Liaoning Institute of Science and Technology, Benxi 117004, China.
Shandong Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Qilu University of Technology (Shandong Academy of Sciences), Jinan 250014, China.
Molecules. 2018 Dec 18;23(12):3353. doi: 10.3390/molecules23123353.
Three phenylethanoid glycosides, echinacoside (), salidroside (), and acteoside (), and three secoiridoid glycosides, isonuezhenide (), nuezhenoside G13 (), and specnuezhenide (), have been extracted and separated by a combined method of ultrahigh pressure extraction (UPE) and high-speed counter-current chromatography (HSCCC) from Ligustri Lucidi Fructus. For the UPE, the optimal extraction was developed with conditions including solvent of 90% ethanol, sample to solvent ratio of 1:20 g/mL, pressure of 200 MPa, and time of 2 min, which rendered the yields of compounds and were 15.0 and 78.0 mg/g, respectively. For the HSCCC separation, the strategy of changing flow rates between 1.0 and 2.0 mL/min allowed the acquisition for 2.7 mg of compound , 4.5 mg of compound , 6.8 mg of compound , 5.9 mg of compound , 11.2 mg of compound , and 2.2 mg of compound in one separation run under the solvent system of ethyl acetate:-butanol:water (2:1:3, /) from 200 mg of the UPE extract. The structures of these phenylethanoid and secoiridoid glycosides were elucidated by extensive spectroscopic methods.
从女贞子中提取并分离出三种苯乙醇苷，即毛蕊花糖苷（）、红景天苷（）和麦角甾苷（），以及三种裂环环烯醚萜苷，即异獐牙菜苷（）、女贞苷 G13（）和新女贞苷（），采用超高压提取（UPE）和高速逆流色谱（HSCCC）相结合的方法。对于 UPE，最佳提取条件为溶剂为 90%乙醇，料液比为 1:20 g/mL，压力为 200 MPa，时间为 2 min，化合物和的收率分别为 15.0 和 78.0 mg/g。对于 HSCCC 分离，通过改变流速在 1.0 和 2.0 mL/min 之间的策略，在溶剂系统为乙酸乙酯：-正丁醇：水（2:1:3，/）下，从 200 mg UPE 提取物中，一次分离运行可获得 2.7 mg 化合物、4.5 mg 化合物、6.8 mg 化合物、5.9 mg 化合物、11.2 mg 化合物和 2.2 mg 化合物。这些苯乙醇苷和裂环环烯醚萜苷的结构通过广泛的光谱方法阐明。
