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Zwitterionic Hydrophilic Interaction Chromatography Stationary Phase Bonded Separately by Anion and Cation, Preparation Method and Application

A chromatographic stationary phase and hydrophilic interaction technology, which is applied in the field of zwitterion-bonded silica gel as a hydrophilic interaction chromatography stationary phase, can solve the problems such as the binding of positive and negative charges, and the inability to stretch freely, and achieve novel and positive charge distribution. The effect of negatively charged structure freedom and good separation selectivity

Inactive Publication Date: 2019-07-16
DALIAN UNIV OF TECH
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Problems solved by technology

In these zwitterionic stationary phases, there are certain differences in charge groups and distribution forms, but the positive and negative charge centers are connected to the molecular structure through covalent bonds, and the entire molecule is bonded to the surface of the stationary phase in a certain way. Sexual species show good HILIC retention and separation, but the positive and negative charge arrangements are bound to each other and cannot stretch freely to interact with the analyte

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  • Zwitterionic Hydrophilic Interaction Chromatography Stationary Phase Bonded Separately by Anion and Cation, Preparation Method and Application
  • Zwitterionic Hydrophilic Interaction Chromatography Stationary Phase Bonded Separately by Anion and Cation, Preparation Method and Application
  • Zwitterionic Hydrophilic Interaction Chromatography Stationary Phase Bonded Separately by Anion and Cation, Preparation Method and Application

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Embodiment Construction

[0027] 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.

[0028] Preparation of ionic liquids in which anions and cations can be bonded separately

[0029] The preparation steps of zwitterionic stationary phases with anions and cations bonded separately are as follows: figure 1 shown. Dissolve 1.23g of 2-bromoethyl acrylate in a small amount of ethyl acetate, add 3.0g of 1-methylimidazole while stirring, and react the reaction solution in the dark under the protection of argon for about 24 hours until the reactant forms a Stirring doesn't work. The solvent in the upper layer was removed by standing, and the viscous product was washed with ethyl acetate for 4-5 to remove unreacted raw materials, and dried under vacuum at 60°C to obtain product 1. The obtained product 1 was exchanged with 3-sulfopropyl acrylate potassium salt...

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Abstract

The invention relates to an anion and cation respectively bonded amphoteric interaction chromatography stationary phase, and a preparation method and an application thereof, and belongs to the field of high performance liquid chromatography stationary phases. The anion and cation respectively bonded amphoteric interaction chromatography stationary phase is prepared through bonding the surface of a 3-mercaptopropyl group modified silica sphere with an ionic liquid through a "mercapto group-double bond" click chemical reaction. The preparation method comprises the following steps: preparing a methylimidazole ionic liquid with the tail end being an acrylate structure, and carrying out ion exchange to obtain an anion and cation combined ionic liquid with the tail end being an acrylate structure; and grafting the surface of a silica sphere with a 3-mercaptopropyl group through a silanization reaction, and bonding the 3-mercaptopropyl group modified silicon sphere surface with the ionic liquid by using a "mercapto group-alkenyl group" click chemical reaction. The hydrophilic interaction chromatography stationary phase has very good reservation and separation selectivity to different types of polar and hydrophilic compounds, and has good application prospect.

Description

technical field [0001] The invention belongs to the field of high-performance liquid chromatography stationary phase, and in particular relates to a zwitterion-bonded silica gel grafted with anions and cations respectively as a hydrophilic interaction chromatography stationary phase, a preparation method and a separation application. Background technique [0002] In recent years, hydrophilic interaction chromatography (HILIC) has been used more and more in the separation of polar and hydrophilic samples, and has attracted widespread attention. It has become a research hotspot in the field of chromatography. No or weak strong polar and hydrophilic substances are retained in phase chromatography (RPLC), while solving the solubility problem of samples in normal phase chromatography (NPLC) and improving compatibility with mass spectrometry, showing very good Application prospect. For the application of HILIC, the development of stationary phase has a great influence on the sele...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/286B01J20/30B01D15/30B01D15/32
CPCB01D15/305B01D15/32B01J20/286B01J2220/52
Inventor 乔利珍
Owner DALIAN UNIV OF TECH
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