CN111103340A - Preparation method and application of glassy carbon electrode modified by nano particles - Google Patents
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Abstract
The invention discloses a preparation method of a glassy carbon electrode modified by nano particles and application of the electrode in electrochemical detection of riboflavin. The detection method of the invention deposits platinum nano particles on the surface of a glassy carbon electrode in chloroplatinic acid solution by cyclic voltammetry, and synthesizes MoS by hydrothermal synthesis2Nano material of MoS2Modifying the surface of a glassy carbon electrode modified by platinum nanoparticles by using a nano material, and performing electrochemical polymerization on the surface of the glassy carbon electrode modified by the platinum nanoparticles2Electrically depositing polythiophene on the surface of the nano material to obtain polythiophene/MoS2The glass carbon electrode is modified by nano materials/platinum nano particles. The differential pulse voltammetry is adopted to detect the riboflavin, the linear range is wide, the sensitivity is high, the electrode can be used for many times, and the operation is convenient.
Description
Technical Field
The invention relates to the technical field of electrochemical analysis, in particular to a preparation method of a nano particle modified glassy carbon electrode and application of the nano particle modified glassy carbon electrode to the electrochemical detection of riboflavin.
Background
Riboflavin, also known as vitamin B2, is sparingly soluble in water, is stable when heated in neutral or acidic solutions, is a component of the prosthetic group of enzymes in the body (xanthases exert their hydrogen-transferring action in biological redox), and in the absence of this, affects biological oxidation of the body and prevents metabolism. The pathological changes are mostly shown as inflammation of the mouth, eyes and external genitalia, such as angular cheilitis, glossitis, conjunctivitis, scrotitis and the like, so the riboflavin can be used for preventing and treating the diseases.
In the prior art, the detection method of riboflavin mainly adopts HPLC combined with ultraviolet detection, for example, Licaixia et al adopts C18 column, uses 0.005 mol.L-1 sodium heptanesulfonate solution (containing 0.5% glacial acetic acid and 0.05% triethylamine) -methanol (65:35, v: v) as mobile phase, and has flow rate of 1.0m L min-1And the ultraviolet detection wavelength is 280nm, and the contents of vitamin B1, vitamin B2 and vitamin B6 in the vitamin B tablets are detected. (Li Caixia et al, strait pharmacology, 6 th 2017).
However, the HPLC method requires a complicated pretreatment step, requires expensive equipment, and requires a complicated detection process. Compared with HPLC method, the electrochemical analysis method has the advantages of good selectivity, high sensitivity, less time consumption, low detection limit, fast response speed and the like, and does not need expensive instruments. Based on polythiophene/MoS2The method for detecting riboflavin by using the glass carbon electrode modified by the nano material/platinum nanoparticles is not reported.
Disclosure of Invention
The invention aims to solve the problems of complex process, long time consumption and the like of riboflavin analysis by methods such as HPLC (high performance liquid chromatography) and the like, and provides a preparation method of a nano particle modified glassy carbon electrode, which can be used for rapidly detecting riboflavin in a solution by applying the glassy carbon electrode to the electrochemical detection of riboflavin, and has the advantages of wide linear range, high sensitivity, repeated use of the electrode and convenient operation.
The purpose of the invention is realized as follows:
(1) pretreating a glassy carbon electrode: sequentially placing a glassy carbon electrode on polishing cloth containing polishing powder with the particle sizes of 1 mu m, 0.3 mu m and 0.05 mu m to polish the glassy carbon electrode to a mirror surface, sequentially placing the glassy carbon electrode in acetone, a sulfuric acid solution with the concentration of 0.5mol/L and ultrapure water to perform ultrasonic treatment for 1 minute, and washing the glassy carbon electrode with the ultrapure water for 1 minute after each ultrasonic treatment to obtain a pretreated glassy carbon electrode;
(2) preparing a platinum nanoparticle modified glassy carbon electrode: placing the pretreated glassy carbon electrode in a hydrogen-containing atmosphere2PtCl6(100mM) potential sweep range-0.8Performing electrodeposition of platinum nanoparticles by cyclic voltammetry at V-0V, washing with ethanol and deionized water after the electrodeposition is finished, and drying under an infrared lamp to obtain a platinum nanoparticle modified glassy carbon electrode;
(3)MoS2preparing a nano material: 0.7mmol (NH)4)6Mo7O24·4H2Dissolving O in 20mL of deionized water by ultrasonic waves, slowly adding 10mg of surfactant-citric acid monohydrate under the condition of magnetic stirring, and continuously stirring for 30min to uniformly mix to obtain a solution A; then, adding 10mmol of thiourea into 20mL of deionized water, and carrying out ultrasonic dissolution to obtain a solution B; slowly dripping the solution B into the solution A under the conditions of room temperature and vigorous stirring, continuously stirring for 1 hour after dripping is finished, transferring the mixed solution into a high-pressure reaction kettle for hydrothermal reaction at the temperature of 180 ℃ and 200 ℃ for 20-24 hours, naturally cooling to room temperature after the reaction is finished, filtering to obtain a solid product, washing the obtained solid product with ethanol and carbon disulfide for a plurality of times, placing the product in a vacuum drying box for drying at the temperature of 50 ℃ overnight to obtain MoS2A nanomaterial; the electron microscope analysis result shows that the molybdenum sulfide nano material has a porous spherical shape.
(4) The obtained MoS2Dispersing 200-300mg of the nano material in 20mL of deionized water containing 0.5% of Nafion by ultrasonic for 5min, dripping 20 mu L of the nano material on the surface of the glassy carbon electrode modified by the platinum nano particles obtained in the step (2), and airing to obtain MoS2Modifying the glassy carbon electrode by the nano material/platinum nano particles;
(5) with the MoS2The nano material/platinum nano particle modified glassy carbon electrode is used as a working electrode, the platinum electrode is used as a counter electrode, Ag/AgCl is used as a reference electrode to form a three-electrode system, the three-electrode system is placed in an aqueous solution containing thiophene monomers, electrochemical polymerization is carried out by cyclic voltammetry, polythiophene is modified on the working electrode, and polythiophene/MoS is obtained2The glass carbon electrode is modified by nano materials/platinum nano particles.
Further, the concentration of the chloroplatinic acid solution in the step (2) is 200 mM.
Further, the potential scanning range of the electrochemical deposition in the step (2) is-0.8V-0V.
Further, the conditions of the hydrothermal reaction in the step (3) are as follows: carrying out hydrothermal reaction at 200 ℃ for 24 h.
Further, in the step (4), 300mgMoS is added2The nanomaterial was ultrasonically dispersed in 20mL of deionized water containing 0.5% Nafion.
The invention also provides polythiophene/MoS2Application of nano material/platinum nano particle modified glassy carbon electrode and polythiophene/MoS2The nano material/platinum nano particle modified glassy carbon electrode is prepared by adopting any one of the methods; the application is to mix polythiophene/MoS2The nano material/platinum nano particle modified glassy carbon electrode is applied to electrochemical detection of riboflavin.
Further, the step of electrochemically detecting riboflavin comprises:
a. preparing riboflavin aqueous solutions with different concentrations by adopting PBS buffer solution;
b. by using polythiophene/MoS2The nano material/platinum nano particle modified glassy carbon electrode is used as a working electrode, the platinum electrode is used as a counter electrode, Ag/AgCl is used as a reference electrode to form a three-electrode system, and the three-electrode system is placed in a riboflavin water solution;
c. carrying out electrochemical detection on riboflavin by adopting a differential pulse voltammetry method to obtain peak currents corresponding to riboflavin with different concentrations;
d. taking the peak current as a vertical coordinate and the concentration as a horizontal coordinate to make a standard curve;
e. and (3) placing the three-electrode system in the riboflavin aqueous solution with unknown concentration to obtain a differential pulse voltammetry curve and a peak current of the riboflavin aqueous solution with unknown concentration, and obtaining the riboflavin concentration according to a standard curve.
Further, the concentrations of the riboflavin aqueous solutions with different concentrations are respectively as follows: 1.0X 10-7mol/L，1.0×10-6mol/L，2.0×10-6mol/L，5.0×10-6mol/L，8.0×10-6mol/L，1.0×10-5mol/L。
Further, the electrochemical parameters of the differential pulse voltammetry are as follows: the scanning potential range is 0.5-1.0V, and the scanning speed is 100 mV/s.
Further, the detection limit of the differential pulse voltammetry for detecting the riboflavin is 6.0 multiplied by 10-8mol/L, linear range of 1.0X 10-7mol/L-8.0×10-6mol/L。
Compared with the prior art, the electrode prepared by the invention for detecting the riboflavin electrochemically has the advantages of simple equipment, convenient operation and short detection time compared with other methods for detecting the riboflavin; MoS formed as a result of the preparation according to the invention2The nano material has a porous spherical structure, and the platinum nanoparticles are modified on the electrode, so that excellent conductivity and extremely high specific surface area of the electrode are provided, and electrochemical polymerization of the polythiophene material can be formed in the porous spherical structure, so that the catalytic effect of the electrode is greatly improved, and the electrode prepared by the method has the advantages of high sensitivity, wide linear range and high accuracy when used for detecting riboflavin.
Drawings
FIG. 1 is a polythiophene/MoS2And detecting riboflavin by using the nano material/platinum nano particle modified glassy carbon electrode to obtain a peak current-concentration standard curve.
Detailed Description
The invention is further described with reference to the accompanying drawings, which are not intended to be limiting in any way, and any variations based on the teachings of the invention are intended to fall within the scope of the invention.
Example 1
(1) Pretreating a glassy carbon electrode: sequentially placing a glassy carbon electrode on polishing cloth containing polishing powder with the particle sizes of 1 mu m, 0.3 mu m and 0.05 mu m to polish the glassy carbon electrode to a mirror surface, sequentially placing the glassy carbon electrode in acetone, a sulfuric acid solution with the concentration of 0.5mol/L and ultrapure water to perform ultrasonic treatment for 1 minute, and washing the glassy carbon electrode with the ultrapure water for 1 minute after each ultrasonic treatment to obtain a pretreated glassy carbon electrode;
(2) preparing a platinum nanoparticle modified glassy carbon electrode: placing the pretreated glassy carbon electrode in a hydrogen-containing atmosphere2PtCl6Performing electrodeposition of platinum nanoparticles in (100mM) solution by cyclic voltammetry under potential scanning range of-0.8V-0V, washing with ethanol and deionized water after deposition, and drying under infrared lamp to obtain the final productModifying a glassy carbon electrode by using platinum nanoparticles;
(3)MoS2preparing a nano material: 0.7mmol (NH)4)6Mo7O24·4H2Dissolving O in 20mL of deionized water by ultrasonic waves, slowly adding 10mg of surfactant-citric acid monohydrate under the condition of magnetic stirring, and continuously stirring for 30min to uniformly mix to obtain a solution A; then, adding 10mmol of thiourea into 20mL of deionized water, and carrying out ultrasonic dissolution to obtain a solution B; slowly dropwise adding the solution B into the solution A under the conditions of room temperature and vigorous stirring, continuously stirring for 1 hour after dropwise adding is finished, transferring the mixed solution into a high-pressure reaction kettle for hydrothermal reaction at 180 ℃ for 20 hours, naturally cooling to room temperature after the reaction is finished, filtering to obtain a solid product, washing the obtained solid product with ethanol and carbon disulfide for a plurality of times, and drying the product in a vacuum drying oven at 50 ℃ overnight to obtain MoS2A nanomaterial; the electron microscope analysis result shows that the molybdenum sulfide nano material has a porous spherical shape.
(4) The obtained MoS2Ultrasonically dispersing 200mg of nano material in 20mL of deionized water containing 0.5% of Nafion for 5min, dropwise coating 20 mu L of nano material on the surface of the glassy carbon electrode modified by the platinum nano particles obtained in the step (2), and airing to obtain MoS2Modifying the glassy carbon electrode by the nano material/platinum nano particles;
(5) with the MoS2The nano material/platinum nano particle modified glassy carbon electrode is used as a working electrode, the platinum electrode is used as a counter electrode, Ag/AgCl is used as a reference electrode to form a three-electrode system, the three-electrode system is placed in aqueous solution containing thiophene monomers, electrochemical polymerization is carried out by cyclic voltammetry, the potential range is-1.0V to-0.5V, polythiophene is modified on the working electrode, and polythiophene/MoS is obtained2The glass carbon electrode is modified by nano materials/platinum nano particles.
Example 2
(1) Pretreating a glassy carbon electrode: sequentially placing a glassy carbon electrode on polishing cloth containing polishing powder with the particle sizes of 1 mu m, 0.3 mu m and 0.05 mu m to polish the glassy carbon electrode to a mirror surface, sequentially placing the glassy carbon electrode in acetone, a sulfuric acid solution with the concentration of 0.5mol/L and ultrapure water to perform ultrasonic treatment for 1 minute, and washing the glassy carbon electrode with the ultrapure water for 1 minute after each ultrasonic treatment to obtain a pretreated glassy carbon electrode;
(2) preparing a platinum nanoparticle modified glassy carbon electrode: placing the pretreated glassy carbon electrode in a hydrogen-containing atmosphere2PtCl6Performing electrodeposition of platinum nanoparticles in a (100mM) solution by cyclic voltammetry under a potential scanning range of-0.8V-0V, washing with ethanol and deionized water after the electrodeposition is finished, and drying under an infrared lamp to obtain a platinum nanoparticle modified glassy carbon electrode;
(3)MoS2preparing a nano material: 0.7mmol (NH)4)6Mo7O24·4H2Dissolving O in 20mL of deionized water by ultrasonic waves, slowly adding 10mg of surfactant-citric acid monohydrate under the condition of magnetic stirring, and continuously stirring for 30min to uniformly mix to obtain a solution A; then, adding 10mmol of thiourea into 20mL of deionized water, and carrying out ultrasonic dissolution to obtain a solution B; slowly dropwise adding the solution B into the solution A under the conditions of room temperature and vigorous stirring, continuously stirring for 1 hour after dropwise adding is finished, transferring the mixed solution into a high-pressure reaction kettle for hydrothermal reaction at 200 ℃ for 24 hours, naturally cooling to room temperature after the reaction is finished, filtering to obtain a solid product, washing the obtained solid product with ethanol and carbon disulfide for a plurality of times, and drying the product in a vacuum drying oven at 50 ℃ overnight to obtain MoS2A nanomaterial; the electron microscope analysis result shows that the molybdenum sulfide nano material has a porous spherical shape.
(4) The obtained MoS2Ultrasonically dispersing 300mg of nano material in 20mL of deionized water containing 0.5% of Nafion for 5min, dropwise coating 20 mu L of nano material on the surface of the glassy carbon electrode modified by the platinum nano particles obtained in the step (2), and airing to obtain MoS2Modifying the glassy carbon electrode by the nano material/platinum nano particles;
(5) with the MoS2The nano material/platinum nano particle modified glassy carbon electrode is used as a working electrode, the platinum electrode is used as a counter electrode, Ag/AgCl is used as a reference electrode to form a three-electrode system, the three-electrode system is placed in aqueous solution containing thiophene monomers, electrochemical polymerization is carried out by cyclic voltammetry, the potential range is-1.0V to-0.5V, polythiophene is modified on the working electrode, and polythiophene/MoS is obtained2Nano materialThe glassy carbon electrode is modified by the material/platinum nano particles.
Example 3
The concentrations of the solutions were 1.0 × 10 in PBS buffer (pH 4.0), respectively-7mol/L，1.0×10-6mol/L，2.0×10-6mol/L，5.0×10-6mol/L，8.0×10-6mol/L，1.0×10-5A riboflavin water solution of mol/L; example 2 Polythiophene/MoS prepared2The nano material/platinum nano particle modified glassy carbon electrode is used as a working electrode, the platinum electrode is used as a counter electrode, Ag/AgCl is used as a reference electrode to form a three-electrode system, and the three-electrode system is placed in a riboflavin water solution;
the differential pulse voltammetry is adopted to carry out electrochemical detection on the riboflavin, the scanning potential range is 0.5-1.0V, and the scanning speed is 100 mV/s. The detection limit of differential pulse voltammetry for detecting riboflavin is 6.0 multiplied by 10-8mol/L, linear range of 1.0X 10-7mol/L-8.0×10-6mol/L。
In conclusion, the detection method disclosed by the invention deposits the platinum nanoparticles on the surface of the glassy carbon electrode in the chloroplatinic acid solution through cyclic voltammetry, and synthesizes MoS through a hydrothermal synthesis method2Nano material of MoS2Modifying the surface of a glassy carbon electrode modified by platinum nanoparticles by using a nano material, and performing electrochemical polymerization on the surface of the glassy carbon electrode modified by the platinum nanoparticles2Electrically depositing polythiophene on the surface of the nano material to obtain polythiophene/MoS2The glass carbon electrode is modified by nano materials/platinum nano particles. The differential pulse voltammetry is adopted to detect the riboflavin, the linear range is wide, the sensitivity is high, the electrode can be used for many times, and the operation is convenient.
The foregoing is directed to the preferred embodiment of the present invention and is not intended to limit the invention to the specific embodiment described. It will be apparent to those skilled in the art that various modifications, equivalents, improvements and the like can be made without departing from the spirit of the invention, and these are intended to be included within the scope of the invention.
Claims (9)
1. A preparation method of a glassy carbon electrode modified by nano particles is characterized by comprising the following steps:
(1) pretreating a glassy carbon electrode: sequentially placing a glassy carbon electrode on polishing cloth containing polishing powder with the particle sizes of 1 mu m, 0.3 mu m and 0.05 mu m to polish the glassy carbon electrode to a mirror surface, sequentially placing the glassy carbon electrode in acetone, a sulfuric acid solution with the concentration of 0.5mol/L and ultrapure water to perform ultrasonic treatment for 1 minute, and washing the glassy carbon electrode with the ultrapure water for 1 minute after each ultrasonic treatment to obtain a pretreated glassy carbon electrode;
(2) preparing a platinum nanoparticle modified glassy carbon electrode: placing the pretreated glassy carbon electrode in a hydrogen-containing atmosphere2PtCl6Performing electrodeposition of platinum nanoparticles in a (100mM) solution by cyclic voltammetry under a potential scanning range of-0.8V-0V, washing with ethanol and deionized water after the electrodeposition is finished, and drying under an infrared lamp to obtain a platinum nanoparticle modified glassy carbon electrode;
(3)MoS2preparing a nano material: 0.7mmol (NH)4)6Mo7O24·4H2Dissolving O in 20mL of deionized water by ultrasonic waves, slowly adding 10mg of surfactant-citric acid monohydrate under the condition of magnetic stirring, and continuously stirring for 30min to uniformly mix to obtain a solution A; then, adding 10mmol of thiourea into 20mL of deionized water, and carrying out ultrasonic dissolution to obtain a solution B; slowly dripping the solution B into the solution A under the conditions of room temperature and vigorous stirring, continuously stirring for 1 hour after dripping is finished, transferring the mixed solution into a high-pressure reaction kettle for hydrothermal reaction at the temperature of 180 ℃ and 200 ℃ for 20-24 hours, naturally cooling to room temperature after the reaction is finished, filtering to obtain a solid product, washing the obtained solid product with ethanol and carbon disulfide for a plurality of times, placing the product in a vacuum drying box for drying at the temperature of 50 ℃ overnight to obtain MoS2A nanomaterial; an electron microscope analysis result shows that the molybdenum sulfide nano material has a porous spherical shape;
(4) the obtained MoS2Dispersing 200-300mg of the nano material in 20mL of deionized water containing 0.5% of Nafion by ultrasonic for 5min, dripping 20 mu L of the nano material on the surface of the glassy carbon electrode modified by the platinum nano particles obtained in the step (2), and airing to obtain MoS2Modifying the glassy carbon electrode by the nano material/platinum nano particles;
(5) to be provided withThe MoS2The nano material/platinum nano particle modified glassy carbon electrode is used as a working electrode, the platinum electrode is used as a counter electrode, Ag/AgCl is used as a reference electrode to form a three-electrode system, the three-electrode system is placed in an aqueous solution containing thiophene monomers, electrochemical polymerization is carried out by cyclic voltammetry, polythiophene is modified on the working electrode, and polythiophene/MoS is obtained2The glass carbon electrode is modified by nano materials/platinum nano particles.
2. The production method according to claim 1, wherein the concentration of the chloroplatinic acid solution in step (2) is 200 mM.
3. The method of claim 1, wherein the potential sweep range of the electrochemical deposition in step (2) is-0.8V-0V.
4. The method according to claim 1, wherein the hydrothermal reaction in the step (3) is carried out under the following conditions: carrying out hydrothermal reaction at 200 ℃ for 24 h.
5. The method according to claim 1, wherein the step (4) is carried out by mixing 300mgMoS2The nanomaterial was ultrasonically dispersed in 20mL of deionized water containing 0.5% Nafion.
6. The application of the glassy carbon electrode modified by the nano particles is characterized in that polythiophene/MoS2The nano material/platinum nano particle modified glassy carbon electrode is prepared by the method of any one of claims 1 to 5; the application is to mix polythiophene/MoS2The nano material/platinum nano particle modified glassy carbon electrode is applied to electrochemical detection of riboflavin.
7. The use of a nanoparticle-modified glassy carbon electrode according to claim 6, wherein: the step of electrochemically detecting riboflavin comprises:
a. preparing riboflavin aqueous solutions with different concentrations by adopting PBS buffer solution;
b. by using polythiophene/MoS2Nanomaterial/platinum nanoparticlesThe particle modified glassy carbon electrode is used as a working electrode, the platinum electrode is used as a counter electrode, the Ag/AgCl electrode is used as a reference electrode to form a three-electrode system, and the three-electrode system is placed in the riboflavin water solution;
c. carrying out electrochemical detection on riboflavin by adopting a differential pulse voltammetry method to obtain peak currents corresponding to riboflavin with different concentrations;
d. taking the peak current as a vertical coordinate and the concentration as a horizontal coordinate to make a standard curve;
e. and (3) placing the three-electrode system in the riboflavin aqueous solution with unknown concentration to obtain a differential pulse voltammetry curve and a peak current of the riboflavin aqueous solution with unknown concentration, and obtaining the riboflavin concentration according to a standard curve.
8. The use of a glassy carbon electrode modified with nanoparticles according to claim 7, wherein the electrochemical parameters of the differential pulse voltammetry are: the scanning potential range is 0.5-1.0V, and the scanning speed is 100 mV/s.
9. The application of the glassy carbon electrode modified by the nano particles as claimed in claim 8, wherein the detection limit of the differential pulse voltammetry for detecting the riboflavin is 6.0 x 10-8mol/L, linear range of 1.0X 10-7mol/L-8.0×10-6mol/L。
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| CN112557471A (en) * | 2020-12-22 | 2021-03-26 | 合肥天一生物技术研究所有限责任公司 | Preparation method and detection method of modified electrode capable of simultaneously detecting vitamins B6 and B9 |
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| CN111990994A (en) * | 2020-09-02 | 2020-11-27 | 天津理工大学 | EEG flexible dry electrode and preparation method and application thereof |
| CN111990994B (en) * | 2020-09-02 | 2023-10-10 | 天津理工大学 | EEG flexible dry electrode and preparation method and application thereof |
| CN112179970A (en) * | 2020-09-22 | 2021-01-05 | 蚌埠学院 | VB12Preparation method of/GCE modified electrode and application of GCE modified electrode in rapid detection of VB2In (1) |
| CN112067674A (en) * | 2020-09-30 | 2020-12-11 | 常州市新鸿医药化工技术有限公司 | Molecular imprinting electrochemical sensor and method for detecting folic acid content by using same |
| CN112557471A (en) * | 2020-12-22 | 2021-03-26 | 合肥天一生物技术研究所有限责任公司 | Preparation method and detection method of modified electrode capable of simultaneously detecting vitamins B6 and B9 |
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| CN115813399A (en) * | 2022-12-08 | 2023-03-21 | 天津大学 | Nano material modified nerve electrode and preparation method thereof |
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