CN106841355B - PtNi nano alloy electrochemical sensor for detecting dopamine - Google Patents
PtNi nano alloy electrochemical sensor for detecting dopamine Download PDFInfo
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- CN106841355B CN106841355B CN201710196635.7A CN201710196635A CN106841355B CN 106841355 B CN106841355 B CN 106841355B CN 201710196635 A CN201710196635 A CN 201710196635A CN 106841355 B CN106841355 B CN 106841355B
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Abstract
The invention discloses a PtNi nano alloy electrochemical sensor for detecting dopamine, which is characterized in that: and (3) coating 4-5 microliters of binary PtNi nanocrystalline ethanol solution on the glassy carbon electrode to form a modified electrode PtNi/GCE, simultaneously using a silver-silver chloride electrode and a platinum sheet electrode as a three-electrode system, and directly detecting dopamine by using an electrochemical workstation. The electrochemical sensor has special sensitivity and stability to dopamine, and has lower detection limit, wider detection range and excellent anti-interference performance.
Description
Technical Field
The invention relates to a detection application of a PtNi alloy electrochemical sensor to dopamine.
Background
PtNi nanoalloys are mainly used in alcohol oxidation, nitrogen fixation, biomass fuel and liquid fuel cells, etc., however, ptNi nanoalloys are rarely used in electrochemical sensors. Dopamine is a neuro-conducting substance that is secreted by the brain and is used to assist cells in delivering impulses. This brain endocrine is mainly responsible for the brain's feelings, and the sensation will excite and happy information transfer, also related to addiction. The general steps for detecting dopamine are complicated, the manufacturing process of the sensor is complex, and a test sample needs to be preprocessed before testing.
Disclosure of Invention
The invention aims to solve the technical problems that: the flower-shaped binary PtNi nanocrystals are novel in structure, uniform in morphology and excellent in electrochemical sensor performance. The flower-shaped binary PtNi nanocrystals are made into modified electrodes PtNi/GCE, and simultaneously, silver-silver chloride electrodes and platinum sheet electrodes are used as a three-electrode system, and an electrochemical workstation is used for directly detecting dopamine.
The technical scheme of the invention is as follows:
a PtNi nano alloy electrochemical sensor for detecting dopamine adopts binary PtNi nano crystal material, wherein the nano crystal structure consists of small particles of sub-5.0 nm, and has a flower-like structure and surface defect-rich active sites.
The preparation method of the PtNi nano alloy electrochemical sensor for detecting dopamine comprises the following synthesis steps of (1) adding sodium chloride and PVP into dimethylacetamide together, and stirring for 5-8 minutes at room temperature, wherein the mass ratio of the sodium chloride to the PVP is 1:2-1:5; the added dimethylacetamide amount needs to completely dissolve sodium chloride and PVP; (2) Adding metal platinum salt and nickel salt precursors into the mixed solution obtained in the step (1), wherein the concentration of the metal salt precursors is 0.05-0.5 mol/L; stirring for 3-5 minutes at room temperature; (3) Adding PVP into the mixed solution obtained in the step (2), and stirring for 10-30 minutes at room temperature, wherein the mass ratio of sodium chloride to PVP is 1:5-1:8; (4) Transferring the mixed solution obtained in the step (3) into a high-pressure reaction kettle for reaction for 2-12 hours, and controlling the temperature at 150-200 ℃; (5) And (3) cooling the product obtained in the step (4), washing, and centrifugally separating to obtain the binary PtNi nanocrystals.
The metal platinum salt and nickel salt precursors are platinum acetylacetonate and nickel acetylacetonate precursors respectively.
According to the application method of the binary PtNi nanocrystals in the electrochemical sensor for detecting dopamine, a binary PtNi nanocrystal ethanol solution is coated on a glassy carbon electrode to form a modified electrode PtNi/GCE, and meanwhile, a silver chloride electrode and a platinum sheet electrode are used as a three-electrode system to directly detect the dopamine through an electrochemical workstation.
The invention has the beneficial effects that: the invention synthesizes a flower-shaped binary PtNi nano crystal and is used for detecting an electrochemical sensor of dopamine. And the PtNi nanocrystals can not only enhance the sensitivity of the electrochemical sensor, but also greatly enhance the stability of the electrochemical sensor due to the special properties of the PtNi nanocrystals. The bright point of the invention is that the prepared PtNi nano alloy electrochemical sensor has lower detection limit, wider linear detection range and excellent anti-interference performance, especially the detection limit of dopamine can be as low as 10nM, and the electrochemical dopamine sensor is the electrochemical dopamine sensor with the lowest detection limit for actually detecting dopamine in the literature reported at present. Meanwhile, the dopamine can be directly detected, and complicated pretreatment steps are reduced.
The electrochemical sensor has special sensitivity and stability to dopamine, has a detection limit of 0.03 mu M, a linear detection range of 0.08-250 mu M and excellent anti-interference performance.
Drawings
FIG. 1 is a view of the results of observation of binary PtNi nanocrystals by a transmission electron microscope;
FIG. 2 is an XRD spectrum of a binary PtNi nano alloy;
FIG. 3 is a linear scan of a binary PtNi nano alloy;
FIG. 4 is a graph showing dopamine sensing performance test of PtNi nano alloy electrochemical sensor;
fig. 5 is an anti-interference test chart of the PtNi nano alloy electrochemical sensor.
Detailed Description
Example 1
The synthesis method of the flower-like binary PtNi nanocrystals comprises the following synthesis steps of (1) adding sodium chloride and PVP into dimethylacetamide together, and stirring for 5 minutes at room temperature, wherein the mass ratio of the sodium chloride to the PVP is 1:2; the added dimethylacetamide amount needs to completely dissolve sodium chloride and PVP; (2) Adding platinum acetylacetonate and nickel acetylacetonate precursor into the mixed solution obtained in the step (1), wherein the concentration of the metal salt precursor is 0.1mol/L; stirring for 3-5 minutes at room temperature; (3) Adding PVP into the mixed solution obtained in the step (2), and stirring for 10-30 minutes at room temperature, wherein the mass ratio of sodium chloride to PVP is 1:5; (4) Transferring the mixed solution obtained in the step (3) into a high-pressure reaction kettle for reaction for 6 hours, and controlling the temperature at 180 ℃; (5) And (3) cooling the product obtained in the step (4), washing, and centrifugally separating to obtain the binary PtNi nanocrystals.
Example 2
The synthesis method of the flower-like binary PtNi nanocrystals comprises the following synthesis steps of (1) adding sodium chloride and PVP into dimethylacetamide together, and stirring for 6 minutes at room temperature, wherein the mass ratio of the sodium chloride to the PVP is 1:5; the added dimethylacetamide amount needs to completely dissolve sodium chloride and PVP; (2) Adding platinum acetylacetonate and nickel acetylacetonate precursor into the mixed solution obtained in the step (1), wherein the concentration of the metal salt precursor is 0.5mol/L; stirring for 3-5 minutes at room temperature; (3) Adding PVP into the mixed solution obtained in the step (2), and stirring for 10-30 minutes at room temperature, wherein the mass ratio of sodium chloride to PVP is 1:7; (4) Transferring the mixed solution obtained in the step (3) into a high-pressure reaction kettle for reaction for 10 hours, and controlling the temperature at 150 ℃; (5) And (3) cooling the product obtained in the step (4), washing, and centrifugally separating to obtain the binary PtNi nanocrystals.
Example 3
The synthesis method of the flower-like binary PtNi nanocrystals comprises the following synthesis steps of (1) adding sodium chloride and PVP into dimethylacetamide together, and stirring for 8 minutes at room temperature, wherein the mass ratio of the sodium chloride to the PVP is 1:4; the added dimethylacetamide amount needs to completely dissolve sodium chloride and PVP; (2) Adding platinum acetylacetonate and nickel acetylacetonate precursor into the mixed solution obtained in the step (1), wherein the concentration of the metal salt precursor is 0.3mol/L; stirring for 3-5 minutes at room temperature; (3) Adding PVP into the mixed solution obtained in the step (2), and stirring for 10-30 minutes at room temperature, wherein the mass ratio of sodium chloride to PVP is 1:8; (4) Transferring the mixed solution obtained in the step (3) into a high-pressure reaction kettle for reaction for 2-12 hours, and controlling the temperature at 200 ℃; (5) And (3) cooling the product obtained in the step (4), washing, and centrifugally separating to obtain the binary PtNi nanocrystals.
Example 4
The synthesis method of the flower-like binary PtNi nanocrystals comprises the following synthesis steps of (1) adding sodium chloride and PVP into dimethylacetamide together, and stirring for 8 minutes at room temperature, wherein the mass ratio of the sodium chloride to the PVP is 1:4; the added dimethylacetamide amount needs to completely dissolve sodium chloride and PVP; (2) Adding platinum acetylacetonate and nickel acetylacetonate precursor into the mixed solution obtained in the step (1), wherein the concentration of the metal salt precursor is 0.5mol/L; stirring for 3-5 minutes at room temperature; (3) Adding PVP into the mixed solution obtained in the step (2), and stirring for 10-30 minutes at room temperature, wherein the mass ratio of sodium chloride to PVP is 1:6; (4) Transferring the mixed solution obtained in the step (3) into a high-pressure reaction kettle for reaction for 12 hours, and controlling the temperature at 150 ℃; (5) And (3) cooling the product obtained in the step (4), washing, and centrifugally separating to obtain the binary PtNi nanocrystals.
And 5 microliters of binary PtNi nanocrystalline solution is absorbed by a pipette and coated on a glassy carbon electrode, the modified electrode PtNi/GCE is formed after ethanol volatilizes, meanwhile, a silver chloride electrode and a platinum sheet electrode are used as a three-electrode system, and an electrochemical workstation is used for directly detecting dopamine.
The three-electrode system is inserted into a blank buffer solution, dopamine is added according to a certain concentration variation, and a series of concentration gradient dopamine test patterns (as shown in figure 4) are obtained through electrochemical workstation testing.
And inserting the three-electrode system into a solution sample to be detected, measuring a current value through the measurement of the electrochemical workstation on the current change, and comparing the current value with a standard result to obtain the concentration of the dopamine.
The present invention utilizes binary PtNi nanocrystals (derived from FIG. 1) with flower-like structures that are surface rich in defect sites. The PtNi/GCE formed by the method uses a silver-silver chloride electrode and a platinum sheet electrode as a three-electrode system, and an electrochemical workstation is used for detecting dopamine. The electrochemical sensor has special sensitivity and stability to dopamine, and has lower detection limit, wider linear detection range and excellent anti-interference performance.
Claims (2)
1. A PtNi nano-alloy electrochemical sensor for detecting dopamine, characterized in that: the binary PtNi nano crystal material is adopted, the nano crystal structure is composed of small particles of sub-5.0 nm, and the nano crystal material has a flower-like structure and a surface rich in defect active sites; adding sodium chloride and PVP into dimethylacetamide together, stirring for 5-8 minutes at room temperature, wherein the mass ratio of the sodium chloride to the PVP is 1:2-1:5; the added dimethylacetamide amount needs to completely dissolve sodium chloride and PVP; (2) Adding platinum acetylacetonate and nickel acetylacetonate precursor into the mixed solution obtained in the step (1), wherein the concentration of the metal salt precursor is 0.05-0.5 mol/L; stirring for 3-5 minutes at room temperature; (3) Adding PVP into the mixed solution obtained in the step (2), and stirring for 10-30 minutes at room temperature, wherein the mass ratio of sodium chloride to PVP is 1:5-1:8; (4) Transferring the mixed solution obtained in the step (3) into a high-pressure reaction kettle for reaction for 2-12 hours, and controlling the temperature at 150-200 ℃; (5) And (3) cooling the product obtained in the step (4), washing, and centrifugally separating to obtain the binary PtNi nanocrystals.
2. An application method of a PtNi nano alloy electrochemical sensor for detecting dopamine according to claim 1, wherein: the binary PtNi nano-crystalline ethanol solution is coated on a glassy carbon electrode GCE to form a modified electrode PtNi/GCE, and meanwhile, a silver-silver chloride electrode and a platinum sheet electrode are used as a three-electrode system, and the dopamine is directly detected through an electrochemical workstation.
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