决明子活性成分的高速逆流色谱分离

为了高效分离得到高纯度的决明子活性成分,应用高速逆流色谱,在流速为2.0 mL/min、固定相为正己烷-乙酸乙酯-乙醇-水(体积比5∶3∶6∶6)的上相、流动相为从正己烷-乙酸乙酯-乙醇-水(体积比5∶3∶6∶6)到正己烷-乙酸乙酯-乙醇-水(体积比5∶3∶5∶7)的梯度洗脱的两相溶剂系统中,从决明子的乙酸乙酯萃取物中同时分离得到5种单体化合物.利用理化常数、质谱(MS)、核磁共振(~1HNMR、~(13)CNMR)等波谱技术鉴定出5种化合物分别为橙钝叶决明素(Ⅰ)、甲基钝叶决明素(Ⅱ)、钝叶决明素(Ⅲ)、大黄素甲醚(Ⅳ)和大黄素(Ⅴ).从500 mg粗提物中分离得到5种化合物的量分别为90.42、45.39、31.84、121.71和39.10 mg;纯度分别为97.4%、93.0%、94.8%、96.3%和95.5%;回收率分别为91.5%、96.7%、93.3%、95.6%和98.4%.

Separation of Active Components from Cassia tora L. Using High-Speed Countercurrent Chromatography

In order to effectively separate high-purity active components from Cassia tora L., a high-speed countercurrent chromatography (HSCCC) procedure was performed to separate five monomers from the acetic ether extraction of the plant. The procedure was performed in a two-phase solvent system at a flow rate of 2.0mL/min. The stationary phase is the upper phase of n -hexane-ethyl acetate-ethanol-water (in a volume ratio of 5∶3∶6∶6). The gradient elution of mobile phase is from the lower phase of n -hexane-ethyl acetate-ethanol-water (in a volume ratio of 5∶3∶6∶6) to the lower phase of n -hexane-ethyl acetate-ethanol-water (in a volume ratio of 5∶3∶5∶7). According to the physicochemical properties and the spectral data of MS, ~1HNMR and ~(13)CNMR, the five separated components were identified as aurantio-obtusin (Ⅰ), chryso-obtusin (Ⅱ), obtusin (Ⅲ), physcion (Ⅳ) and emodin (Ⅴ). Moreover, 90.42, 45.39, 31.84, 121.71 and 39.10 mg of the five components were respectively separated from 500 mg of crude extract, with the purities of 97.4%, 93.0%, 94.8%, 96.3% and 95.5% and the recoveries of 91.5%, 96.7%, 93.3%, 95.6% and 98.4%, respectively.