Institute of Chinese Material Medical, China Academy of Chinese Medical Sciences, Beijing, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Apr 1;879(11-12):811-4. doi: 10.1016/j.jchromb.2011.02.001.
Following an initial clean-up step on silica gel, high-speed counter-current chromatography (HSCCC) was used to separate cyclic peptides from an extract of the seeds of Vaccaria segetalis. The two-phase solvent system used for HSCCC separation was composed of petroleum ether-ethyl acetate-methanol-water at an optimized volume ratio of 0.5:3.5:1:5. From 190 mg of crude extract, 38.0 mg of segetalin B and 28.5 mg of segetalin A were obtained with purities of 98.1% and 95.6% as determined by HPLC, respectively. The chemical structures of the target compounds were confirmed by high resolution electrospray ionization time of flight MS (HRESI-TOF-MS) and (1)H NMR analyses.
在用硅胶初步清洗后，高速逆流色谱（HSCCC）被用于从菥蓂种子的提取物中分离环肽。用于 HSCCC 分离的两相溶剂系统由石油醚-乙酸乙酯-甲醇-水组成，优化的体积比为 0.5:3.5:1:5。从 190 毫克粗提物中，分别获得了 38.0 毫克的菥蓂素 B 和 28.5 毫克的菥蓂素 A，纯度分别通过 HPLC 测定为 98.1%和 95.6%。目标化合物的化学结构通过高分辨率电喷雾电离飞行时间质谱（HRESI-TOF-MS）和（1）H NMR 分析得到确认。
