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Metal organic framework-silicon based composite material, and preparation method and application thereof

A metal-organic framework and silicon-based composite material technology, which is applied in the field of mass spectrometry and can solve the problems of interfering with the determination of small molecular compounds and low sensitivity, etc.

Active Publication Date: 2020-01-17
INST OF ENVIRONMENTAL MEDICINE & OCCUPATIONAL MEDICINE ACAD OF MILITARY MEDICINE ACAD OF MILITARY SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above matrices still have deficiencies. For example, graphene itself has strong adhesion on the MALDI target plate, and it will have a strong adsorption on small molecular compounds, so the sensitivity is not high; although the organic salt matrix has good salt tolerance, However, when analyzing small molecular compounds, many isotope peaks will appear, so it will interfere with the determination of many small molecular compounds

Method used

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  • Metal organic framework-silicon based composite material, and preparation method and application thereof
  • Metal organic framework-silicon based composite material, and preparation method and application thereof
  • Metal organic framework-silicon based composite material, and preparation method and application thereof

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preparation example Construction

[0047] In the present invention, the preparation method of the siloxane-modified silicon-based material preferably includes the following steps:

[0048] The silicon-based raw material, 3-aminopropyltriethoxysilane and solvent are mixed and then hydrolyzed to obtain the silicon-based material modified by siloxane.

[0049] In the present invention, the surface of the silicon-based raw material is modified with silanol, which can be hydrolyzed with 3-aminopropyltriethoxysilane to obtain a siloxane-modified silicon-based material. In the present invention, the silicon-based raw material preferably includes silica microspheres or SBA-15 mesoporous materials; the particle size of the silica microspheres is preferably 25-100 nm, more preferably 25-50 nm. In the present invention, there is no special limitation on the source of the silicon-based raw material, and commercially available products well known to those skilled in the art can be used. In the present invention, the amount...

Embodiment 1

[0067] (1) Preparation of MOF materials

[0068] 4.63g of Al(NO 3 ) 3 9H 2 O and 2.75 g of 2,5-dimercaptoterephthalic acid were mixed in 30 mL of ultrapure water; the resulting mixture was transferred to a Teflon-lined autoclave reactor, sealed and placed in an oven at React at 150°C for 5 hours; after the reaction is completed, centrifuge the obtained system at 4000rpm for 5min, alternately wash the centrifuged solid material with dimethylformamide (DMF) and absolute ethanol for 4 times, centrifuge at 4000rpm for 5min after each washing, and The solid material obtained after the last centrifugation was dried in a vacuum oven at 120°C for 12 hours to obtain the MOF material.

[0069] (2) Preparation of SBA-15@APTES@MOF

[0070] Ultrasonically disperse 0.5g of SBA-15 mesoporous material and 50mL of absolute ethanol in a beaker and transfer it to a three-necked flask, wash the beaker with 100mL of absolute ethanol, and combine the washings into the three-necked flask; then a...

Embodiment 2

[0073] Only the SBA-15 mesoporous material in Example 1 is replaced by silica microspheres (average particle size is 25nm), and the rest of the operations are carried out according to the method of Example 1, through the prepared MOF material and SiO 2 @APTES, SiO was finally prepared 2 @APTES @MOF.

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Abstract

The invention provides a metal organic framework-silicon based composite material, and a preparation method and application thereof, and belongs to the technical field of mass spectrometry analysis. The metal organic framework-silicon based composite material provided by the invention is formed by a condensation reaction of a metal-organic framework material containing a pi-pi conjugated structureand a siloxane modified silicon based material, and the advantages of the metal-organic framework material and the siloxane modified silicon based material are combined. In the composite material, the metal-organic framework material can enhance ionization efficiency of a target in MALDI-TOF MS analysis process, and the siloxane modified silicon based material can promote desorption efficiency ofthe target in MALDI-TOF MS analysis, so that the composite material can be well applied to MALDI-TOF MS detection of small molecular compounds, the problem of serious background interference caused in traditional matrix detection of small molecular compounds can be effectively overcome, and detection sensitivity can be improved.

Description

technical field [0001] The invention relates to the technical field of mass spectrometry, in particular to a metal organic framework-silicon-based composite material and a preparation method and application thereof. Background technique [0002] Matrix-assisted laser desorption ionization-time-of-flight mass spectrometry (Matrix-assisted laserdesorption / ionizationtime offlightmass spectrometry, MALDI-TOF MS), as a soft ionization technique, has developed rapidly since the 1980s. Due to its high sensitivity, simple operation, and reasonable tolerance to impurities, MALDI-TOF MS has been widely used in the analysis and identification of peptides, proteins, and polymers. It is used in disease diagnosis, proteomics, environmental science, Research fields such as analytical chemistry are playing an increasingly important role. [0003] The basic principle of MALDI-TOF MS is: the sample to be tested is uniformly mixed with the matrix. When the co-crystal film formed between the s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/30G01N27/64
CPCB01J20/226G01N27/64
Inventor 周焕英高志贤王永辉闫宏远范冰燕吴瑾
Owner INST OF ENVIRONMENTAL MEDICINE & OCCUPATIONAL MEDICINE ACAD OF MILITARY MEDICINE ACAD OF MILITARY SCI
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