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Hydrophilic interaction chromatographic stationary phase based on amide functional imidazole ionic liquid and preparation method and application of hydrophilic interaction chromatographic stationary phase

A technology of imidazole ionic liquid and chromatographic stationary phase, which is applied in separation methods, chemical instruments and methods, solid adsorbent liquid separation, etc., can solve the problems of insufficient coverage of polar compounds, insufficient hydrophilicity, low column efficiency, etc., and achieve Good hydrophilic retention and separation selectivity, high column efficiency and novel structure

Inactive Publication Date: 2017-08-11
DALIAN UNIV OF TECH
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Problems solved by technology

At present, there are still problems such as insufficient hydrophilicity, low column efficiency, short lifetime and insufficient coverage of polar compounds due to limited types of HILIC stationary phases. Therefore, the development of new HILIC stationary phases is important for expanding the coverage of HILIC and promoting its development. It is of great significance and has now become an important research branch in the field of chromatography. At present, the main way to obtain a new type of HILIC stationary phase is to modify the surface of the carrier matrix by using different hydrophilic selection molecules.

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  • Hydrophilic interaction chromatographic stationary phase based on amide functional imidazole ionic liquid and preparation method and application of hydrophilic interaction chromatographic stationary phase
  • Hydrophilic interaction chromatographic stationary phase based on amide functional imidazole ionic liquid and preparation method and application of hydrophilic interaction chromatographic stationary phase
  • Hydrophilic interaction chromatographic stationary phase based on amide functional imidazole ionic liquid and preparation method and application of hydrophilic interaction chromatographic stationary phase

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Embodiment Construction

[0026] The present invention is further illustrated by examples below, and the examples are only limited to illustrate the present invention for easy understanding, rather than limiting the present invention.

[0027] Preparation of Amide Functionalized Imidazolium Ionic Liquid Bonded Silica Stationary Phase

[0028] The preparation process of amide-functionalized imidazolium ionic liquid bonded silica stationary phase is as follows: figure 1 As shown, the amide-functionalized imidazolium ionic liquid was obtained first, and then bonded to the surface of 3-mercaptopropyl-modified silica spheres to obtain the target stationary phase. First, 9.2 g of 2-bromoacetamide was dissolved in acetonitrile solvent, added to a round bottom flask and mixed with 10.0 g of 1-vinylimidazole under stirring, and the mixture was continuously stirred for 48 hours under the protection of argon. The reaction solution was filtered to obtain a white solid, which was washed at least five times with ac...

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Abstract

The invention discloses a hydrophilic interaction chromatographic stationary phase based on amide functional imidazole ionic liquid and a preparation method and application of the hydrophilic interaction chromatographic stationary phase, and belongs to the field of high performance liquid chromatography stationary phases. Ionic liquid is bonded to a 3-sulfydryl propyl modified silicon dioxide ball surface to prepare the hydrophilic interaction chromatographic stationary phase through a sulfydryl-double bond clicking chemical reaction. The preparation method comprises the steps that firstly, the amide functional imidazole ionic liquid of terminal alkenyl is prepared firstly, the silicon dioxide ball surface is grafted with 3-sulfydryl propyl groups through a silanization reaction, and the ionic liquid is bonded to the silicon ball surface modified by 3-sulfydryl propyl. The surface bonded amide imidazole ionic liquid serves as the hydrophilic interaction chromatography stationary phase to show good reservation and selectivity on typical hydrophilic compounds, and the column efficiency amounts to that of a commercial amide hydrophilic interaction chromatography stationary phase. In addition, due to the unique multiple interactions of the hydrophilic interaction chromatographic stationary phase, the stationary phase has especially good reservation and separation selectivity on flavonoid matter under the hydrophilic chromatography mode, and good application prospects are achieved.

Description

technical field [0001] The invention belongs to the field of high-performance liquid chromatography stationary phase, and in particular relates to amide functionalized imidazole ionic liquid bonded silica gel as a hydrophilic interaction chromatography stationary phase, a preparation method thereof and the separation application of hydrophilic compounds in a hydrophilic interaction mode. Background technique [0002] Chromatography is a very important modern separation and analysis technology, which plays a very important role in many aspects. Among them, high-performance liquid chromatography (HPLC) has been greatly developed since the 1970s. It is currently used in food safety, environmental protection, Drug analysis and metabolomics and other fields have been widely used. For chromatographic separation, the stationary phase plays a key role. Therefore, the research and development of stationary phase has always been a research hotspot in the field of chromatography. HPLC...

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Application Information

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IPC IPC(8): B01J20/286B01J20/30B01D15/32
CPCB01D15/32B01J20/286B01J2220/52
Inventor 乔利珍
Owner DALIAN UNIV OF TECH
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