Zhu Lijie, Li Bin, Liu Xiuying, Meng Xianjun
College of Food, Shenyang Agricultural University, Shenyang 110866, People's Republic of China.
College of Food, Shenyang Agricultural University, Shenyang 110866, People's Republic of China
J Chromatogr Sci. 2014 Oct;52(9):1082-8. doi: 10.1093/chromsci/bmt168. Epub 2013 Nov 12.
A method for preparative purification of corosolic acid and nigranoic acid from Schisandra chinensis (SC) was established using a combination of macroporous absorption resin column separation and high-speed counter-current chromatography (HSCCC). The crude extracts obtained from SC using 70% ethanol were separated on a macroporous resin column and then eluted with a graded ethanol series. The 70% ethanol fraction was used as the sample for separation of the two triterpenoids by HSCCC. The two-phase solvent system used for HSCCC separation was chloroform-n-butanol-methanol-water (10:0.5:7:4, v/v/v/v). The upper phase was used as the stationary phase of HSCCC. Corosolic acid (16.4 mg) of 96.3% purity and nigranoic acid (9.5 mg) of 98.9% purity were obtained in a one-step HSCCC separation from 100 mg of the sample. The structures of corosolic acid and nigranoic acid were identified by (1)H-nuclear magnetic resonance (NMR) and (13)C-NMR.
建立了一种采用大孔吸附树脂柱分离与高速逆流色谱(HSCCC)相结合的方法,从五味子(SC)中制备纯化科罗索酸和黑蔓藤酸。用70%乙醇从五味子中获得的粗提物在大孔树脂柱上进行分离,然后用梯度乙醇系列洗脱。70%乙醇馏分用作HSCCC分离这两种三萜类化合物的样品。用于HSCCC分离的两相溶剂体系为氯仿-正丁醇-甲醇-水(10:0.5:7:4,v/v/v/v)。上相用作HSCCC的固定相。从100 mg样品中通过一步HSCCC分离得到了纯度为96.3%的科罗索酸(16.4 mg)和纯度为98.9%的黑蔓藤酸(9.5 mg)。通过¹H-核磁共振(NMR)和¹³C-NMR对科罗索酸和黑蔓藤酸的结构进行了鉴定。