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Sea urchin-type Prussian blue-palladium core-shell structure loaded nitrogen-doped graphene nanocomposites and its prepared electrodes and applications

A technology of nitrogen-doped graphene and nanocomposite materials is applied in the fields of material preparation and electrochemical analysis, which can solve the problems of low sensitivity and high detection limit, and achieve the effects of high sensitivity, low detection limit and strong anti-interference performance.

Active Publication Date: 2020-10-09
HENGYANG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The primary technical problem to be solved by the present invention is to provide a sea urchin-type Prussian for preparing a modified electrode for detecting guanine in order to overcome the problems of high detection limit and low sensitivity of the modified electrode used for detecting guanine in the prior art. Nitrogen-doped graphene nanocomposites supported by blue-palladium core-shell structure

Method used

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  • Sea urchin-type Prussian blue-palladium core-shell structure loaded nitrogen-doped graphene nanocomposites and its prepared electrodes and applications
  • Sea urchin-type Prussian blue-palladium core-shell structure loaded nitrogen-doped graphene nanocomposites and its prepared electrodes and applications
  • Sea urchin-type Prussian blue-palladium core-shell structure loaded nitrogen-doped graphene nanocomposites and its prepared electrodes and applications

Examples

Experimental program
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Effect test

Embodiment 1

[0044] Example 1 Preparation of sea urchin type Prussian blue-palladium core-shell structure loaded nitrogen-doped graphene nanocomposite

[0045] S11. Add 0.016g K 3 Fe(CN) 6 Add it to a mixed solution consisting of 2.5mL concentrated hydrochloric acid, 2.5mL deionized water and 12.5 mL DMF, and magnetically stir to dissolve;

[0046] S12. Put the above solution into a hydrothermal reaction kettle and place it in an oven at 80°C for 24 hours, then let it stand for 12 hours and centrifuge, wash and dry to obtain Prussian blue;

[0047] S13. Take 2 mg of Prussian blue and add it to 2 mg of water, after ultrasonic dispersion, add 2 mL of PdCl dropwise within 30 min under magnetic stirring 2 solution (1mg / mL) and NaBH 4 solution (1mg / mL); then stand still for 1h and then centrifuge and wash to obtain the sea urchin-type Prussian blue-palladium core-shell structure material;

[0048] S14. Take the prepared Prussian blue-palladium core-shell structure material and disperse it i...

Embodiment 2

[0051] Example 2 Preparation of sea urchin-type Prussian blue-palladium core-shell structure loaded nitrogen-doped graphene nanocomposite modified electrode

[0052] S21. Take a glassy carbon electrode with a diameter of 3 mm, firstly grind it on the aluminum powder with a particle size of 0.3 μm for 8 minutes, then grind it on the aluminum powder of 0.05 μm for 8 minutes, and then wash it ultrasonically with dilute nitric acid, acetone and deionized water respectively , to obtain a pretreated glassy carbon electrode after drying;

[0053] S22. The sea urchin-type Prussian blue-palladium core-shell structure-loaded nitrogen-doped graphene nanocomposite material described in embodiment 1 was dispersed with DMF ultrasonically for 10min to obtain a 1mg / mL dispersion;

[0054] S23. Take 6.0 μL of the dispersion liquid and add it dropwise on the surface of the pretreated glassy carbon electrode, and after drying, the sea urchin-type Prussian blue-palladium core-shell structure-supp...

Embodiment 3

[0055] Example 3 Detection performance of sea urchin-type Prussian blue-palladium core-shell structure-loaded nitrogen-doped graphene composite membrane modified electrode

[0056] In this example, the sea urchin-type Prussian blue-palladium core-shell structure-supported nitrogen-doped graphene composite film modified electrode prepared in Example 2 was used as the experimental object, and it was combined with a platinum auxiliary electrode and an SCE reference electrode to form a three-electrode system. Connected to CHI660 electrochemical workstation (Shanghai Chenhua Instrument Co., Ltd.) for electrochemical performance testing.

[0057] (1) Characterization of electrochemical performance of different electrodes

[0058] with K 3 [Fe(CN) 6] as a probe to investigate the electrochemical performance of different modified electrodes by cyclic voltammetry. Fig. 3A shows that the probe ions on glassy carbon electrode (a), nitrogen-doped graphene modified glassy carbon electro...

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Abstract

The invention discloses a sea urchin-type Prussian blue-palladium core-shell structure supported nitrogen-doped graphene nanocomposite material and a prepared electrode and application thereof. The preparation method of the material comprises the following steps: S11. adding K3Fe(CN)6 to a mixed solution and dissolving by magnetic stirring; S12. putting the above solution into a hydrothermal reaction kettle and placing the hydrothermal reaction kettle in an oven to perform a reaction to obtain the Prussian blue; S13. adding the Prussian blue into water, uniformly dispersing by ultrasonic waves, and respectively adding PdCl 2 solution and NaBH 4 solution dropwise under magnetic stirring to obtain a sea urchin-type Prussian blue-palladium core-shell structure material; S14, preparing the obtained sea urchin-type Prussian blue-palladium core-shell structure material into a dispersion liquid in DMF, mixing with a nitrogen-doped graphene dispersion liquid by the ultrasonic waves, and centrifugally drying to obtain the material. The electrode prepared from the material can be used for quantitatively detecting the content of guanine in human urine and rabbit serum, and has the advantagesof being wide in detection range, high in sensitivity, low in detection limit, good in stability, high in anti-interference performance and the like.

Description

technical field [0001] The invention relates to the technical fields of material preparation and electrochemical analysis, in particular to a sea urchin-type Prussian blue-palladium core-shell structure-supported nitrogen-doped graphene nanocomposite material, an electrode prepared therefrom, and an application thereof. Background technique [0002] Guanine is an important purine group that constitutes the basic component of DNA structure. It participates in various processes such as energy transduction, metabolic cofactors and cell signaling in organisms, and plays an important role in genetic and metabolic processes. Abnormal changes in the concentration of guanine in the organism indicate a defect in the immune system. Therefore, the quantitative detection of guanine in organisms can play an important role in the fields of clinical diagnosis, disease treatment and scientific research. The current assay methods for guanine detection include high performance liquid chromat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/327
CPCG01N27/3275
Inventor 李俊华贺灵芝刘梦琴许志锋刘兴欧亚平
Owner HENGYANG NORMAL UNIV
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