-O-(6"-O-acetyl-β-D-glucopyranoside), 31.8 mg of eupalitin 3-O-β-D-galactopyranoside and 36.7 mg of eupalitin were obtained with the purities of 96.0%, 91.2%, 82.3%, 95.1% and 85.6%, respectively. The structures of the separated compounds were identified by EI-MS, (1)HNMR and (13)CNMR.
采用由体积比为10:1:10和5:1:5（v/v）的乙酸乙酯 - 甲醇 - 水组成的两相溶剂系统进行梯度洗脱，成功地运用半制备型高速逆流色谱（HSCCC）从紫茎泽兰中分离纯化了4种生物活性黄酮类化合物。从378.5 mg粗提物中分别获得了24.1 mg咖啡酸、6.7 mg 4'-甲基槲皮万寿菊素7 - O -（6"-O - E - 咖啡酰吡喃葡萄糖苷）、6.5 mg槲皮万寿菊素7 - O -（6"-O - 乙酰基 - β - D - 吡喃葡萄糖苷）、31.8 mg泽兰素3 - O - β - D - 吡喃半乳糖苷和36.7 mg泽兰素，纯度分别为96.0%、91.2%、82.3%、95.1%和85.6%。通过电子轰击质谱（EI-MS）、氢核磁共振（¹H NMR）和碳核磁共振（¹³C NMR）对分离得到的化合物结构进行了鉴定。
