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Polymer chain-modified silica gel matrix hydrophilic interaction chromatography stationary phase as well as preparation and application thereof

A chromatographic stationary phase and hydrophilic interaction technology, which is applied in the field of hydrophilic interaction liquid chromatography stationary phase and its preparation, can solve the problems of complex preparation, insufficient hydrophilicity of stationary phase, insufficient separation selectivity, etc., and achieves high reaction efficiency and dispersion. Good performance and wide application range

Active Publication Date: 2017-06-09
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above-mentioned stationary phases still have problems such as insufficient hydrophilicity, insufficient separation selectivity, and complicated preparation.

Method used

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  • Polymer chain-modified silica gel matrix hydrophilic interaction chromatography stationary phase as well as preparation and application thereof
  • Polymer chain-modified silica gel matrix hydrophilic interaction chromatography stationary phase as well as preparation and application thereof
  • Polymer chain-modified silica gel matrix hydrophilic interaction chromatography stationary phase as well as preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] 1. Preparation of mercaptosilica spheres: In a 250mL round bottom flask, add 120mL of toluene, add 5g of silica gel particles with a particle size of 5μm, and 2ml of 3-mercaptopropyltriethoxysilane, and disperse evenly by ultrasonication for 2 minutes. Connect a condenser tube to the flask, stir mechanically, maintain a speed of 300 rad / min, and pass nitrogen gas for 10 minutes. The reaction device was placed in an oil bath, heated to reflux at 110°C for 13 hours, the reaction was stopped, and cooled to room temperature. Centrifuge at a speed of 3000 rad / min in a high-speed centrifuge, remove the supernatant, use toluene, acetone, methanol, and acetone to filter and wash in sequence, repeat the suction and filter for 3 times, and dry in a vacuum oven at 50°C for 24 hours to obtain Silica gel particles modified with mercapto groups.

[0041]2. Preparation of hydrophilic polymer chains on the surface of silica gel: In a 250mL round bottom flask, add 100mL of the reaction...

Embodiment 2

[0045] The stationary phase particles prepared in Example 1 were filled in a 4.6mm*150mm stainless steel HPLC column, and the prepared chromatographic column was used to separate the mixture of nucleosides and bases in a hydrophilic mode. The separation conditions are: acetonitrile / water (volume ratio is 81 to 19) as mobile phase, flow rate is 1ml / min, column temperature is 25°C, the separation chromatogram is as follows figure 2 As shown, 1, 2, 3, 4, and 5 in the figure are respectively thymidine, uridine, cytidine, cytosine, and guanosine. The separation results show that on the hydrophilic interaction chromatographic column provided by the invention, nucleosides and bases are well separated by baseline, indicating that the stationary phase has typical hydrophilic interaction characteristics and good separation selectivity.

Embodiment 3

[0047] Organic acidic compounds were separated using the hydrophilic interaction chromatographic column prepared in Example 2. The separation conditions are as follows: 88% acetonitrile, 2% ammonium acetate (100 mM concentration), and 10% water are used as the mobile phase, the flow rate is 1 ml / min, and the column temperature is 25° C. The separation chromatogram is as image 3 As shown, 1, 2, 3, 4, and 5 in the figure are respectively phenol, p-cresol, 3,5-dinitrobenzoic acid, benzoic acid, and 4-hydroxybenzoic acid. The separation chromatogram shows that these several organic acids have good retention on the chromatographic column provided by the invention, and good baseline separation is obtained.

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Abstract

The invention relates to a polymer chain-modified silica gel matrix hydrophilic interaction chromatography stationary phase as well as a preparation method and application thereof. Silica gel particles are taken as a matrix, and a hydroxyl-containing allyl monomer and methylene bisacrylamide are grafted on the surface of silica gel by means of a click copolymerization reaction of thiol-ene, so that a chromatography stationary phase which has a three-dimensional dendritic polymer chain, is rich in hydroxyl and amide hydrophilic functional groups and has hydrophilic interaction can be formed. The hydroxyl and amide hydrophilic functional groups and the like are introduced according to the method provided by the invention, so that not only are the defects that the traditional post-modification method is complicated in steps and low in reaction efficiency overcome, but a rich hydrophilic layer can be also formed by the three-dimensional polymer chain-shaped structure, therefore, the hydrophilic chromatography stationary phase has better advantages. The liquid chromatography stationary phase provided by the invention is novel in structure and excellent in hydrophilic performance, can be widely used for separation of various samples and selective enrichment and separation of glycopeptides, and has a very high practical value in the fields of separation analysis, glycoproteomics, and the like.

Description

technical field [0001] The invention relates to a hydrophilic interaction liquid chromatography stationary phase and a preparation method thereof, as well as its application in separation analysis and glycoproteomics. Background technique [0002] Since the 1970s, high-performance liquid chromatography (HPLC) technology has been greatly developed in terms of instrument systems, stationary phases, and separation theory. Due to its high efficiency and rapidity, this technique is widely used in different research fields, such as pharmaceuticals, life sciences, environmental analysis, and food safety, etc. (Fekete, S et al, TrAC. 2014, 63, 2-13). As the core of chromatography technology, stationary phase fundamentally determines the separation selectivity and separation efficiency of chromatography. In recent years, with the continuous development of proteomics, metabolomics, drug analysis and other fields, the separation of highly polar substances has attracted the attention o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30B01D15/08C08F292/00
CPCB01D15/08B01J20/286B01J2220/54C08F292/00C08F220/58C08F222/385
Inventor 张丽华邵文亚梁玉杨开广张玉奎
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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