决明子活性成分的高速逆流色谱分离

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

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2.0mL/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(1HNMR1、3CNMR)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%.

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 ^13CNMR, 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 500mg 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.