Core-shell type gold/mesoporous silicon carbon composite nanometer material, preparation method and application

A composite nanomaterial and nanomaterial technology, which is applied in the field of preparation, core-shell type gold/mesoporous silicon carbon composite nanomaterials, can solve problems such as background interference of low molecular weight analytes, and avoid the interference of matrix molecular ion peak signals. , to achieve the effect of accurate analysis, high mechanical strength and chemical stability

Inactive Publication Date: 2015-09-16
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the introduction of organic matrix will generate a large number of matrix molecular ion peaks in the low molecular weight range, which will cause serious background interference to the detection of low molecular weight analytes (Analytical and Bioanalytical Chemistry.2002.373:571; Mass Spectrometry Reviews.2011.30:101)

Method used

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  • Core-shell type gold/mesoporous silicon carbon composite nanometer material, preparation method and application
  • Core-shell type gold/mesoporous silicon carbon composite nanometer material, preparation method and application
  • Core-shell type gold/mesoporous silicon carbon composite nanometer material, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Example 1, Preparation of core-shell gold / mesoporous silicon-carbon composite nanomaterials

[0042] (1) Mix ethanol and water at a ratio of 1:1, add 0.640g of cetyltrimethylammonium bromide, heat up to 70°C and stir well; add 55mg of chloroauric acid, stir for 5-10min, then add Adjust the pH to 10-12 with KOH, maintain the reaction at 70°C for 30 minutes, add deionized water twice the volume of the initially added water, add tetraethyl orthosilicate dropwise and add KOH again to maintain the pH between 10-12, and react at 70°C for 2 hours , centrifuged, washed, and dried to prepare a nanomaterial with gold nanoparticles as the core and an ordered mesoporous structure of silica-surfactant as the shell;

[0043] (2) Disperse the above composite material in a dilute sulfuric acid solution, raise the temperature to 100°C and 160°C in turn, and maintain it for 12h, and then calcinate at 600°C for 3h under an argon atmosphere to realize the synthesis of the surfactant cetylt...

Embodiment 2

[0044] Example 2, Preparation of Core-shell Gold / Mesoporous Silicon Carbon Composite Nanomaterials

[0045] (1) Mix methanol and water at a ratio of 1:3, add 0.640g of cetyltrimethylammonium bromide, heat up to 60°C and stir well; add 55mg of chloroauric acid, stir for 5-10min, then add Adjust the pH to 10-12 with NaOH, maintain the reaction at 60°C for 30 minutes, add 1.5 times the volume of deionized water initially added, add methyl orthosilicate dropwise and add NaOH again to maintain the pH between 10-12, and react at 60°C for 2 hours , centrifuged, washed, and dried to prepare a nanomaterial with gold nanoparticles as the core and an ordered mesoporous structure of silica-surfactant as the shell;

[0046] (2) Disperse the above composite material in dilute sulfuric acid solution, raise the temperature to 100°C and 160°C in sequence, and maintain it for 12h, then calcinate at 550°C for 3h under a nitrogen atmosphere to achieve the synthesis of the surfactant cetyltrimethy...

Embodiment 7

[0050] Embodiment 7, the method for detecting amino acid sample arginine

[0051] (1) The instrument is: AB SCIEX TOF / TOF TM 5800System mass spectrometer; nitrogen laser, wavelength 337nm, adopts ion delayed extraction (delayed extraction) and reflection (reflectorn) working mode, positive ion detection.

[0052] (2) The mixed spotting method was used, that is, the amino acid sample solution and the core-shell gold / mesoporous silicon carbon composite nanomaterial solution were pre-mixed, fixed on a MALDI plate, dried naturally, and analyzed by laser desorption ionization mass spectrometry.

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Abstract

The invention discloses a core-shell type gold / mesoporous silicon carbon composite nanometer material, a preparation method and application. The core-shell type gold / mesoporous silicon carbon composite nanometer material is characterized in that a core-shell type nanometer material is synthesized with gold nanometer particles as an inner core and ordered mesoporous structure silicon dioxide surface active agent as a shell, and a core-shell type nanometer material with gold nanometer particles as an inner core and a mesoporous silicon carbon composite structure as a shell is prepared through in-situ carbonization of the surface active agent in the mesoporous silicon dioxide shell. The material has the advantages that the specific surface area is high, the pore volume is high, the material is wrapped by a uniform ordered mesoporous structure silicon carbon shell, and the thickness of the shell is controllable. The nanometer material mainly serves as a matrix of the surface auxiliary laser desorption ionization mass spectrometry, the background interference of a traditional organic matrix within the low-molecular-weight range can be avoided, and the efficient laser desorption ionization of compound to be measured is achieved.

Description

technical field [0001] The invention belongs to the field of advanced nanocomposite materials and biological and medical analysis and detection, and specifically relates to a core-shell type gold / mesoporous silicon carbon composite nanomaterial, a preparation method and an application. Background technique [0002] In 1988, German scientists Karas and Hillenkamp proposed matrix-assisted laser desorption / ionization (MALDI). MALDI uses the laser energy absorbed by the matrix to assist the analyte to enter the gas phase desorption ionization, which solves the ionization problem of non-volatile and thermally unstable high-mass biomolecules (Analytical Chemistry.1988.60:2299). In MALDI, the matrix plays a decisive role in absorbing, transmitting laser energy, and ionizing the sample. At present, the commonly used commercial substrates are mostly organic molecules, such as 2,5-dihydroxybenzoic acid (DHB), α-cyano-4-hydroxycinnamic acid (CHCA), sinapinic acid (SA) and their deriva...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F1/00B22F9/24B82Y40/00B82Y30/00
Inventor 吴仁安徐桂菊张红燕
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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