应用高速逆流色谱对决明子活性成分的分离

为了高效率地分离决明子中的高纯度活性成分，应用高速逆流色谱法从决明子的乙酸乙酯萃取物中同时分离得到5个单体化合物。两相溶剂系统的固定相为正己烷–乙酸乙酯–乙醇–水（体积比5:3:6:6）的上相，流动相是从正己烷–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，流速为2.0 mL/min。利用理化常数、质谱（MS）、核磁共振（1H–NMR、13C–NMR）等波谱技术鉴定5个化合物分别为橙钝叶决明素（1）、甲基钝叶决明素（2）、钝叶决明素（3）、大黄素甲醚（4）和大黄素（5）。从500mg粗提物中分得的量分别是90.42mg、45.39mg 、31.84mg、121.71 mg和39.10mg， 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 Active Components from Cassia tora L. Using High-Speed Counter-Current Chromatography

In order to simultaneously separate high purity active components from Cassia tora L. in high efficiency，a high-speed counter-current chromatography (HSCCC) procedure was developed for the preparative separation of five monomers from the acetic ether extration of the plant in a simultaneous process. The stationary phase of the two-phase solvent system is the upper phase of n-hexane–ethyl acetate–ethanol–water (volume ratio is 5:3:6:6). The gradient elution of mobile phase is from the lower phase of n-hexane–ethyl acetate–ethanol–water (volume ratio is 5:3:6:6) to the lower phase of n-hexane–ethyl acetate–ethanol–water (volume ratio is 5:3:5:7).The preparative HSCCC was successfully performed with a flow-rate of 2.0 mL/min. The five separated compounds were identified as aurantio-obtustin, chryso-obtustin, obtusin, physcion and edomin. They were quantified by the determinations of their physicochemical properties and spectral data of MS, 1HNMR, 13CNMR. 90.42 mg, 45.39 mg, 31.84 mg, 121.71 mg and 39.10mg of the five compounds could be prepared respectively from 500mg of crude extract by the one-step procedure. Their purities were 97.4%、93.0%、94.8%、96.3% and 95.5% with a recovery of 91.5%、96.7%、93.3%、95.6 and 98.4%, respectively.