【摘要】 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%.更多还原

【Abstract】 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 39.10mg 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.更多还原