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Titanium-zirconium double-metal-atom horizontally-doped honeycomb-shaped mesoporous composite material as well as synthesis method and application of titanium-zirconium double-metal-atom horizontally-doped honeycomb-shaped mesoporous composite material

A technology of composite materials and synthesis methods, which is applied in the field of honeycomb mesoporous composite materials doped with titanium-zirconium double metal atoms and its synthesis, which can solve the problems of low ionization efficiency and low abundance of phosphorylated proteins/peptides , to achieve high signal-to-noise ratio, good hydrophilic pore structure, and good stability

Inactive Publication Date: 2016-05-11
FUDAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, biological mass spectrometry is widely used in the analysis of protein post-translational modifications, but due to the low abundance and low ionization efficiency of phosphorylated proteins / peptides, and the mass spectrometry signals of phosphorylated peptides are often suppressed by non-phosphorylated peptides , leading to the direct analysis and detection of mass spectrometry will face great challenges

Method used

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  • Titanium-zirconium double-metal-atom horizontally-doped honeycomb-shaped mesoporous composite material as well as synthesis method and application of titanium-zirconium double-metal-atom horizontally-doped honeycomb-shaped mesoporous composite material
  • Titanium-zirconium double-metal-atom horizontally-doped honeycomb-shaped mesoporous composite material as well as synthesis method and application of titanium-zirconium double-metal-atom horizontally-doped honeycomb-shaped mesoporous composite material
  • Titanium-zirconium double-metal-atom horizontally-doped honeycomb-shaped mesoporous composite material as well as synthesis method and application of titanium-zirconium double-metal-atom horizontally-doped honeycomb-shaped mesoporous composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1: Synthesis of a honeycomb mesoporous composite material doped at the atomic level with Ti-Zr bimetals based on pollen as a template.

[0030] (1) Treatment of pollen samples: uniformly mix chloroform and methanol solutions at a volume ratio of 1:3.5, and then soak the ground pollen particles (PGs) in the above mixed solution for overnight; , the pollen particles were heated and refluxed in methanol solution for 24 hours; after cooling, they were centrifuged, washed with deionized water for 5 times, and dried under vacuum at 50°C;

[0031] (2) Disperse 70 mg of the product PGs obtained in step (1) in 90 mL of isopropanol solution, and sonicate for 0.5 hours;

[0032] (3) Add titanium isopropoxide (1.5mL), zirconium isopropoxide (1.0g) and diethylamine (0.04mL) to the mixed solution obtained in step (2), and stir thoroughly for 1.0 hour;

[0033] (4) The mixed solution obtained in step (3) is fully stirred, then transferred to a hydrothermal reaction kettle, ...

Embodiment 2

[0039] Example 2: The honeycomb mesoporous composite material doped with titanium-zirconium double metal atom level based on pollen as a template was applied to the enrichment and MALDI-TOF-MS detection of phosphorylated peptides in the standard β-casein enzymatic hydrolysis solution. The specific steps are as follows:

[0040] (1) Preparation of standard β-casein protein hydrolyzate: Accurately weigh 1mg of standard protein β-casein and dissolve in 25mM ammonium bicarbonate buffer, boil for 10 minutes, dilute to 1mg / mL with 25mM ammonium bicarbonate buffer, and then Add an appropriate amount of trypsin according to the protein mass ratio of 1:40, and enzymatically hydrolyze at 37°C for 16 hours;

[0041] (2) 10 mg of titanium-zirconium bimetallic doped honeycomb mesoporous composites were washed three times with 50% acetonitrile / 0.1% trifluoroacetic acid buffer, and then dispersed in 1 mL of 50% acetonitrile / 0.1% trifluoroacetic acid. In fluoroacetic acid buffer, ultrasonic...

Embodiment 3

[0045] Example 3: Apply the honeycomb mesoporous composite material doped with titanium-zirconium double metal atoms at the atomic level based on pollen as a template obtained in Example 1 to enrich the mixed solution of β-casein enzymatic hydrolyzate and bovine serum albumin (BSA) enzymatic hydrolyzate Detection with MALDI-TOF-MS.

[0046] (1) Preparation of standard protein hydrolyzate: Accurately weigh 1mg of standard protein β-casein and 10mg of standard protein BSA, dissolve them in 1mL of 25mM ammonium bicarbonate buffer, boil for 10 minutes, and mix them according to the ratio of 1:40 to protein. Add appropriate amount of trypsin to 1mg / mLβ-casein protein solution and 10mg / mLBSA protein solution, and enzymatically digest at 37°C for 16 hours.

[0047] (2) Enrichment of the sample: Mix the β-casein enzymolysis solution with the BSA enzymolysis solution according to the protein mass ratio of 1:1500, take 2 μL of the standard proteolysis solution mixed solution and add i...

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Abstract

The invention belongs to the technical field of nano materials and detection, and in particular relates to a synthesis method and application of a titanium-zirconium double-metal-atom horizontally-doped honeycomb-shaped mesoporous composite material taking pollen as a template. The titanium-zirconium double-metal-atom horizontally-doped honeycomb-shaped mesoporous composite material taking pollen particles as the template is formed by synthesizing the pollen particles coated with titanium-zirconium double-metal oxide through a one-pot method and calcining at a high temperature. The material has a large specific surface area, strong hydrophily and relatively good biocompatibility; the template pollen is removed in a calcining process and titanium-zirconium double-metal-atom horizontal doping is performed to form double-metal oxide, and the composite material can have relatively good coordination with a phosphorylated peptide section of a phosphate radical containing negative charges, so that efficient separation and enrichment of a low-abundance phosphorylated peptide mixed sample can be realized. The titanium-zirconium double-metal-atom horizontally-doped honeycomb-shaped mesoporous composite material is novel, simple and convenient, low in cost, practical and efficient, has good repeatability and high stability, and has a wide application prospect.

Description

technical field [0001] The invention belongs to the technical field of advanced nanometer materials and detection, and in particular relates to a honeycomb-shaped mesoporous composite material doped with titanium-zirconium double metal atoms at the atomic level and its synthesis method and application. technical background [0002] With the completion of the Human Genome Sequencing Project, the study of proteomics has become the focus of research in the field of life sciences. Reversible phosphorylation of proteins is the most common post-translational modification of proteins in biological cells, and plays an irreplaceable role in life processes such as cell development, metabolism, disease monitoring, signal transduction, enzyme activity regulation, and gene expression. At present, biological mass spectrometry is widely used in the analysis of protein post-translational modifications, but due to the low abundance and low ionization efficiency of phosphorylated proteins / pep...

Claims

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Application Information

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IPC IPC(8): B01J20/282B01D15/38G01N27/62
CPCB01D15/3828G01N33/6848B01J20/282B01D2015/3838
Inventor 高明霞张祥民王嘉希李杰王亚楠
Owner FUDAN UNIV
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