title: [Preparative isolation and purification of scopoletin from Lycium barbarum L. by high-speed countercurrent chromatography].
abstract: An effective and rapid method for the separation of scopoletin from Lycium barbarum L. by high-speed counter-current chromatography (HSCCC) was established. The ethyl alcohol extract of the Lycium barbarum L. was initially separated using D-101 macroporous resins and further purified by HSCCC. The thin layer chromatography coupling with fluorometric spectrophotometry (TLC-F) method was used to determine the partitioning coefficient of scopoletin in different solvent systems. The results showed the solvent system of chloroformmethanol-water (10:7:3, v/v/v) was the best one for the HSCCC separation. A total of 10.2 mg of scopoletin with high purity (98. 3%, analyzed by high performance liquid chromatography (HPLC)) was obtained in one step by the following separation procedures: the upper phase as the stationary phase, the lower phase as the mobile phase, with a flow rate of 1.5 mL/min, with the apparatus rotated at 850 r/min, and detected at 365 nm. The structure of the obtained compound was identified by 'H-nuclear magnetic resonance and 13C-nuclear magnetic resonance. The sample could be injected into HSCCC twice successively and the whole separation was achieved with satisfactory peak resolution. These results suggested that the TLC-F method is useful in measuring the partitioning coefficients of the target compound in HSCCC solvent systems and HSCCC is a fast and convenient method for the separation of scopoletin.
authors.affiliation: College of Life Science, Southwest University, Chongqing 400715, China.
authors.forename: Xiaoduo
authors.initials: X
authors.lastname: Li
authors.forename: Xuegang
authors.initials: X
authors.lastname: Li
authors.forename: Shanghua
authors.initials: S
authors.lastname: Song
authors.forename: Bo
authors.initials: B
authors.lastname: Zhang
authors.forename: Xujing
authors.initials: X
authors.lastname: Liu
authors.forename: Xiaoli
authors.initials: X
authors.lastname: Ye
mesh_terms: D002855:Chromatography, Thin Layer / Q000379:methods; D003377:Countercurrent Distribution / Q000379:methods*; D032305:Lycium / Q000737:chemistry*; D012603:Scopoletin / Q000302:isolation & purification*; D012997:Solvents / Q000737:chemistry; D013050:Spectrometry, Fluorescence / Q000379:methods
chemical_list: D012997:Solvents; D012603:Scopoletin