CN110514725B - Fe-PANI-based dopamine electrochemical sensing electrode and preparation thereof - Google Patents

Fe-PANI-based dopamine electrochemical sensing electrode and preparation thereof Download PDF

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CN110514725B
CN110514725B CN201910687668.0A CN201910687668A CN110514725B CN 110514725 B CN110514725 B CN 110514725B CN 201910687668 A CN201910687668 A CN 201910687668A CN 110514725 B CN110514725 B CN 110514725B
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林玲玲
游东宏
应少明
黄仁昆
李武连
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Ningde Normal University
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Abstract

The invention provides a dopamine electrochemical sensing electrode based on an iron-doped polyaniline (Fe-PANI) nano material and a preparation method thereof, wherein the preparation method comprises the following steps: s1, adding aniline monomer into dichloromethane solution, and performing ultrasonic treatment to form organic phase solution; s2, sequentially and slowly adding an N-methylpyrrolidone aqueous solution and an iron chloride solution into the organic phase solution under the stirring condition, stirring at room temperature in a dark place for a period of time, and standing; s3, slowly adding an ammonium persulfate-hydrochloric acid solution into the reaction solution in the step S2, standing for reaction, and filtering with an organic filter membrane to obtain a solid product; s4, cleaning, filtering and naturally airing the solid product to obtain Fe-PANI powder; s5, grinding and polishing the glassy carbon electrode for later use; s6, taking Fe-PANI powder, ultrasonically dispersing the powder in absolute ethyl alcohol, adding a Nafion solution, and ultrasonically dispersing the powder to form a suspension; and S7, dropwise adding the suspension to the glassy carbon electrode polished in the step S5 to obtain the Fe-PANI modified electrode.

Description

Fe-PANI-based dopamine electrochemical sensing electrode and preparation thereof
Technical Field
The invention relates to a dopamine electrochemical sensing electrode based on iron-doped polyaniline and a preparation method thereof.
Background
Dopamine (DA) is a neurotransmitter that has important roles in the central nervous system, cardiovascular system, kidney system, and endocrine system, and affects the thinking, work, movement, and other behaviors of people in the human body. The normal content of dopamine in human body is 0.2-0.4g/ml, and when the content of dopamine in human body is too low, diseases such as schizophrenia, heart failure, Parkinson's disease, neuromuscular disorder and the like can be caused. On the contrary, excessive DA content can cause people to be excited and happy and is easy to addict. In addition, dopamine is also commonly used in medicine for the treatment of depression, renal failure, endotoxemia, and other diseases. Therefore, the method has important application value for diagnosing the diseases on a molecular level by selectively and highly sensitively detecting the concentration of the neurotransmitter dopamine, and has important significance for the research of neurophysiology and the quality control of related medicines.
Currently, common detection methods for dopamine include fluorescence spectrometry, college liquid phase method, capillary electrophoresis, colorimetric method, electrochemical analysis and detection method and the like. The electrochemical detection method has the advantages of easiness in operation, high sensitivity, good selectivity and the like, and becomes a common method for detecting dopamine. However, in addition to dopamine, Uric Acid (UA) and Ascorbic Acid (AA) are contained in brain and body fluid, and their oxidation potentials are very close to each other, so that the presence of uric acid and ascorbic acid in the detection system interferes with the measurement of dopamine. Therefore, how to effectively eliminate interference of uric acid and ascorbic acid on dopamine detection is an important research content of dopamine electrochemical sensing at present.
Disclosure of Invention
The invention provides a dopamine electrochemical sensing electrode based on iron-doped polyaniline, which can effectively solve the problems.
The invention is realized by the following steps:
the invention provides a preparation method of a dopamine electrochemical sensing electrode based on an iron-doped polyaniline nano material, which comprises the following steps:
s1, adding 0.5mL aniline monomer into 50mL dichloromethane solution, and performing ultrasonic treatment to uniformly disperse the aniline monomer to form transparent and uniform organic phase solution;
s2, adding 50mL of 0.2mol/L N-methylpyrrolidone aqueous solution and 0.05mL of 0.5mol/L ferric chloride solution into the organic phase solution in sequence under the stirring condition, stirring at room temperature in a dark place for a period of time, and standing;
s3, adding 0.3g of ammonium persulfate into 8.6mL of 2mol/L hydrochloric acid solution to form ammonium persulfate-hydrochloric acid solution, slowly adding the ammonium persulfate-hydrochloric acid solution into the reaction solution in the step S2, standing for reaction for a period of time, and filtering with an organic filter membrane to obtain a solid product;
s4, cleaning, filtering and naturally airing the solid product to obtain Fe-PANI powder;
s5, grinding and polishing the glassy carbon electrode by using alumina micro powder with the particle size of 3 microns, 1 micron, 0.3 micron and 50nm in sequence for later use;
s6, ultrasonically dispersing 1-3 mg of Fe-PANI powder into 0.5mL of absolute ethyl alcohol, and adding 5-15 mu L of Nafion solution for ultrasonic dispersion to form uniform suspension;
s7, dripping 10-40 mu L of suspension liquid 10-20 mu L/time on the surface of the glassy carbon electrode polished in the step S5, standing, continuing to drip the suspension liquid after the solution is volatilized, and repeating the operation to finally obtain the Fe-PANI modified electrode.
The invention also provides a dopamine electrochemical sensing electrode based on the iron-doped polyaniline nano material obtained by the method; the test environment is as follows: and (2) carrying out DPV test by using a Fe-PANI modified electrode as a working electrode, a graphite electrode or a platinum electrode as a counter electrode and a saturated calomel electrode as a reference electrode, wherein the potential range is-0.1V-0.9V (vs. SCE), the scanning amplitude is 50mV, the pulse width is 50ms, and the whole test environment is carried out in a phosphate buffer solution with the pH value of 6.6-7.2.
The invention has the beneficial effects that: the Fe-PANI modified electrode has better anti-interference capability on UA when used for detecting DA, and is not interfered by AA under the condition that the concentration of AA is lower than 1 mM; the detection limit was 0.005. mu.M for DA and 0.5. mu.M for UA. Therefore, the Fe-PANI modified electrode can simultaneously detect UA when detecting DA under the condition of not being interfered by AA.
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In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a DPV graph of 1mM UA, 2mM AA, 200. mu.M DA on a polyaniline-modified electrode in 0.1M pH 6.8 phosphate buffer.
FIG. 2 is a DPV graph of 1mM UA, 2mM AA, 200. mu.M DA on Fe-PANI modified electrodes in phosphate buffer at a concentration of 0.1M and pH 6.8.
FIG. 3 is a graph of DPV at a series of concentrations DA on Fe-PANI modified electrodes in phosphate buffer at a concentration of 0.1M and pH 6.8.
Fig. 4 is a graph of the linear relationship of DA concentration to peak current.
FIG. 5 is a graph of DPV at a series of UA concentrations on Fe-PANI modified electrodes in phosphate buffer at 0.1M pH 6.8.
Fig. 6 is a graph of UA concentration versus peak current linearity.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings of the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
In the description of the present invention, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
The embodiment of the invention provides a preparation method of a dopamine electrochemical sensing electrode based on an iron-doped polyaniline nano material, which comprises the following steps:
s1, adding 0.5mL aniline monomer into 50mL dichloromethane solution, and performing ultrasonic treatment to uniformly disperse the aniline monomer to form transparent and uniform organic phase solution;
s2, adding 50mL of 0.2mol/L N-methylpyrrolidone aqueous solution and 0.05mL of 0.5mol/L ferric chloride solution into the organic phase solution in sequence under the stirring condition, stirring at room temperature in a dark place for a period of time, and standing;
s3, adding 0.3g of ammonium persulfate into 8.6mL of 2mol/L hydrochloric acid solution to form ammonium persulfate-hydrochloric acid solution, slowly adding the ammonium persulfate-hydrochloric acid solution into the reaction solution in the step S2, standing for reaction for a period of time, and filtering with an organic filter membrane to obtain a solid product;
s4, cleaning, filtering and naturally airing the solid product to obtain Fe-PANI powder;
s5, grinding and polishing the glassy carbon electrode by using alumina micro powder with the particle size of 3 microns, 1 micron, 0.3 micron and 50nm in sequence for later use;
s6, ultrasonically dispersing 1-3 mg of Fe-PANI powder into 0.5mL of absolute ethyl alcohol, and adding 5-15 mu L of Nafion solution for ultrasonic dispersion to form uniform suspension;
s7, dripping 10-40 mu L of suspension liquid 10-20 mu L/time on the surface of the glassy carbon electrode polished in the step S5, standing, continuing to drip the suspension liquid after the solution is volatilized, and repeating the operation to finally obtain the Fe-PANI modified electrode.
The test environment of the Fe-PANI modified electrode is as follows: and (2) carrying out DPV test by using a Fe-PANI modified electrode as a working electrode, a graphite electrode or a platinum electrode as a counter electrode and a saturated calomel electrode as a reference electrode, wherein the potential range is-0.1V-0.9V (vs. SCE), the scanning amplitude is 50mV, the pulse width is 50ms, and the whole test environment is carried out in phosphate buffer solution with the pH value of 6.6-7.2. As a further improvement, in addition, the pH of the environment has a large influence on the test throughout the test, and when the pH is 6.6 to 7.2, the proton doping degree of polyaniline changes, thereby affecting the anti-interference property, sensitivity and stability of the detection substance, and therefore, it is preferable that the entire test environment is performed in a phosphate buffer at pH 6.8 to 7.2.
As a further improvement, in step S2, the mixed solution is protected from light for 10-50 h.
As a further improvement, in step S3, the reaction time is 15-35min after the ammonium persulfate-hydrochloric acid solution is added.
As a further modification, in step S4, the step of washing the solid product includes:
and S41, washing and cleaning the solid product by using distilled water, a hydrochloric acid solution and ethanol in sequence, wherein the concentration range of the hydrochloric acid solution is 0.1-2 mol/L. In step S41, the polyaniline maintains a certain conductivity and dispersibility by washing with a hydrochloric acid solution. However, the hydrochloric acid cleaning solution with high solubility can easily disperse polyaniline into a uniform solution, which affects the cleaning of the product and destroys the filter membrane layer. Therefore, it is more preferable that the concentration of the hydrochloric acid solution is in the range of 0.1 to 1.2 mol/L.
In a further improvement, in step S6, the step of ultrasonically dispersing 1 to 3mg of Fe-PANI powder in 0.5mL of absolute ethanol, and adding 5 to 15 μ L of Nafion solution to ultrasonically disperse the powder to form a uniform suspension includes:
s61, taking 2mg of Fe-PANI powder, ultrasonically dispersing the powder in 0.5mL of absolute ethyl alcohol, adding 10 mu L of Nafion solution, and ultrasonically dispersing the powder to form uniform suspension.
In step S7, as a further improvement, 10 to 40 μ L of the suspension is dropped onto the surface of the glassy carbon electrode polished in step S5 at a rate of 10 to 20 μ L per time, the step of continuing dropping the suspension after the solution is volatilized after standing, and the step of repeating the operation to finally obtain the Fe-PANI modified electrode comprises:
s71, directly dripping 20 mu L of suspension liquid on the surface of the glassy carbon electrode polished in the step S5, standing, and volatilizing the solution to obtain the Fe-PANI modified electrode.
Example 1:
50mL of methylene chloride was added to a round bottom flask, and 0.5mL of aniline monomer was added to the methylene chloride solution and uniformly dispersed by sonication to form a clear and homogeneous solution of the organic phase. Placing the obtained organic phase solution on a magnetic stirrer, sequentially and slowly adding 50mL of 0.2mol/L N-methyl pyrrolidone aqueous solution and 0.05mL of 0.5mol/L ferric chloride solution into the solution under the stirring condition, stirring the solution at room temperature in a dark place for 20 hours, and standing the solution. 0.3g of ammonium persulfate is weighed and dissolved in 8.6mL of 2mol/L hydrochloric acid solution, and the ammonium persulfate-hydrochloric acid solution is obtained after complete dissolution. Slowly adding ammonium persulfate-hydrochloric acid mixed solution into dichloromethane-N-methyl pyrrolidone reaction solution under a standing condition along the bottle wall of the round-bottom flask, standing for reacting for 20 minutes, filtering with an organic filter membrane with the aperture of 0.22 mu m to obtain a solid product, washing and cleaning the filtered product with distilled water, 1mol/L hydrochloric acid solution and ethanol in sequence, and naturally airing to obtain Fe-PANI powder. Grinding and polishing a glassy carbon electrode with the diameter of 5mm by using alumina micro powder with the diameter of 3 mu m, 1 mu m, 0.3 mu m and 50nm in sequence for later use. Ultrasonically dispersing 2mg of Fe-PANI powder into 0.5mL of absolute ethyl alcohol, and adding 10 mu L of Nafion solution for ultrasonic dispersion for 30min to form uniform suspension. And dripping 20 mu L of suspension liquid on the surface of the clean glassy carbon electrode, standing, and volatilizing the solution to obtain the Fe-PANI modified electrode for later use. And performing pulse voltammetry (DPV) test by using a Fe-PANI modified electrode as a working electrode, a graphite electrode as a counter electrode and a saturated calomel electrode as a reference electrode. Wherein the potential range is-0.1V-0.9V (vs. SCE), the scanning amplitude is 50mV, and the pulse width is 50 ms. The whole experiment was performed in the presence of phosphate buffered saline (0.1M PBS solution, pH 6.8).
Comparative example:
50mL of methylene chloride was added to a round bottom flask, and 0.5mL of aniline monomer was added to the methylene chloride solution and uniformly dispersed by sonication to form a clear and homogeneous solution of the organic phase. Placing the obtained organic phase solution on a magnetic stirrer, sequentially and slowly adding 50mL0.2mol/L of N-methylpyrrolidone aqueous solution into the solution under the stirring condition, stirring the solution at room temperature in a dark place for 20 hours, and standing the solution. 0.3g of ammonium persulfate is weighed and dissolved in 8.6mL of 2mol/L hydrochloric acid solution, and the ammonium persulfate-hydrochloric acid solution is obtained after complete dissolution. Slowly adding ammonium persulfate-hydrochloric acid mixed solution into dichloromethane-N-methyl pyrrolidone reaction solution under a standing condition along the bottle wall of the round-bottom flask, standing for reacting for 20 minutes, filtering with an organic filter membrane with the aperture of 0.22 mu m to obtain a solid product, washing and cleaning the filtered product with distilled water, 1mol/L hydrochloric acid solution and ethanol in sequence, and naturally airing to obtain PANI powder. Grinding and polishing a glassy carbon electrode with the diameter of 5mm by using alumina micro powder with the diameter of 3 mu m, 1 mu m, 0.3 mu m and 50nm in sequence for later use. Taking 2mg PANI powder, ultrasonically dispersing in 0.5mL absolute ethyl alcohol, adding 10 mu L Nafion solution, and ultrasonically dispersing for 30min to form uniform suspension. And dripping 20 mu L of suspension liquid on the surface of the clean glassy carbon electrode, standing, and volatilizing the solution to obtain the PANI electrode for later use. And (3) carrying out pulse voltammetry (DPV) test by using a PANI electrode as a working electrode, a graphite electrode as a counter electrode and a saturated glyco-co electrode as a reference electrode. Wherein the potential range is-0.1V-0.9V (vs. SCE), the scanning amplitude is 50mV, and the pulse width is 50 ms. The whole experiment was performed in the presence of phosphate buffered saline (0.1M PBS solution, pH 6.8).
Test example:
FIG. 1 is a DPV graph of 1mM UA, 2mM AA, 200. mu.M DA on a polyaniline-modified electrode in 0.1M pH 6.8 phosphate buffer. As can be seen from FIG. 1, the oxidation potential of DA is between 0.2V and 0.7V, and the peak potential is 0.27V; the oxidation potential of UA is between 0.3V and 0.7V, and the peak potential is 0.4V. Therefore, the electrochemical response signals of DA and UA are partially overlapped, i.e., the existence of UA can interfere with the detection of DA to a certain extent. In the system, AA has two oxidation peaks at the potentials of 0.1V-0.3V and 0.7V-0.85V, wherein the oxidation signal between 0.1V-0.3V has an influence on the detection of DA to a certain extent. Therefore, the polyaniline modified electrode is interfered by UA and AA to a certain extent in the process of detecting DA.
FIG. 2 is a DPV graph of 1mM UA, 2mM AA, 200. mu.M DA on Fe-PANI modified electrodes in phosphate buffer at a concentration of 0.1M and pH 6.8. As can be seen from FIG. 2, the oxidation potential of DA on the Fe-PANI modified electrode is between 0.15V and 0.4V, and the peak potential is 0.25V; the oxidation potential of UA is between 0.3V and 0.7V, and the peak potential is 0.38V; the peak potential of AA was 0.14V and the peak current was small. Because the overlapping degree of the DPV oxidation potential intervals of UA and DA is small, UA has small interference to DA signals when the DA signals are detected. Under the condition of high concentration of AA, certain signal overlapping still exists between the peak potentials of AA and UA, and certain interference exists in the detection of the UA by the AA. The detection limit of the Fe-PANI modified electrode on AA is 1mM, and when the concentration of AA is lower than 1mM, AA has no obvious electrochemical response behavior on the Fe-PANI modified electrode and has no obvious interference on the detection of DA.
FIG. 3 is a graph of DPV at a series of concentrations of DA on Fe-PANI modified electrodes in 0.1M phosphate buffer pH 6.8, where the oxidation potential of DA ranges from 0.15V to 0.45V, and the peak potential is 0.25V. As the DA concentration increased, the response current on the electrode also increased, with a detection limit of 0.005. mu.M.
Fig. 4 is a graph of the linear relationship of DA concentration to peak current. As can be seen from the graph, the concentration range detected herein is 0.005 μ M to 200 μ M, and there is a bilinear relationship between the DA concentration and the peak current. Linear curve at high concentration (10. mu.M-200. mu.M) is y10.06993x +2.57355, the correlation coefficient R20.983. At low concentrations (0.005. mu.M-10. mu.M) the linear curve is y20.27676x +0.48846, the correlation coefficient R2＝0.94948。
FIG. 5 is a DPV graph of UA at a series of concentrations on an Fe-PANI modified electrode in phosphate buffer at a concentration of 0.1M and pH 6.8, where the oxidation signal of UA is seen to have a potential range of 0.25V to 0.55V and a peak potential of 0.38V. As the UA concentration increases, the response current at the electrode also increases, with a detection limit of 0.5 μ M.
Fig. 6 is a graph of UA concentration versus peak current linearity. As can be seen from the figure, the concentration range detected herein is 0.1. mu.M-1 mM, and the UA concentration and the peak current exhibit a bilinear relationship. Linear curve at high concentration (50. mu.M-1 mM) is y10.0099x +0.97386, the correlation coefficient R20.99995. At low concentration (0.1. mu.M-50. mu.M) the linear curve is y20.02777x +0.09553, the correlation coefficient R2＝0.98998。
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (5)

1. A preparation method of a dopamine electrochemical sensing electrode based on an iron-doped polyaniline nano material is characterized by comprising the following steps:
s1, adding 0.5mL aniline monomer into 50mL dichloromethane solution, and performing ultrasonic treatment to uniformly disperse the aniline monomer to form transparent and uniform organic phase solution;
s2, slowly adding 50mL of 0.2mol/L N-methylpyrrolidone aqueous solution and 0.05mL of 0.5mol/L ferric chloride solution into the organic phase solution under the stirring condition to obtain a mixed solution, stirring at room temperature in a dark place for a period of time, and standing;
s3, adding 0.3g of ammonium persulfate into 8.6mL of 2mol/L hydrochloric acid solution to form ammonium persulfate-hydrochloric acid solution, slowly adding the ammonium persulfate-hydrochloric acid solution into the reaction solution in the step S2, standing for reaction for a period of time, and filtering with an organic filter membrane to obtain a solid product;
s4, cleaning, filtering and naturally airing the solid product to obtain Fe-PANI powder;
s5, grinding and polishing the glassy carbon electrode by using alumina micro powder with the particle size of 3 microns, 1 micron, 0.3 micron and 50nm in sequence for later use;
s6, ultrasonically dispersing 1-3 mg of Fe-PANI powder into 0.5mL of absolute ethyl alcohol, and adding 5-15 mu L of Nafion solution for ultrasonic dispersion to form uniform suspension;
s7, dripping 10-40 mu L of suspension liquid 10-20 mu L/time on the surface of the glassy carbon electrode polished in the step S5, standing, continuing to drip the suspension liquid after the solution is volatilized, and repeating the operation to finally obtain the Fe-PANI modified electrode;
in step S2, the mixed solution is kept away from light for 10-50 h;
in step S3, ammonium persulfate-hydrochloric acid solution is added and then the mixture is kept stand for reaction for 15-35 min.
2. The method of claim 1, wherein the step of washing the solid product in step S4 comprises:
and S41, washing and cleaning the solid product by using distilled water, a hydrochloric acid solution and ethanol in sequence, wherein the concentration range of the hydrochloric acid solution is 0.1-2 mol/L.
3. The method of claim 1, wherein in step S6, the step of taking 1-3 mg of Fe-PANI powder and ultrasonically dispersing in 0.5mL of absolute ethanol, and adding 5-15 μ L of Nafion solution to ultrasonically disperse to form a uniform suspension comprises:
s61, taking 2mg of Fe-PANI powder, ultrasonically dispersing the powder in 0.5mL of absolute ethyl alcohol, adding 10 mu L of Nafion solution, and ultrasonically dispersing the powder to form uniform suspension.
4. The method of claim 1, wherein in step S7, 10-40 μ L of the suspension is dropped onto the polished glassy carbon electrode surface in step S5 by 10-20 μ L/time, and the suspension is dropped continuously after the solution is volatilized, and the step of repeating the operation to obtain the Fe-PANI modified electrode comprises:
s71, directly dripping 20 mu L of suspension liquid on the surface of the glassy carbon electrode polished in the step S5, standing, and volatilizing the solution to obtain the Fe-PANI modified electrode.
5. A dopamine electrochemical sensing electrode based on an iron-doped polyaniline nanomaterial, which is characterized in that the dopamine electrochemical sensing electrode is prepared by the method of any one of claims 1 to 4; the test environment is as follows: and (3) carrying out DPV test by using a Fe-PANI modified electrode as a working electrode, a graphite electrode or a platinum electrode as a counter electrode and a saturated calomel electrode as a reference electrode, wherein the potential range is-0.1V-0.9 Vvs.SCE, the scanning amplitude is 50mV, the pulse width is 50ms, and the whole test environment is carried out in a phosphate buffer solution with the pH = 6.6-7.2.
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