Graphite phase nitrogen carbide-chitosan modified electrode, preparation method thereof, and method using same as work electrode to detect protocatechuic acid

A technology for modifying electrodes and protocatechuic acid, which is applied in the direction of material electrochemical variables, etc., to achieve the effects of short time consumption, high sensitivity and good selectivity

Inactive Publication Date: 2016-10-26
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

As a simple phenolic acid, protocatechuic acid not only has good oxidative properties, but also has anti-inflammatory and hypoglycemic effects, which protects human nerve activity to a certain extent, but when the intake is too much, the Poisoning symptoms such as lack of energy and shortness of breath

Method used

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  • Graphite phase nitrogen carbide-chitosan modified electrode, preparation method thereof, and method using same as work electrode to detect protocatechuic acid
  • Graphite phase nitrogen carbide-chitosan modified electrode, preparation method thereof, and method using same as work electrode to detect protocatechuic acid
  • Graphite phase nitrogen carbide-chitosan modified electrode, preparation method thereof, and method using same as work electrode to detect protocatechuic acid

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Experimental program
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Effect test

Embodiment 1

[0034] (1) Graphite phase nitrogen carbide nanosheets (g-C 3 N 4 ) solution preparation

[0035] Directly roast 4g of melamine in a muffle furnace at 520°C for 4.0h, cool and grind to obtain g-C 3 N 4 Powder, weigh 0.1g of g-C 3 N 4 The powder was dissolved in 10mL aqueous solution, diluted with water to 1mg / mL, ultrasonicated for 10h, and g-C was obtained by liquid phase exfoliation 3 N 4 nanosheet solution.

[0036] (2) Preparation of graphitic nitrogen carbide-chitosan modified electrode

[0037] The glassy carbon electrode (GCE) is sequentially used with 0.3 and 0.05 μm α-A1 2 o 3 Polish until it becomes a mirror surface. After each polishing, first wash off the surface dirt, then use absolute ethanol to sonicate for 5 minutes, and finally wash with distilled water, repeat three times, and finally dry naturally at room temperature; take the g-C prepared in step (1) 3 N 4 Sonicate the solution to form a uniformly dispersed suspension, and pipette 4 μL of g-C 3 N...

Embodiment 2

[0040] Using cyclic voltammetry (CV), graphite-phase nitrogen carbide-chitosan modified electrodes (g-C 3 N 4 / CS modified electrode), glassy carbon electrode, PEDOT / g-C 3 N 4 / CS modified electrode and GR-COOH / CS modified electrode are working electrodes, in which PEDOT is prepared from EDOT and PSS, both EDOT and PSS are purchased from Shanghai Dibai Chemicals Co., Ltd. g-C prepared in Example 1 3 N 4 / CS modified electrode surface to prepare PEDOT / g-C 3 N 4 / CS modified electrode; carboxylated graphene was directly purchased from Nanjing Xianfeng Nano Material Technology Co., Ltd. In the experiment, 5 μL of 1 mg / mL carboxylated graphene aqueous solution and chitosan acetic acid solution were drip-coated on the surface of the glassy carbon electrode. GR-COOH / CS modified electrode.

[0041] In 1mmol / L [Fe(CN) containing 0.1mol / L KCl 6 ] 3- / 4- Scan the cyclic voltammetry curve in the mixed aqueous solution of (1:1), the potential scanning range is -0.2~0.6V, and the s...

Embodiment 3

[0043] Electrochemical impedance spectroscopy (EIS) was used to measure g-C 3 N 4 / CS modified electrode, glassy carbon electrode, PEDOT / g-C 3 N 4 / CS modified electrode and GR-COOH / CS modified electrode were used as working electrodes, in 5mmol / L [Fe(CN) 6 ] 3- / 4- (1:1) scan the impedance value of each electrode in the solution, the initial potential is 0.2V, the scanning rate is 100mV / s, and the frequency range is 1~100000Hz, such as image 3 shown, since g-C 3 N 4 With a unique two-dimensional layered structure, it can improve the conductivity of the electrode and promote the electron transfer between the solution and the electrode interface, so g-C 3 N 4 The interfacial electron transfer resistance of / CS modified electrode is very small, compared with that, GR-COOH inhibits the [Fe(CN) 6 ] 3- / 4- The electron transfer between the redox probe and the electrode interface increases the boundary resistance of the GR-COOH / CS modified electrode.

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Abstract

The invention discloses a graphite phase nitrogen carbide-chitosan modified electrode, a preparation method thereof, and a method using the same as a work electrode to detect protocatechuic acid. The preparation method comprises the following steps: directly heating melamine to synthesize g-C3N4, preparing g-C3N4 nano sheets through liquid phase peeling, and then utilizing a self-assembling method to fix g-C3N4 and chitosan onto the surface of a glass-carbon electrode in sequence so as to construct a graphite phase nitrogen carbide-chitosan modified electrode. The detection method of protocatechuic acid comprises the following steps: utilizing the graphite phase nitrogen carbide-chitosan modified electrode as the work electrode, through a differential pulse voltammetry, and drawing a curve representing linear relationship between the corresponding current and the protocatechuic acid concentration so as to analyze the protocatechuic acid in the environment quantitatively and qualitatively. The provided electrode has good chemical responding to protocatechuic acid, has a strong anti-interference performance, and can be used to detect an actual sample. The detection method has the advantages of simple operation, short time, little using amount, and low cost, and a novel thinking is provided for the detection of phenolic acids.

Description

technical field [0001] The invention relates to an electrode material and its preparation method and application, in particular to a graphite phase nitrogen carbide-chitosan modified electrode and its preparation method and a method for detecting protocatechuic acid as a working electrode. Background technique [0002] Nowadays, with the continuous development of society and the continuous improvement of people's living standards, the incidence of cancer is also increasing. Therefore, the problem of cancer has attracted more and more attention. At the same time, the prevention and treatment of cancer have also aroused heated discussions among the public. . Epidemiological studies have shown that the incidence of cancer in a country is directly proportional to its consumption of fruits and vegetables. Phenolic acid compounds are organic acids containing phenolic rings, which are found in vegetables, fruits and nuts, and have good antioxidant activity. As a simple phenolic a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/30G01N27/48
CPCG01N27/30G01N27/48
Inventor 杨小弟景丽君李彩红
Owner NANJING NORMAL UNIVERSITY
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