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Nickel particle modified carbon matrix, preparation and mass spectrometry application of small molecule metabolism

A technology for the analysis of metabolic small molecules and mass spectrometry, which is applied in the application of mass spectrometry of metabolic small molecules, in the field of nickel particle modified carbon matrix, which can solve the problems of low solubility, limit the ionization efficiency and sensitivity of MS, and achieve high-throughput performance. , the effect of good UV absorption ability and simple preparation method

Active Publication Date: 2021-06-22
SHANXI MEDICAL UNIV
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Problems solved by technology

Although the research on new carbon substrates has become a hot spot, their low solubility still limits the MS ionization efficiency and sensitivity of some small molecules.

Method used

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  • Nickel particle modified carbon matrix, preparation and mass spectrometry application of small molecule metabolism
  • Nickel particle modified carbon matrix, preparation and mass spectrometry application of small molecule metabolism
  • Nickel particle modified carbon matrix, preparation and mass spectrometry application of small molecule metabolism

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preparation example Construction

[0039] Preparation method of nickel particles modified carbon matrix, including the following steps:

[0040] S1, a solution of tetrahydrate acetate is dispersed into a solution of polyvinylpyrrolidone, and the mixed solution is slowly added dropwise to the oxide oxide solution under agitation conditions, and the gel is formed for 12 hours, further freeze drying For use; the oxide oxide solution is 3 mg / ml to 5 mg / ml; the quadrhant acid nickel added amount is 100 mg to 300 mg; the concentration of the polyvinylpyrrolidone solution is 10 mg / mL ~ 50 mg / ml;

[0041] S2, the product of step S1, in h 2 / AR atmosphere, high temperature thermal reduction can obtain nickel particles modified graphene to use; the high temperature heat reduction temperature rise procedure is: the temperature rise rate is 2 ° C / min ~ 5 ° C / min, heated to 500 ° C ~ 700 ° C Insulation 1 to 3 h, then it was subsequent to the room temperature to obtain nickel particles modified graphene;

[0042] S3...

Embodiment 1

[0052] (1) After 124.42 mg of tetrahydrate acetate, the solution of 16 mg / ml of polyvinylpyrrolidone is taken sufficiently dissolved, and the mixed solution is slowly added dropwise to 4 mg / ml oxide solution under stirring, forming gel shape. Keep 12 hours, further freeze drying for use.

[0053] (2) Put the above product in h 2 (10%) / Ar atmosphere, heating rate of heat supplementation at 4 ° C / min was heated to 650 ° C for 2 h, followed by a graphene modified of nickel particles to be used.

[0054] (3) The graphene modified with nickel particles is heated under argon, and the temperature of the temperature of 4 ° C / min is heated to 800 ° C, and the acetonitrile solution is loaded into the tube furnace, and the vapor deposition remains 0.5 h, then only in argon The tubular furnace is naturally cooled under the atmosphere to obtain a complex of nickel-particle modified nitrogen doped carbon nanotube / graphene (Ni / N-CNT / GR).

[0055] The prepared Ni / N-CNT / GR comp...

Embodiment 2

[0057] (1) After the solution of 248.84 mg of nickel acetate dispersion of 16 mg / ml polyvinylpyrrolidone is sufficiently dissolved, the mixed solution is slowly added dropwise to 4 mg / ml oxide solution under agitation conditions to form gels. Keep 12 hours, further freeze drying for use.

[0058] (2) Put the above product in h 2 (10%) / Ar atmosphere, heating rate of heat supplementation at 4 ° C / min was heated to 650 ° C for 2 h, followed by a graphene modified of nickel particles to be used.

[0059] (3) The graphene modified with nickel particles is heated under argon, and the temperature of the temperature of 4 ° C / min is heated to 800 ° C, and the acetonitrile solution is loaded into the tube furnace, and the vapor deposition remains 0.5 h, then only in argon The tubular furnace is naturally cooled under the atmosphere to obtain a complex of nickel-particle modified nitrogen doped carbon nanotube / graphene (Ni / N-CNT / GR). Through analysis, the graphene / porous ca...

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Abstract

The invention relates to a nickel particle modified carbon substrate, which is formed by compounding nitrogen and oxygen heteroatoms, nickel particles and carbon nanotube / graphene, and the compound has large specific surface area, good ultraviolet absorption capability and strong electron donor performance. The nickel particle modified carbon matrix has a large specific surface area of 100m<2> / g-300m<2> / g, has strong ultraviolet absorption capacity at 355nm, and has an absorbance value of 0.35-0.56, so that the nickel particle modified carbon-based compound can be used as a novel mass spectrum carbon matrix to enhance the desorption ionization effect of low molecular weight substances, and is applied to analysis of small molecular metabolites with m / z less than 700. Furthermore, the substrate can be applied to gastric cancer saliva metabolite detection and screening. The nickel particle modified nitrogen-doped carbon nanotube / graphene compound synthesized by the invention is low in preparation cost and simple in preparation method. The large-scale production can be met; the industrialization is realized. The detection method provided by the invention has the advantages of high throughput, rapidness, high sensitivity and the like, and has the potential of being applied to clinical screening of early gastric cancer patients.

Description

Technical field [0001] The present invention relates to a low molecular weight material detection application field based on matrix auxiliary laser analysis ionization flight time, and more particularly to a nickel particle modified carbon matrix, a preparation method, and a mass spectrometry of metabolic small molecules. Background technique [0002] Gastric cancer is one of the common digestive system malignant cancer and the third cause of global cancer death. At present, gastric cancer is the second common malignant tumor and the third tumor death caused by my country, which seriously threatens the health of the people. At the same time, 80% of patients with gastric cancer are not obvious in early period, and it is easy to neglect or missed diagnosis. Clinically, the diagnosis and staging of gastric cancer is mainly analyzed by fiber endoscopy and tissue pathological analysis, but the symptoms of early gastric cancer are not significantly missed, invasive diagnosis gives disc...

Claims

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Application Information

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IPC IPC(8): C01B32/184C01B32/16B22F9/22G01N27/626
CPCC01B32/184C01B32/16B22F9/22G01N27/628C01B2202/32C01B2204/32
Inventor 张瑞平赵慧芳赵华宇刘玉龙
Owner SHANXI MEDICAL UNIV
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