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Method for producing capillary electrochromatography monolithic column made from silicon dioxide-titanic oxide integral material and uses thereof

A technology of titanium dioxide and silicon dioxide, which is applied in the field of preparation of electrochromatographic monolithic columns, can solve problems such as powder agglomeration, performance index impact, and inappropriate filling of capillary electrochromatographic packed columns, and achieve good stability and repeatability and long service life Longer, less non-specific adsorption effect

Inactive Publication Date: 2009-04-15
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The commonly used sol-gel method, chemical precipitation method, and gas phase method to prepare nano-titanium dioxide require post-calcination. In addition to easily causing powder agglomeration, which greatly affects its performance indicators, the particle size of nano-titanium dioxide is also unsuitable. Directly Packed Capillary Electrochromatographic Columns

Method used

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  • Method for producing capillary electrochromatography monolithic column made from silicon dioxide-titanic oxide integral material and uses thereof
  • Method for producing capillary electrochromatography monolithic column made from silicon dioxide-titanic oxide integral material and uses thereof
  • Method for producing capillary electrochromatography monolithic column made from silicon dioxide-titanic oxide integral material and uses thereof

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Embodiment 1

[0036] Preparation of monolithic column: mix 2.08g tetraethyl orthosilicate, 2.404g isopropanol, and 0.36g water, add hydrochloric acid dropwise to make the pH of the solution 2, stir for 1h; add titanium with a molar ratio of 1:1 dropwise Add 0.16 g of CTAB, heat at 40° C. for 3 hours, and age for 1 day. figure 1 For coated SiO 2 -TiO 2 SEM image of the overall material.

Embodiment 2

[0038] Preparation of monolithic column: mix 2.08g tetraethyl orthosilicate, 2.404g isopropanol, and 0.36g water, add hydrochloric acid dropwise to make the pH of the solution 2, stir for 1h; add titanium with a molar ratio of 1:1 dropwise Add 0.18 g of CTAB, heat at 30° C. for 5 hours, and age for 1 day. figure 2 Digested peptides of α-casein treated with SiO 2 -TiO 2 Mass spectra before and after monolithic column enrichment.

Embodiment 3

[0040]Preparation of monolithic column: mix 2.08g tetraethyl orthosilicate, 2.404g isopropanol, and 0.36g water, add hydrochloric acid dropwise to make the pH of the solution 2, stir for 1h; add titanium with a molar ratio of 1:1 dropwise A mixed solution of 4.47 g tetrabutyl acetylacetone and acetylacetone was stirred for 30 minutes; 0.2 g of CTAB was added, heated at 40° C. for 5 hours, and aged for 1 day. Figure 3a and Figure 3b Digested peptides of α-casein treated with SiO 2 -TiO 2 Mass spectra before and after monolithic column enrichment.

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Abstract

The invention discloses a method for preparing an electrochromatography monolithic column of silicon dioxide-titanium dioxide monolithic materials, as well as application thereof. The titanium dioxide-silicon dioxide forms a mesopore molecular sieve under the action of a supramolecular template of which the mechanical strength is good, and pore diameter is easy to control according to requirement. A uniform capillary electrochromatography column with high specific surface area is prepared by one-step method. The method has the advantages that the mesopore molecular sieve which is prepared by using the supramolecular template as a structure-directing agent and has a specific pore structure, extremely high specific surface area and uniform adjustable pore diameter has the advantages of simple preparation method, good repeatability and high separation efficiency, and is suitable for the separation and enrichment of phosphorylated polypeptide, wherein titanium dioxide and silicon dioxide molecules are combined with silicon hydroxyl on the surface of the inner wall of a capillary through chemical bonds; a framework structure and the pore diameter of nanometer pores can be conveniently controlled by changing the categories and proportion of the supramolecular template; and surface properties and the chemical environment of a pore cavity are regulated so as to provide a specific molecular field.

Description

【Technical field】 [0001] The invention relates to the technical field of monolithic electrochromatographic columns, in particular to a preparation method and application of an electrochromatographic monolithic column of a silica-titania monolithic material. 【Background technique】 [0002] Protein phosphorylation plays an important regulatory role in life activities, so it is also a hot spot in the research of post-translational modification proteome. However, large-scale analysis of phosphorylated proteins is technically challenging, and the main technical challenge is analytical sensitivity. [0003] Due to the low content and low stoichiometric value of phosphorylated proteins in organisms, only a small part of most proteins in the cell is phosphorylated. Generally, the phosphorylated part of a phosphorylated protein accounts for only 10% of the total amount, so Even when the protein is expressed at a relatively high level, analysis of the phosphorylated portion of the pr...

Claims

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Application Information

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IPC IPC(8): B01J20/281B01D15/22G01N30/60C07K1/16
Inventor 张凌怡张维冰杜一平
Owner EAST CHINA UNIV OF SCI & TECH
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