title: Two-dimensional preparative liquid chromatography system for preparative separation of minor amount components from complicated natural products.
abstract: An on-line comprehensive two-dimensional preparative liquid chromatography system was developed for preparative separation of minor amount components from complicated natural products. Medium-pressure liquid chromatograph (MPLC) was applied as the first dimension and preparative HPLC as the second one, in conjunction with trapping column and makeup pump. The performance of the trapping column was evaluated, in terms of column size, dilution ratio and diameter-height ratio, as well as system pressure from the view of medium pressure liquid chromatograph. Satisfactory trapping efficiency can be achieved using a commercially available 15 mm × 30 mm i.d. ODS pre-column. The instrument operation and the performance of this MPLC×preparative HPLC system were illustrated by gram-scale isolation of crude macro-porous resin enriched water extract of Rheum hotaoense. Automated multi-step preparative separation of 25 compounds, whose structures were identified by MS, (1)H NMR and even by less-sensitive (13)C NMR, could be achieved in a short period of time using this system, exhibiting great advantages in analytical efficiency and sample treatment capacity compared with conventional methods.
authors.affiliation: School of Pharmaceutical Sciences and the Key Laboratory for Chemical Biology of Fujian Province, Xiamen University, South Xiang-An Road, Xiamen, 361100, China. Electronic address: qyk@xmu.edu.cn.
authors.forename: Ying-Kun
authors.initials: YK
authors.lastname: Qiu
authors.affiliation: School of Pharmaceutical Sciences and the Key Laboratory for Chemical Biology of Fujian Province, Xiamen University, South Xiang-An Road, Xiamen, 361100, China.
authors.forename: Fang-Fang
authors.initials: FF
authors.lastname: Chen
authors.affiliation: School of Pharmaceutical Sciences and the Key Laboratory for Chemical Biology of Fujian Province, Xiamen University, South Xiang-An Road, Xiamen, 361100, China.
authors.forename: Ling-Ling
authors.initials: LL
authors.lastname: Zhang
authors.affiliation: School of Pharmaceutical Sciences and the Key Laboratory for Chemical Biology of Fujian Province, Xiamen University, South Xiang-An Road, Xiamen, 361100, China.
authors.forename: Xia
authors.initials: X
authors.lastname: Yan
authors.affiliation: School of Pharmaceutical Sciences and the Key Laboratory for Chemical Biology of Fujian Province, Xiamen University, South Xiang-An Road, Xiamen, 361100, China.
authors.forename: Lin
authors.initials: L
authors.lastname: Chen
authors.affiliation: School of Pharmaceutical Sciences and the Key Laboratory for Chemical Biology of Fujian Province, Xiamen University, South Xiang-An Road, Xiamen, 361100, China.
authors.forename: Mei-Juan
authors.initials: MJ
authors.lastname: Fang
authors.affiliation: School of Pharmaceutical Sciences and the Key Laboratory for Chemical Biology of Fujian Province, Xiamen University, South Xiang-An Road, Xiamen, 361100, China. Electronic address: wuzhen@xmu.edu.cn.
authors.forename: Zhen
authors.initials: Z
authors.lastname: Wu
mesh_terms: D001688:Biological Products / Q000302:isolation & purification*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D056148:Chromatography, Reverse-Phase; D011312:Pressure; D013997:Time Factors; D014867:Water / Q000737:chemistry
chemical_list: D001688:Biological Products; D014867:Water
keywords: Anthraquinones; Medium-pressure liquid chromatograph×preparative high-performance liquid chromatography; Rheum hotaoense L; Rheumin; Stilbenes; Two-dimensional preparative liquid chromatography