中国现代中药2016，Vol.18Issue(5)：554-557,578,5.DOI:10.13313/j.issn.1673-4890.2016.5.003
pH 区带逆流色谱结合制备液相分离制备大黄根化学成分
Separation and Purification of Anthraquinones from Root of Rheum palmatum L.by pH-Zone-refining Counter-current Chromatography and Preparative HPLC
摘要
Abstract
Objective:To separate and purify the compounds from the root of Rheum palmatum L.by pH-zone-refining counter-current chromatography and preparative HPLC.Methods:The solvent system used in this separation was petroleum-ether-ethyl acetate-methanol-water (1∶1∶1∶1).10 mmol·L -1 TFA was added to the upper phase as stationary phase and 20 mmol·L -1 NaOH was added to the lower phase as mobile phase.The revolution speed is 850 r·min -1 and the flow rate is 2 mL·min -1.The effluent was continuously monitored by a UV monitor at 254 nm.The make-up fluid was further separated by preparative HPLC.Results:From 750 mg extract of Rh.palmatum L.root,85.8 mg cinnamic acid (2)and three anthraquinones 34.9 mg rhein (1),52.5 mg aloe-emodin (3)and 50.4 mg emodin (4)were obtained in a single run.And 215.4 mg of chrysophanol and 26.8 mg of physcion were obtained by the preparative HPLC.The purities of these compounds are 95.46%,97.28%,94.75%,95.02%,98.84% and 98.12% analyzed by HPLC.Conclusion:The compounds of Rh.palmatum L.root as weakly acidic compounds could be separated by pH-zone-refining counter-current chromatography.When combined with the preparative HPLC,an efficient method has been established for the separation of these compounds.关键词
pH 区带逆流色谱/制备液相/大黄/化学成分Key words
pH-Zone-refining counter-current chromatography/preparative HPLC/Rheum palmatum L./compounds引用本文复制引用
孙常磊,王召平,孙兆林,耿岩玲,李佳,杨鹏..pH 区带逆流色谱结合制备液相分离制备大黄根化学成分[J].中国现代中药,2016,18(5):554-557,578,5.基金项目
［基金项目］山东省科技发展计划项目 （）
