文献类型：期刊文献

中文题名：亲水/反相二维制备液相色谱法分离纯化络石藤中的化学成分

英文题名：Separation and purification of the components in Trachelospermum jasminoides by two dimensional hydrophilic interaction liquid chromatography-reversed-phase liquid chromatography

作者：贾有梅[1];蔡剑锋[1];辛华夏[1];丰加涛[2];付艳辉[3];傅青[1];金郁[1]

机构：[1]华东理工大学药学院,上海200237;[2]中国科学院大连化学物理研究所,辽宁大连116023;[3]海南师范大学化学与化工学院,海南海口571158

年份：2017

卷号：35

期号：6

起止页码：650

中文期刊名：色谱

外文期刊名：Chinese Journal of Chromatography

收录：CSTPCD;;Scopus;WOS:【ESCI(收录号:WOS:000411255400013)】；北大核心:【北大核心2014】；CSCD:【CSCD2017_2018】；PubMed;

基金：National Natural Science Foundation of China (No. 81403100).

语种：中文

中文关键词：二维色谱法;亲水作用液相色谱法;反相液相色谱法;分离纯化;络石藤

外文关键词：two dimensional (2D ) chromatography; hydrophilic interaction liquid chromatography(HILIC) ; reversed-phase liquid chromatography (RPLC) ; separation and purification ;Trachelospermum jasminoides

摘要：建立了亲水/反相二维制备液相色谱(Pre-2D-HILIC/RPLC)分离纯化络石藤中化学成分的分析方法。络石藤药材经醇提、活性炭脱色后用反相固相萃取柱除去色素和强极性物质,最终得到干燥的浅黄色粉末。一维亲水色谱选择Click XIon色谱柱(250 mm×20 mm,10μm)作为固定相,水和乙腈作为流动相,进行梯度洗脱,以紫外触发模式收集馏分,共得到15个组分。二维反相色谱选择C18色谱柱(250 mm×20 mm,5μm)作为固定相,水和乙腈作为流动相,进行梯度洗脱,最终得到14个高纯度化合物,并通过质谱和核磁共振对其进行确认。实验结果表明,该法具有良好的正交选择性,可以有效提高分离度和峰容量,对于分离络石藤等复杂样品具有重要意义。
A preparative two dimensional hydrophilic interaction liquid chromatography/reversed-phase liquid chromatography(Pre-2D-HILI^^RPLC)method was established to separate and purify the components in Trachelospermum jasm inoides.The pigments and strongly polar components were removed from the crude extract after the active carbon decolorization and solid phase extraction processes.A Click XIon column(250mm x20mm,10pm)was selected as stationary phase and water-acetonitrile as mobile phases in the first dimensional HILIC.Finally,15fractions were collected under UV-triggered mode.In the second dimensional RPLC,a C18column(250mmx20mm,5pm)was selected and water-acetonitrile was used as mobile phases.As a result,14compounds with high purity were obtained,which were further identified by mass spectrometry(MS)and nuclear magnetic resonance(NMR).Finally,11lignan compounds and three flavonoid compounds were obtained.The method has a good orthogonality,and can improve the resolution and the peak capacity.It is significant for the separation of complex components from Trachelospermum jasm inoides.