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Oligopeptide phase reversal chromatography stationary phase and preparation method thereof

A technology of reversed-phase chromatography and stationary phase, applied in chemical instruments and methods, and other chemical processes, can solve problems such as scarcity, and achieve the effect of single reaction site, high selectivity, high conversion rate, and regular and orderly structure

Inactive Publication Date: 2010-04-07
EAST CHINA UNIV OF SCI & TECH
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  • Abstract
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  • Claims
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Problems solved by technology

However, there is still a lack of new reversed-phase stationary phases that can be combined with C18 stationary phases for two-dimensional chromatographic separations.

Method used

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  • Oligopeptide phase reversal chromatography stationary phase and preparation method thereof
  • Oligopeptide phase reversal chromatography stationary phase and preparation method thereof
  • Oligopeptide phase reversal chromatography stationary phase and preparation method thereof

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Embodiment

[0040] An embodiment comprises the following steps:

[0041] (1) Preparation of Azidesulfonylimidazole Hydrochloride

[0042] Add 50mmol sulfonyl chloride (about 4mL) dropwise to 50mmol NaN in an ice-water bath 3 (about 3.2 g) in 100 mL of anhydrous MeCN suspension, the mixture was stirred overnight at room temperature;

[0043] Slowly add 100mmol imidazole (about 6.8g) into the above system under an ice-water bath, and stir the obtained emulsion at room temperature overnight;

[0044] Add 75mL of ethyl acetate to the mixture to dilute, successively wash with 2×75mL H 2 O, 2 x 120mL saturated NaHCO 3 The solution was extracted, and the organic phase was added with anhydrous Na 2 SO 4 Drying, suction filtration, and salt formation: Add HCl in EtOH solution (5.4mL acetyl chloride was added dropwise to 19mL EtOH under ice-water bath) to the above organic phase, a white solid was precipitated, suction filtration, washing with ethyl acetate, Obtain solid azidesulfonylimidazol...

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Abstract

The invention relates to an oligopeptide phase reversal chromatography stationary phase and a preparation method thereof. The preparation method adopts 'link chemistry' as a bonding reaction method to bond oligopeptide molecules and comprises the following steps: firstly, introducing terminal alkynyl on a silica gel surface; and then, taking methanol, acetonitrile, dimethyl sulfoxide or a mixture of the solvents as a reaction solvent to bond oligopeptide modified with azide groups on the silica gel surface, thereby obtaining the oligopeptide phase reversal chromatography stationary phase. The oligopeptide phase reversal chromatography stationary phase has orderly structure and single reaction site; moreover, the structure of the stationary phase introduces triazole rings, urea bonds, benzene rings, peptide bonds and ester groups to generate multiple kinds of acting force, such as hydrogen-bonding action, electrostatic interaction, Pi-Pi action, dipole-dipole interaction, hydrophobic interaction and the like, thereby realizing orthogonal separation on complex compositions in a two-dimensional structure constructed with C18; and 'link chemistry' is adopted as the bonding reaction method to realize immobilization of high selectivity and high conversation efficiency under moderate conditions.

Description

【Technical field】 [0001] The invention relates to liquid chromatography stationary phase technology, specifically, a method for preparing a reversed-phase chromatography stationary phase using "click chemistry" as a bonding method to bond oligopeptides. 【technical background】 [0002] Reversed-phase high-performance liquid chromatography (RP-HPLC for short) is currently the most widely used high-efficiency separation technology. However, the most commonly used hydrophobic stationary phases in reversed-phase chromatography, such as C18, C8, etc., are mainly long-chain alkanes, resulting in The force between the stationary phase and the separated components is too single (mainly hydrophobic interaction), which makes the separation of complex components (such as in the fields of proteomics, metabolomics, pharmaceutical industry, natural products, etc.) huge challenge. Reversed-phase / reversed-phase two-dimensional chromatography is an important means for the separation of compl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/287
Inventor 梁鑫淼薛梅云黄洪雪褚长虎
Owner EAST CHINA UNIV OF SCI & TECH
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