CN110988072A - Single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube electrochemical sensor and application thereof in detection of nitenpyram - Google Patents
Single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube electrochemical sensor and application thereof in detection of nitenpyram Download PDFInfo
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- CN110988072A CN110988072A CN201911330025.7A CN201911330025A CN110988072A CN 110988072 A CN110988072 A CN 110988072A CN 201911330025 A CN201911330025 A CN 201911330025A CN 110988072 A CN110988072 A CN 110988072A
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Abstract
The invention relates to the technical field of electrochemical sensing detection, in particular to a single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube electrochemical sensor and application thereof in detecting nitenpyram. The invention discloses a single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube electrochemical sensor and application thereof in detecting nitenpyram, wherein the sensor comprises the following components: preparing a single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube electrochemical sensor; the electrochemical sensor is used for detecting nitenpyram. The invention overcomes the defects of complicated method, complicated steps and the like existing in the prior art when detecting the nitenpyram, better improves the detection sensitivity, and is easy to automate the detection of the nitenpyram.
Description
Technical Field
The invention relates to the field of electrochemical sensors, in particular to a single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube electrochemical sensor and application thereof in detection of nitenpyram.
Background
The harm of pesticide residue to human health and environment is more and more paid attention by people. Nitenpyram (Nitenpyram) is a novel neonicotinoid insecticide, is widely applied to crops such as rice, corn, sunflower, rape, vegetables, fruits and the like, and achieves satisfactory effect in agricultural production. With the progress of research, it has been reported that nitenpyram has serious adverse effects on non-target organisms, is toxic to the organisms, and causes some environmental problems. Therefore, the method for quickly determining and reliably quantifying the nitenpyram in trace amount, which is beneficial to the environment and the human health, has important significance.
The electrochemical sensor is a sensor for detecting a target object based on the principle of electrochemical reaction, and takes an electrode as a sensor conversion element, a material modified on the electrode as a sensitive element, the sensitive element is contacted with ions or molecules of a detected object to generate chemical reaction or change, the conversion element directly or indirectly converts the reaction or change into an electric signal, and the relationship between chemical quantities such as the concentration and the composition of the target object and an output electric signal is established, so that the quantitative detection of the target object is realized. The carbon nanotube material has the advantages of high specific surface area, easy storage and improved conductivity, can be covalently bonded with an electrode material, and can be used for preparing an electrochemical sensor. However, some conventional electrochemical sensors still have problems of low sensitivity and excessively high detection limit although carbon nanotube materials are used in the preparation process.
Disclosure of Invention
In view of the above problems, it is an object of the present invention to provide a single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube electrochemical sensor, which is prepared by the following steps:
(1) and (3) treating the glassy carbon electrode:
polishing a glassy carbon electrode with the diameter of 3mm by using gamma-alumina with the particle size of 0.05 mu m, ultrasonically cleaning by using redistilled water, and airing at room temperature to obtain a glassy carbon electrode pretreatment substance;
(2) pretreatment of the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode:
dripping single-wall carbon nanohorn dispersion liquid on the surface of the glassy carbon electrode pretreatment object, and placing under an infrared lamp for irradiation till drying to obtain a single-wall carbon nanohorn modified electrode; then, the hydroxylated multi-walled carbon nanotube dispersion liquid is dripped on the surface of the single-walled carbon nanohorn modified electrode, and the single-walled carbon nanohorn modified electrode is placed under an infrared lamp to be irradiated to be dried, so that a pretreatment substance of the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode is obtained;
(3) the construction of the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode comprises the following steps:
placing the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode in a PBS buffer solution, and scanning by using differential pulse voltammetry to stabilize the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode; then carrying out constant potential enrichment under magnetic stirring at 1000rpm to obtain the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode;
wherein the potential interval during differential pulse voltammetry scanning is-1.0V to-1.4V, and the interval between two times of scanning is 1 min;
the potential interval of constant potential enrichment is-0.4V to-1.1V, and the enrichment time is 0-8 min;
(4) setting of the electrochemical sensor:
and (3) taking the working electrode as a single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode, taking the counter electrode as a hollow titanium rod and taking the reference electrode as a saturated calomel electrode to obtain the electrochemical sensor.
Preferably, the concentration of the PBS buffer solution in the step (3) is 0.2 mol/L.
Preferably, the potentiostatic enrichment is at a potential of-0.5V.
Preferably, the enrichment time of the potentiostatic enrichment is 6 min.
The invention also aims to provide a single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube electrochemical sensor and application thereof in detecting nitenpyram, which specifically comprise the following components:
placing the electrochemical sensor in an electrolytic cell loaded with electrolyte, and detecting the concentration of nitenpyram in the object to be detected by using differential pulse voltammetry;
wherein the electrolyte is PBS buffer solution; the volume of the electrolytic cell is 25mL, the volume of the loaded electrolyte is 20mL during each detection, and an electromagnetic stirrer is adopted for stirring;
high-purity nitrogen is introduced into the electrolyte for 3min before use so as to fully remove dissolved oxygen in the electrolyte.
Preferably, the pH of the liquid in the cell is 11.0.
Preferably, the concentration of the PBS buffer solution is 0.2 mol/L.
The invention has the beneficial effects that:
1. the invention utilizes the double amplification effect of the single-walled carbon nanohorn and the hydroxylated multi-walled carbon nanotube to prepare the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode, and utilizes the electrode to prepare the electrochemical sensor which can be used for detecting nitenpyram with high sensitivity.
2. The electrochemical sensor for detecting the trace nitenpyram, which is prepared by the invention, overcomes the defects of complicated method, complicated steps and the like existing in the prior art when the nitenpyram is detected, better improves the detection sensitivity, and is easy to automate for the detection of the nitenpyram.
Drawings
The invention is further illustrated by means of the attached drawings, but the embodiments in the drawings do not constitute any limitation to the invention, and for a person skilled in the art, other drawings can be obtained on the basis of the following drawings without inventive effort.
FIG. 1 shows differential pulse voltammograms of electrodes prepared in different ways;
FIG. 2 shows a standard absorption curve of a sensor according to example 1 of the present invention;
FIG. 3 is a graph showing the effect of interferents in the detection of nitenpyram.
Detailed Description
The invention is further described with reference to the following examples.
Example 1
A single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube electrochemical sensor is prepared by the following steps:
(1) and (3) treating the glassy carbon electrode:
polishing a glassy carbon electrode with the diameter of 3mm by using gamma-alumina with the particle size of 0.05 mu m, ultrasonically cleaning by using redistilled water, and airing at room temperature to obtain a glassy carbon electrode pretreatment substance;
(2) pretreatment of the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode:
dripping single-wall carbon nanohorn dispersion liquid on the surface of the glassy carbon electrode pretreatment object, and placing under an infrared lamp for irradiation till drying to obtain a single-wall carbon nanohorn modified electrode; then, the hydroxylated multi-walled carbon nanotube dispersion liquid is dripped on the surface of the single-walled carbon nanohorn modified electrode, and the single-walled carbon nanohorn modified electrode is placed under an infrared lamp to be irradiated to be dried, so that a pretreatment substance of the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode is obtained;
(3) the construction of the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode comprises the following steps:
placing the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode in PBS (phosphate buffer solution) with the concentration of 0.2mol/L, and scanning by using differential pulse voltammetry to stabilize the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode; then carrying out constant potential enrichment under magnetic stirring at 1000rpm to obtain the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode;
wherein the potential interval during differential pulse voltammetry scanning is-1.0V to-1.4V, and the interval between two times of scanning is 1 min;
the potential interval of constant potential enrichment is-0.4V to-1.1V, and the enrichment time is 0-8 min;
(4) setting of the electrochemical sensor:
and (3) taking the working electrode as a single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode, taking the counter electrode as a hollow titanium rod and taking the reference electrode as a saturated calomel electrode to obtain the electrochemical sensor.
Example 2
A single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube electrochemical sensor is prepared by the following steps:
(1) and (3) treating the glassy carbon electrode:
polishing a glassy carbon electrode with the diameter of 3mm by using gamma-alumina with the particle size of 0.05 mu m, ultrasonically cleaning by using redistilled water, and airing at room temperature to obtain a glassy carbon electrode pretreatment substance;
(2) pretreatment of the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode:
dripping single-wall carbon nanohorn dispersion liquid on the surface of the glassy carbon electrode pretreatment object, and placing under an infrared lamp for irradiation till drying to obtain a single-wall carbon nanohorn modified electrode; then, the hydroxylated multi-walled carbon nanotube dispersion liquid is dripped on the surface of the single-walled carbon nanohorn modified electrode, and the single-walled carbon nanohorn modified electrode is placed under an infrared lamp to be irradiated to be dried, so that a pretreatment substance of the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode is obtained;
(3) the construction of the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode comprises the following steps:
placing the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode in PBS (phosphate buffer solution) with the concentration of 0.2mol/L, and scanning by using differential pulse voltammetry to stabilize the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode; then carrying out constant potential enrichment under magnetic stirring at 1000rpm to obtain the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode;
wherein the potential interval during differential pulse voltammetry scanning is-1.0V to-1.4V, and the interval between two times of scanning is 1 min;
the potential interval of constant potential enrichment is-0.5V, and the enrichment time is 6 min;
(4) setting of the electrochemical sensor:
and (3) taking the working electrode as a single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode, taking the counter electrode as a hollow titanium rod and taking the reference electrode as a saturated calomel electrode to obtain the electrochemical sensor.
Example 3
The method for detecting the nitenpyram by the electrochemical sensor comprises the following steps:
placing an electrochemical sensor in an electrolytic cell loaded with electrolyte, and detecting the concentration of nitenpyram in the object to be detected by using differential pulse voltammetry;
wherein the electrolyte is PBS buffer solution with the concentration of 0.2 mol/L; the volume of the electrolytic cell is 25mL, the volume of the loaded electrolyte is 20mL during each detection, and an electromagnetic stirrer is adopted for stirring; the pH of the liquid in the cell was 7.0.
High-purity nitrogen is introduced into the electrolyte for 3min before use so as to fully remove dissolved oxygen in the electrolyte.
Example 4
Establishing a linear equation for detecting nitenpyram:
based on the sensitivity reaction degree (shown in fig. 2) of the electrochemical sensor prepared in the embodiment 1 of the invention to nitenpyram, a linear equation for electrochemical detection of nitenpyram is established; wherein, I represents peak current with the unit of muA; c represents the detection concentration of nitenpyram, and the unit is nmol/L.
As shown in FIG. 2, the concentration of nitenpyram is 20-2000 × 10-9At mol/L, the electrochemical signal response and the nitenpyram concentration are in a good linear relation, and the peak current and the nitenpyram concentration are in a good linear relation.
The linear equation is I (mu A) ═ 0.017C-0.125;
wherein, the correlation coefficient R is 0.995, and the detection limit is 4 nmol/L;
i represents the peak current in μ A; c represents the detection concentration of nitenpyram, and the unit is nmol/L.
Example 5
Effect of interferents in the detection of nitenpyram:
the nitenpyram concentration is set to be 100nmol/L, and ascorbic acid with the concentration of 200 times, fipronil with the concentration of 200 times, glucose with the concentration of 500 times and vitamin A acetate interferent with the concentration of 500 times are respectively added into the nitenpyram concentration as a reference, the electrochemical sensor prepared in the embodiment 1 of the invention and the method in the embodiment 3 are used for detecting the nitenpyram, the influence of the interferent on the detection result is observed, and the result is shown in figure 3: ordinate I0Represents the peak current of the flavanonoside in the absence of interferents, and I represents the peak current of the flavanonoside in the presence of interferents.
As can be seen from FIG. 3, the ascorbic acid was 200 times concentrated, fipronil was 200 times concentrated, glucose was 500 times concentrated, and vitamin A acetate was 500 times concentratedThe ratio (I/I) of the peak current of the nitenpyram to the peak current of the nitenpyram without interfering substances0) In the vicinity of 100%, it was further confirmed that the sensitivity of the present invention for detecting nitenpyram is hardly affected by the presence of the above-mentioned interferents when detected using the electrochemical sensor prepared in example 1 of the present invention and the method of example 3.
Comparative example 1
The preparation method is as in example 1, except that the electrode is not modified by using single-walled carbon nanohorns and hydroxylated multi-walled carbon nanotubes (i.e. step (2) is omitted), namely the electrochemical sensor is prepared by directly using the glassy carbon electrode pretreatment as a working electrode.
Comparative example 2
The preparation method is as in example 1, except that the hydroxylated multi-walled carbon nanotube modified electrode is not used, only the single-walled carbon nanohorn modified electrode is used, and the prepared single-walled carbon nanohorn modified electrode is used as a working electrode to prepare the electrochemical sensor.
Comparative example 3
The preparation method is as in example 1, except that the electrode is modified by using only the hydroxylated multi-walled carbon nanotube without using the single-walled carbon nanohorn modified electrode, and the electrochemical sensor is prepared by using the prepared hydroxylated multi-walled carbon nanotube modified electrode as the working electrode.
In order to more clearly illustrate the contents of the present invention, the following experiments were performed with respect to the electrochemical sensors prepared in example 2, comparative example 1, comparative example 2 and comparative example 3 of the present invention:
1. the sensitivity of different electrochemical sensors to nitenpyram is detected as follows:
the concentration of the nitenpyram ethanol solution is set to be 2.0 multiplied by 10-6At mol/L, the electrochemical sensors prepared in example 1, comparative example 2 and comparative example 3 of the present invention are used for detecting nitenpyram by using the detection method of example 3 of the present invention, and the detection result is shown in fig. 1, in fig. 1: 1-comparative example 1; 2-comparative example 2; 3-comparative example 3; 4-example 1.
As shown in FIG. 1, the concentration of nitenpyram is 2.0 × 10-6At mol/L, the peak current of comparative example 1 was hardly seen, showing that the peak current was0.12 μ A, comparative example 2 showed a peak current of 6.65 μ A, comparative example 3 showed a current of 10.27 μ A, and example 1 showed a peak current of 17.36 μ A.
The peak current of the nitenpyram shown in example 1 in fig. 1 is 144 times larger than that of comparative example 1, which indicates that the electrochemical sensor prepared in example 1 of the present invention has good electrocatalytic performance on electrode reaction, and nitenpyram can generate sensitive electrochemical response on the electrochemical sensor prepared in example 1 of the present invention, and is very suitable for sensitive detection of nitenpyram.
2. Detection of the actual sample:
after the corn sample is subjected to the standard adding treatment (namely, the nitenpyram is added by adopting a standard adding method), the extract liquid of the corn sample is taken, the electrochemical sensor prepared in the embodiment 1 of the invention and the method in the embodiment 3 are used for carrying out electrochemical measurement, the average value of each group of data is obtained in parallel five times, and the measurement result is shown in table 1.
TABLE 1 maize sample spiking test results
| Standard concentration (nmol/L) | Recovery (%) | Relative standard deviation RSD (%) |
| 50 | 95.77～102.78 | 3.67 |
| 100 | 96.54～112.68 | 7.78 |
| 200 | 93.41～103.01 | 4.89 |
As can be seen from Table 1, the detection results show that the recovery rate is 93.41% -112.68%, and the relative standard deviation is 3.67-7.78%, so that the method for detecting nitenpyram by using the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube electrochemical sensor is feasible.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube electrochemical sensor is characterized by comprising the following steps:
(1) and (3) treating the glassy carbon electrode:
polishing a glassy carbon electrode with the diameter of 3mm by using gamma-alumina with the particle size of 0.05 mu m, ultrasonically cleaning by using redistilled water, and airing at room temperature to obtain a glassy carbon electrode pretreatment substance;
(2) pretreatment of the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode:
dripping single-wall carbon nanohorn dispersion liquid on the surface of the glassy carbon electrode pretreatment object, and placing under an infrared lamp for irradiation till drying to obtain a single-wall carbon nanohorn modified electrode; then, the hydroxylated multi-walled carbon nanotube dispersion liquid is dripped on the surface of the single-walled carbon nanohorn modified electrode, and the single-walled carbon nanohorn modified electrode is placed under an infrared lamp to be irradiated to be dried, so that a pretreatment substance of the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode is obtained;
(3) the construction of the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode comprises the following steps:
placing the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode in a PBS buffer solution, and scanning by using differential pulse voltammetry to stabilize the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode; then carrying out constant potential enrichment under magnetic stirring at 1000rpm to obtain the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode;
wherein the potential interval during the differential pulse voltammetry scanning is-0.4V to-1.1V, and the interval between the two times of scanning is 1 min;
the potential interval of constant potential enrichment is-0.4V to-1.1V, and the enrichment time is 0-8 min;
(4) setting of the electrochemical sensor:
and (3) taking the working electrode as a single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube modified electrode, taking the counter electrode as a hollow titanium rod and taking the reference electrode as a saturated calomel electrode to obtain the electrochemical sensor.
2. The single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube electrochemical sensor of claim 1, wherein the solvent of the single-walled carbon nanohorn dispersion and the solvent of the hydroxylated multi-walled carbon nanotube dispersion are both N, N-dimethylformamide.
3. The single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube electrochemical sensor of claim 1, wherein the concentration of the single-walled carbon nanohorn dispersion is 2 mg/mL; the amount of the single-walled carbon nanohorn dispersion was 5. mu.L.
4. The single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube electrochemical sensor of claim 1, wherein the concentration of the hydroxylated multi-walled carbon nanotube dispersion is 2 mg/mL; the dosage of the hydroxylated multi-wall carbon nano tube dispersion liquid is 1 mu L.
5. The single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube electrochemical sensor as claimed in claim 1, wherein the concentration of the PBS buffer solution in the step (3) is 0.2 mol/L.
6. The single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube electrochemical sensor as claimed in claim 1, wherein the potentiostatic enrichment has a potential of-0.5V and an enrichment time of 6 min.
7. The application of the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube electrochemical sensor in detecting nitenpyram is characterized in that the electrochemical sensor as claimed in any one of claims 1 to 6 is used for detecting nitenpyram.
8. The application of the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube electrochemical sensor in detecting nitenpyram according to claim 7, wherein the detection of nitenpyram is specifically as follows:
placing the electrochemical sensor in an electrolytic cell loaded with electrolyte, and detecting the concentration of nitenpyram in the object to be detected by using differential pulse voltammetry;
wherein the electrolyte is PBS buffer solution; the volume of the electrolytic cell is 25mL, the volume of the loaded electrolyte is 20mL during each detection, and an electromagnetic stirrer is adopted for stirring;
high-purity nitrogen is introduced into the electrolyte for 3min before use so as to fully remove dissolved oxygen in the electrolyte.
9. The use of the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube electrochemical sensor as claimed in claim 8, wherein the pH of the liquid in the electrolytic cell is 11.0.
10. The application of the single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube electrochemical sensor in detecting nitenpyram according to claim 8, wherein the concentration of the PBS buffer solution is 0.2 mol/L.
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