CN110865116A - Electrochemical nano enzyme sensor for detecting 5-nitroguaiacol sodium - Google Patents
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Abstract
The invention discloses an electrochemical nano enzyme sensor for detecting 5-nitroguaiacol sodium, which belongs to the technical field of electrochemical sensorsDetecting the content of the 5-nitroguaiacol sodium in the solution to be detected by an ampere method; the composite electrode is molybdenum disulfide (MoS)2) And a carboxylated multi-walled carbon nanotube (COOH-MWCNT). The sensor not only can successfully detect the 5-nitroguaiacol sodium, but also has the characteristics of high sensitivity, strong selectivity, good stability, enzyme property and the like.
Description
Technical Field
The invention belongs to the technical field of electrochemical sensors, and particularly relates to an electrochemical nano enzyme sensor for detecting 5-nitroguaiacol sodium.
Background
The compound sodium nitrophenolate is a plant growth regulator, can promote wound healing and accelerate plant growth, and comprises the chemical components of 5-nitroguaiacol sodium (called 2-methoxy-5-nitrophenolate sodium), o-nitrophenolate sodium and p-nitrophenolate sodium, wherein the 5-nitroguaiacol sodium is the most key component of the compound sodium nitrophenolate, and has the best regulating capability, but the excessive use can cause the risk of teratogenesis. So far, the detection of the 5-nitroguaiacol sodium comprises a high performance liquid chromatography and electrochemical workstation combined technology, a high performance liquid chromatography-normal pressure chemical ionization-mass spectrometry combined technology and a high performance liquid chromatography, but the technologies are time-consuming, high in operation technology, expensive in equipment, complex in sample preparation and not suitable for wide application.
Enzymes play an important role in biocatalysts, but the activity of enzymes is easily destroyed under certain severe conditions, such as inappropriate pH or temperature. With the development of the technology, the nano enzyme becomes a bright point in the field of sensors, has the activity of the enzyme, meets the kinetic equation of the enzyme, and overcomes the severe requirements on catalytic conditions. In addition, nanoenzymes are easy to prepare and have strong durability. Recently, a new generation of materials such as carbon materials, metal nanoparticles, metal oxide nanoparticles, and the like have shown activity of nanoenzymes. These materials have been used for sensing (e.g., detection of ions, molecules, elimination of cells), therapeutic and environmental engineering.
The sensor has the advantages of time saving, high sensitivity, rapidness, simplicity, convenience and high efficiency, the sensor is widely applied to the detection of the aspects of optics, biology, clinic, food, pesticide and the like at present, the electrochemical detection research report on the 5-nitroguaiacol sodium is few at present, and the electrochemical behavior and the determination of the internal wile sensitivity and the like (wile sensitivity, Chenliji, 5-nitroguaiacol on the multiwalled carbon nanotube modified electrode [ J]The 'analysis and test journal' 2010) utilizes a multiwalled carbon nanotube modified electrode to carry out electrochemical detection on 5-nitroguaiacol sodium in a sodium citrate solution, and the linear range is 5 multiplied by 10-5-5×10-4mol L-1The detection limit is 8.6 multiplied by 10-7mol L-1The linear range obtained by the method is narrow, and the sensitivity is low.
Disclosure of Invention
Aiming at the technical problems, the invention provides the electrochemical nano enzyme sensor for detecting the 5-nitroguaiacol sodium, which realizes the electrochemical detection of the 5-nitroguaiacol sodium and has the advantages of simpleness, high efficiency, low cost, rapidness and good selectivity.
In order to achieve the purpose, the invention adopts the following technical scheme:
an electrochemical nanoenzyme sensor for detecting 5-nitroguaiacol sodium comprises a three-electrode system, wherein a saturated calomel electrode is used as a reference electrode, a platinum sheet electrode is used as a counter electrode, a composite electrode is used as a working electrode, acetate buffer solution is used as electrolyte solution, and the content of the 5-nitroguaiacol sodium in a solution to be detected is detected by using a differential pulse voltammetry method; the composite electrode is molybdenum disulfide (MoS)2) And a carboxylated multi-walled carbon nanotube (COOH-MWCNT).
Preferably, the acetate buffer solution has a concentration of 0.1M, a pH of 4, and a voltage window of 0.5-1.0V.
Preferably, the preparation method of the composite electrode is as follows:
(1) weighing single-layer molybdenum disulfide powder, preparing with deionized water, and performing ultrasonic treatment for 30min to obtain 1mg/mL molybdenum disulfide dispersion;
(2) weighing carboxylated multi-walled carbon nanotubes, preparing by using 0.5% perfluorosulfonic acid, and carrying out ultrasonic treatment for 30min to obtain 1mg/mL carboxylated multi-walled carbon nanotube dispersion liquid;
(3) mixing the obtained molybdenum disulfide dispersion liquid and the carboxylated multi-walled carbon nanotube dispersion liquid according to the volume ratio of 1: 1, and performing ultrasonic treatment for 1 hour to obtain the composite material MoS2-COOH-MWCNT；
(4) Polishing glassy carbon electrode, dropping 10 μ L of the above composite material on the glassy carbon electrode, and drying at 60 deg.C to obtain composite electrode MoS2-COOH-MWCNT。
The beneficial technical effects of the invention are as follows: the preparation method of the 5-nitroguaiacol sodium electrochemical nanoenzyme sensor established by the invention has the characteristics of low preparation cost, simple process and simple operation, can successfully detect the 5-nitroguaiacol sodium, has high sensitivity (the lower detection limit can reach 0.03 mu mol/L), strong selectivity, good stability, enzyme property and the like, and can be used for determining the content of the 5-nitroguaiacol sodium in chicken feed and tomatoes.
Drawings
FIG. 1 shows the MoS prepared2-electron micrograph of COOH-MWCNT composite;
FIG. 2 shows the MoS prepared2-differential pulsed voltammogram of COOH-MWCNT/GCE in 20 μmol/L5-nitroguaiacol sodium acetate buffer;
FIG. 3 is a differential pulse voltammogram of prepared composite electrodes in acetate buffer solutions of sodium 5-nitroguaiacol at different concentrations;
FIG. 4 is a graph of current versus concentration for prepared composite electrodes in acetate buffer solutions of sodium 5-nitroguaiacol at various concentrations;
FIG. 5 is a graph of the linear relationship between the reciprocal current and the reciprocal concentration of a prepared composite electrode in acetate buffer solutions of sodium 5-nitroguaiacol at different concentrations;
FIG. 6 is a graph of the stability of the electrochemical nanoenzyme sensor of sodium nitroguaiacol.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1
An electrochemical nanoenzyme sensor for detecting 5-nitroguaiacol sodium comprises a three-electrode system, wherein a saturated calomel electrode is used as a reference electrode, a platinum sheet electrode is used as a counter electrode, a composite electrode is used as a working electrode, acetate buffer solution is used as electrolyte solution, and the content of the 5-nitroguaiacol sodium in a solution to be detected is detected by using a differential pulse voltammetry method; the composite electrode is molybdenum disulfide (MoS)2) And a carboxylated multi-walled carbon nanotube (COOH-MWCNT).
The concentration of acetate buffer solution is 0.1M, pH is 4, and the voltage window is 0.5-1.0V.
The preparation method of the composite electrode comprises the following steps:
(1) weighing single-layer molybdenum disulfide powder, preparing with deionized water, and performing ultrasonic treatment for 30min to obtain 1mg/mL molybdenum disulfide dispersion;
(2) weighing carboxylated multi-walled carbon nanotubes, preparing by using 0.5% perfluorosulfonic acid, and carrying out ultrasonic treatment for 30min to obtain 1mg/mL carboxylated multi-walled carbon nanotube dispersion liquid;
(3) mixing the obtained molybdenum disulfide dispersion liquid and the carboxylated multi-walled carbon nanotube dispersion liquid according to the volume ratio of 1: 1, and performing ultrasonic treatment for 1 hour to obtain the composite material MoS2-COOH-MWCNT；
(4) Polishing glassy carbon electrode, dropping 10 μ L of the above composite material on the glassy carbon electrode, and drying at 60 deg.C to obtain composite electrode MoS2-COOH-MWCNT。
MoS obtained in example 12-COOH-MWCNT composite for appearance characterization, MoS2The morphology of the-COOH-MWCNT composite material is shown in an electron microscope picture of figure 1, the COOH-MWCNT is well dispersed in a perfluorosulfonic acid solution to obtain a uniform dispersion liquid, MoS2The sheet structure is presented, and the composite material shows the appearance of both materials.
The performance of the electrochemical nano enzyme sensor of the 5-nitroguaiacol sodium obtained in the example 1 is detected:
electrochemical behavior of sodium 5-nitroguaiacol: the electrochemical behavior of sodium 5-nitroguaiacol is shown in FIG. 2: in a 0.1mol/L acetate buffer solution containing 20 mu mol/L5-nitroguaiacol sodium, a peak is arranged near 0.8V, a composite electrode has a peak near 0.73V, and the peak current is about 6.5 times of that of a bare electrode, which shows that the composite electrode has good electrocatalytic effect on the 5-nitroguaiacol sodium.
Electrochemical response of sodium 5-nitroguaiacol: the 5-nitroguaiacol sodium with different concentrations is added into the acetate buffer solution with the concentration of 0.1mol/L in sequence, and as can be seen by combining the graph in figure 3 and figure 4, the current is gradually increased between the concentration of 0.09 and 70 mu mol/L, the current is almost saturated and does not change at 70 mu mol/L, the characteristic is similar to the characteristic of the enzyme, and according to the characteristic, the relationship between the reciprocal current and the reciprocal concentration is further studied, the reciprocal current and the reciprocal concentration are found to show a good linear relationship, as shown in figure 5, the Mie's constant of the enzyme can be calculated to be 16.02mM by using the Mie's equation of the enzyme, and the characteristic shows that the composite material has relatively high affinity. In addition, the linearity of the detection of 5-nitroguaiacol sodium is 0.09-70 mu mol/L, and the detection limit is 0.03 mu mol/L.
Reproducibility of detection of 5-nitroguaiacol sodium: 20 mu mol/L of 5-nitroguaiacol sodium is added into 0.1mol/L acetate buffer solution, six different composite electrodes are used for detection in the buffer solution, and as shown in figure 6, the obtained current relative standard deviation RSD value is 0.4839%, which indicates that the repeatability of the composite electrode is good.
In conclusion, the electrochemical nano enzyme sensor for detecting the 5-nitroguaiacol sodium has the characteristics of good repeatability, wide linear range, low detection limit and high affinity of nano enzyme, and in addition, the sensor is a nano enzyme sensor, so that a foundation is provided for application in other fields.
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 variations which do not require inventive efforts and are made by those skilled in the art are still within the scope of the present invention.
Claims (3)
1. DetectionThe electrochemical nanoenzyme sensor of the 5-nitroguaiacol sodium is characterized in that a three-electrode system is formed by taking a saturated calomel electrode as a reference electrode, a platinum sheet electrode as a counter electrode and a composite electrode as a working electrode, acetate buffer solution is taken as electrolyte solution, and the content of the 5-nitroguaiacol sodium in the solution to be detected is detected by using a differential pulse voltammetry method; the composite electrode is molybdenum disulfide (MoS)2) And a carboxylated multi-walled carbon nanotube (COOH-MWCNT).
2. The electrochemical nanoenzyme sensor for detecting sodium 5-nitroguaiacol as claimed in claim 1, wherein the concentration of acetate buffer solution is 0.1M, pH is 4, and the voltage window is 0.5-1.0V.
3. The electrochemical nanoenzyme sensor for detecting sodium 5-nitroguaiacol as claimed in claim 1, wherein the composite electrode is prepared by the following steps:
(1) weighing single-layer molybdenum disulfide powder, preparing with deionized water, and performing ultrasonic treatment for 30min to obtain 1mg/mL molybdenum disulfide dispersion;
(2) weighing carboxylated multi-walled carbon nanotubes, preparing by using 0.5% perfluorosulfonic acid, and carrying out ultrasonic treatment for 30min to obtain 1mg/mL carboxylated multi-walled carbon nanotube dispersion liquid;
(3) mixing the obtained molybdenum disulfide dispersion liquid and the carboxylated multi-walled carbon nanotube dispersion liquid according to the volume ratio of 1: 1, and performing ultrasonic treatment for 1 hour to obtain the composite material MoS2-COOH-MWCNT；
(4) Polishing glassy carbon electrode, dropping 10 μ L of the above composite material on the glassy carbon electrode, and drying at 60 deg.C to obtain composite electrode MoS2-COOH-MWCNT。
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111337558A (en) * | 2020-04-06 | 2020-06-26 | 东莞正大康地饲料有限公司 | Method for measuring sodium content in feed by using ion selective electrode |
| CN115165988A (en) * | 2022-03-01 | 2022-10-11 | 浙江大学 | Working electrode for detecting nitrite and detection method thereof |
| CN115389601A (en) * | 2022-09-09 | 2022-11-25 | 湘潭大学 | Preparation of luteolin electrochemical sensor and method for detecting luteolin |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111337558A (en) * | 2020-04-06 | 2020-06-26 | 东莞正大康地饲料有限公司 | Method for measuring sodium content in feed by using ion selective electrode |
| CN111337558B (en) * | 2020-04-06 | 2023-03-28 | 正大康地农牧集团有限公司 | Method for measuring sodium content in feed by using ion selective electrode |
| CN115165988A (en) * | 2022-03-01 | 2022-10-11 | 浙江大学 | Working electrode for detecting nitrite and detection method thereof |
| CN115389601A (en) * | 2022-09-09 | 2022-11-25 | 湘潭大学 | Preparation of luteolin electrochemical sensor and method for detecting luteolin |
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