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

doi:10.3724/SP.J.1123.2017.01010

色谱 ›› 2017, Vol. 35 ›› Issue (6): 650-655.DOI: 10.3724/SP.J.1123.2017.01010

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

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

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

收稿日期:2017-01-11 出版日期:2017-06-08 发布日期:2013-09-29
通讯作者: 金郁,Tel:(021)64250633,E-mail:jiny@ecust.edu.cn.
基金资助:
国家自然科学基金项目（81403100）.

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

JIA Youmei¹, CAI Jianfeng¹, XIN Huaxia¹, FENG Jiatao², FU Yanhui³, FU Qing¹, JIN Yu¹

1. School of Pharmacy, East China University of Science and Technology, Shanghai 200237, China;
2. Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China;
3. College of Chemistry and Chemical Engineering, Hainan Normal University, Haikou 571158, China

Received:2017-01-11 Online:2017-06-08 Published:2013-09-29
Supported by:
National Natural Science Foundation of China (No. 81403100).

摘要/Abstract

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，10 μm）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，5 μm）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。

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

Abstract:

A preparative two dimensional hydrophilic interaction liquid chromatography/reversed-phase liquid chromatography (Pre-2D-HILIC/RPLC) method was established to separate and purify the components in Trachelospermum jasminoides. 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 (250 mm×20 mm, 10 μm) was selected as stationary phase and water-acetonitrile as mobile phases in the first dimensional HILIC. Finally, 15 fractions were collected under UV-triggered mode. In the second dimensional RPLC, a C18 column (250 mm×20 mm, 5 μm) was selected and water-acetonitrile was used as mobile phases. As a result, 14 compounds with high purity were obtained, which were further identified by mass spectrometry (MS) and nuclear magnetic resonance (NMR). Finally, 11 lignan 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 jasminoides.

Key words: Trachelospermum jasminoides, hydrophilic interaction liquid chromatography (HILIC), reversed-phase liquid chromatography (RPLC), separation and purification, two dimensional (2D) chromatography

中图分类号:

O658

贾有梅, 蔡剑锋, 辛华夏, 丰加涛, 付艳辉, 傅青, 金郁. 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[J]. 色谱, 2017, 35(6): 650-655.

JIA Youmei, CAI Jianfeng, XIN Huaxia, FENG Jiatao, FU Yanhui, FU Qing, JIN Yu. Separation and purification of the components in Trachelospermum jasminoides by two dimensional hydrophilic interaction liquid chromatography- reversed-phase liquid chromatography[J]. Chinese Journal of Chromatography, 2017, 35(6): 650-655.

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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

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

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