色谱Issue(1):84-89,6.DOI:10.3724/SP.J.1123.2014.09033
循环制备液相色谱分离芳香新塔花中的化学成分
Isolation of chemical constituents from Ziziphora clinopodioides Lam. with recycling preparative high performance liquid chromatography
摘要
Abstract
The combination of alternate recycling and direct recycling preparative liquid chro-matography method was developed for the isolation of chemical constituents from Ziziphora clinopodioides Lam. The crude extract was obtained from Ziziphora clinopodioides Lam. by solvent extraction,column chromatography and reversed-phase( RP ) flash chromatography. All the separations were performed with methanol and water as mobile phases and the devel-oped recycling preparative method was used with twin RP columns switched by a two-position ten-way valve for the separation. The mobile phase was recycled in close loop with a two-posi-tion six-way valve. The fraction Ⅰ and fraction Ⅱ from reversed-phase flash chromatography were selected for the demonstration of separation power of the proposed protocol,and five compounds were obtained from Ziziphora clinopodioides Lam. The isolated five compounds were identified as pinocembrin-7-O-rutinoside,pinocembrin-7-O-rutinoside,acacetin-7-O-ruti-noside,picein and protocatechuic acid with nuclear magnetic resonance( NMR). The experi-mental results showed that the developed preparation method exhibited higher separation effi-ciency with less mobile phase used than the reported methods,and could be expected as an effective method for the separation of complex natural products,especially the compounds with similar structures.关键词
交替循环/直接循环/制备色谱/化学成分/芳香新塔花Key words
alternate recycling/direct recycling/preparative liquid chromatography/chemical constituents/Ziziphora clinopodioides Lam分类
化学化工引用本文复制引用
李国柱,孟庆艳,罗碧,葛振红,刘文杰..循环制备液相色谱分离芳香新塔花中的化学成分[J].色谱,2015,(1):84-89,6.基金项目
国家自然科学基金项目(21365018);新疆生产建设兵团科技攻关项目(2011AB030);新疆生产建设兵团塔里木盆地生物资源保护利用重点实验室开放课题( BRYB1404). ()