CN113311045A - Preparation method of graphene nano-roll cured clenbuterol hydrochloride sensor - Google Patents
Preparation method of graphene nano-roll cured clenbuterol hydrochloride sensor Download PDFInfo
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- CN113311045A CN113311045A CN202110807155.6A CN202110807155A CN113311045A CN 113311045 A CN113311045 A CN 113311045A CN 202110807155 A CN202110807155 A CN 202110807155A CN 113311045 A CN113311045 A CN 113311045A
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Abstract
The invention relates to a preparation method of a graphene nano-roll cured clenbuterol hydrochloride sensor. The method comprises the following steps: adding graphene oxide into hydrogen peroxide to obtain purified graphene oxide; weighing the purified graphene oxide, and adding deionized water, water glass, ammonia water and hexadecyl trimethyl ammonium chloride to obtain an SI @ graphene solution. Dropwise adding hydrazine hydrate into the SI @ graphene solution, and stirring to obtain an SI @ graphene nano roll; and (3) dropwise adding the SI @ graphene nano roll solution on a glassy carbon electrode to form an adsorption adhesive film. And continuously dropwise adding a clenbuterol hydrochloride antibody solution to the adsorption film on the glassy carbon electrode, and uniformly vacuum-drying the film to obtain the clenbuterol hydrochloride electrochemical sensor. The sensor constructed by the invention is applied to the detection of the target component clenbuterol hydrochloride, and the actual concentration range of the detection is 0.05 multiplied by 10‑7‑8×10‑7mol/L. Compared with the prior art, the invention has the advantages of simple synthesisAnd the cost is reduced.
Description
Technical Field
The invention relates to the technical field of clenbuterol hydrochloride food safety detection, and particularly relates to a preparation method of a graphene nano-roll cured clenbuterol hydrochloride sensor.
Background
The two-dimensional material is used as a construction unit for assembly and cutting, and a new material with special appearance and function can be obtained. This is an important direction for the development of two-dimensional materials. The nano-coil is a special one-dimensional material constructed by two-dimensional materials, and is a one-dimensional nano-structure formed by curling two-dimensional nano-materials. Nanoscrolls are a promising material structure to advance the application of two-dimensional materials in battery, sensing, filtering and photocatalytic processes. Such one-dimensional nanostructures not only retain the superior properties of a two-dimensional matrix, but also exhibit new properties resulting from one-dimensional geometric arrangements. The spiral rolling of two-dimensional nanoplates to form one-dimensional nanostructures, nanoscrolls, has been a hot research topic of scientists in recent years, and according to theoretical prediction, these one-dimensional nanostructures will exhibit unusual electronic, mechanical and optical properties due to their unique, open tubular structure and adjustable interlayer spacing. Graphene-based nanoscrolls are the most representative class of one-dimensional materials. Therefore, the performance of the graphene-based nano roll in the fields of flexible electronic devices, sensors and the like is superior to that of other one-dimensional nano roll materials.
According to the invention, the advantages that the graphene nano-roll material is easy to disperse, the specific surface area is large, and the high loading capacity of the graphene nano-roll material on electroactive substances and biomolecules is utilized to provide more uniform and larger electroactive site distribution, and the like are utilized, so that the clenbuterol hydrochloride antibody is loaded on the surface of the electrode, the effective fixation on the electrode is realized, and the sensitivity of the prepared electrochemical immunosensor is effectively improved.
Disclosure of Invention
The invention aims to provide a preparation method and application of a clenbuterol hydrochloride electrochemical sensor. The clenbuterol hydrochloride electrochemical sensor has the advantages of simple operation, low cost, high detection sensitivity and the like.
The method for preparing the electrochemical sensor by solidifying the clenbuterol hydrochloride antibody by the graphene nanocolloid is characterized in that the clenbuterol hydrochloride antibody is coated on graphene by dropwise adding the clenbuterol hydrochloride antibody on a modified electrode due to the fact that the graphene has a porous structure, and silica sol and graphene solution prepared on the surface modification of a glassy carbon electrode. And obtaining the electrochemical sensor for detecting the clenbuterol hydrochloride.
The preparation method comprises the following steps:
1. purifying graphene oxide:
adding 5-8 g of graphene oxide into 20 ml of hydrogen peroxide, stirring for 10 minutes, filtering, leaching, and freeze-drying to obtain purified graphene oxide.
The filtration leaching is to use 20 ml of deionized water to carry out filtration leaching for 2 times, and after the filtration leaching is finished, the purified graphene oxide is freeze-dried and is reserved after the drying is finished;
preparation of SI @ graphene solution:
weighing 0.01-0.1 g of purified graphene oxide, adding 50 ml of deionized water, and ultrasonically dispersing in an ultrasonic device for 60 minutes; and continuously adding 3-5 g of water glass, 1-3 ml of ammonia water and 0.03-0.08 g of hexadecyl trimethyl ammonium chloride, performing ultrasonic dispersion for 60 minutes again to obtain an SI @ graphene solution, and standing for 48 hours at 4 ℃ after 2 times of dispersion.
Preparing an SI @ graphene nanocolloid solution:
and (3) taking out 10 ml of SI @ graphene solution, dropwise adding 0.2-2 g of hydrazine hydrate, stirring for 60 minutes, and then quickly immersing the reactor into liquid nitrogen for quick freezing to obtain the SI @ graphene nano roll for later use.
4. And (4) taking out the SI @ graphene nano-roll prepared in the step (3), standing for 4 hours at room temperature, and naturally thawing.
5. Taking out 1-2 ml of unfrozen SI @ graphene nano roll solution, dropwise adding the solution on a glassy carbon electrode, and performing vacuum drying for 1h at the temperature of 30 ℃ to enable colloidal particles to be adsorbed on the glassy carbon electrode to form an adsorption adhesive film.
6. And continuously dropwise adding 5-12 drops of clenbuterol hydrochloride antibody solution (50 mg/L) into the adsorption film on the glassy carbon electrode, uniformly coating by rotating at a medium speed, and then drying in vacuum for 5-12 h at the temperature of 30 ℃ to obtain the clenbuterol hydrochloride electrochemical sensor.
Drawings
Figure 1 is a simulated graph of frozen crimp of graphene under cooling conditions.
Fig. 2 is a linear relation curve diagram of peak current and clenbuterol hydrochloride in a specific concentration interval when the sensor constructed by the invention is applied to clenbuterol hydrochloride detection.
Detailed Description
The following examples illustrate the invention in detail: the present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a process are given, but the scope of the present invention is not limited to the following embodiments.
Example 1:
1. purifying graphene oxide:
and adding 5 g of graphene oxide into 20 ml of hydrogen peroxide, stirring for 10 minutes, filtering, leaching, and freeze-drying to obtain purified graphene oxide for later use. The filtration rinsing step was 2 filtration rinsing with 20 ml of deionized water.
Preparation of SI @ graphene solution:
weighing 0.05 g of purified graphene oxide, adding the purified graphene oxide into 50 ml of deionized water, and carrying out ultrasonic dispersion in an ultrasonic device for 60 minutes; and continuously adding 3 g of water glass, 3 ml of ammonia water and 0.05 g of hexadecyl trimethyl ammonium chloride, and performing ultrasonic dispersion for 60 minutes again to obtain the SI @ graphene solution. After the completion of the 2-time dispersion, the mixture was left at 4 ℃ for 48 hours.
Preparing an SI @ graphene nanocolloid solution: and (3) taking 10 ml of SI @ graphene solution out, dropwise adding 1 g of hydrazine hydrate, stirring for 60 minutes, and then quickly immersing the reactor into liquid nitrogen for quick freezing to obtain the SI @ graphene nano roll as shown in the attached drawing 1.
4. And (4) taking out the SI @ graphene nano coil solution prepared in the step (3), standing for 4 hours at room temperature, and unfreezing the refrigerating fluid.
5. Taking out 1 ml of unfrozen SI @ graphene nano coil solution, dropwise adding the solution on a glassy carbon electrode, and carrying out vacuum drying for 1h at the temperature of 30 ℃ to enable colloidal particles to be adsorbed on the glassy carbon electrode;
6. continuously dropwise adding 5 drops of clenbuterol hydrochloride antibody solution (50 mg/L) into the adsorption film on the glassy carbon electrode, uniformly coating by rotating at a medium speed, and then drying in vacuum for 5 hours at the temperature of 30 ℃ to obtain the clenbuterol hydrochloride electrochemical sensor.
Application of clenbuterol hydrochloride electrochemical sensor:
the clenbuterol hydrochloride electrochemical sensor prepared by the preparation method is characterized in that a three-electrode system serving as a working electrode is placed in a measuring solution with a certain concentration range, and peak current of a CV curve is recorded. And due to the excellent selectivity of the clenbuterol hydrochloride antibody, the clenbuterol hydrochloride antibody is only combined with clenbuterol hydrochloride, so that the phenomenon of remarkable reduction of peak current can be generated only under the condition that the clenbuterol hydrochloride exists, the existence of the clenbuterol hydrochloride is confirmed, and the successful construction of the sensor is confirmed.
The sensor constructed by the invention is applied to the detection of the target component clenbuterol hydrochloride in an actual sample, and the detection rate is 0.05 multiplied by 10-7-8×10-7mol/L is good in linear relation of detected peak current and concentration, R =0.9914, as shown in fig. 2.
Example 2:
1. purifying graphene oxide:
and adding 8 g of graphene oxide into 20 ml of hydrogen peroxide, stirring for 10 minutes, filtering, leaching, and freeze-drying. In the filtering and leaching step, 20 ml of deionized water is used for filtering and leaching for 2 times, and after the filtering and leaching are finished, the purified graphene oxide is freeze-dried and is reserved after the drying is finished;
preparation of SI @ graphene solution:
weighing 0.01 g of purified graphene oxide, adding the purified graphene oxide into 50 ml of deionized water, and carrying out ultrasonic dispersion in an ultrasonic device for 60 minutes; and continuously adding 5 g of water glass, 1 ml of ammonia water and 0.08 g of hexadecyl trimethyl ammonium chloride, carrying out ultrasonic dispersion again for 60 minutes, and standing for 48 hours at 4 ℃ after 2 times of dispersion.
Preparing an SI @ graphene nanocolloid solution:
and (3) taking 10 ml of SI @ graphene solution, dropwise adding 2 g of hydrazine hydrate, stirring for 60 minutes, and quickly immersing the reactor into liquid nitrogen for quick freezing to obtain the SI @ graphene nano roll for later use.
4. Taking out the SI @ graphene nanocolloid solution prepared in the step 3, standing for 2 hours at room temperature, unfreezing the refrigerating fluid,
5. taking out 2 ml of unfrozen SI @ graphene nano coil solution, dropwise adding the solution on a glassy carbon electrode, and carrying out vacuum drying for 1h at the temperature of 30 ℃ to enable colloidal particles to be adsorbed on the glassy carbon electrode;
6. and continuously dropwise adding 12 drops of clenbuterol hydrochloride antibody solution (50 mg/L) into the adsorption film on the glassy carbon electrode, uniformly coating by rotating at a medium speed, and then drying in vacuum for 8 hours at the temperature of 30 ℃ to obtain the clenbuterol hydrochloride electrochemical sensor.
Example 3:
1. purifying graphene oxide:
and adding 6 g of graphene oxide into 20 ml of hydrogen peroxide, stirring for 10 minutes, filtering, leaching, and freeze-drying. In the filtering and leaching step, 20 ml of deionized water is used for filtering and leaching for 2 times, and after the filtering and leaching are finished, the purified graphene oxide is freeze-dried and is reserved after the drying is finished;
preparation of SI @ graphene solution:
weighing 0.07 g of purified graphene oxide, adding the purified graphene oxide into 50 ml of deionized water, and carrying out ultrasonic dispersion in an ultrasonic instrument for 60 minutes; 4 g of water glass, 2 ml of ammonia water and 0.03 g of hexadecyl trimethyl ammonium chloride are continuously added, ultrasonic dispersion is carried out for 60 minutes again, and the mixture is placed for 48 hours at 4 ℃ after 2 times of dispersion.
Preparing an SI @ graphene nanocolloid solution:
and (3) taking 10 ml of SI @ graphene solution, dropwise adding 1.0 g of hydrazine hydrate, stirring for 60 minutes, and quickly immersing the reactor into liquid nitrogen for quick freezing to obtain the SI @ graphene nano roll for later use.
4. Taking out the SI @ graphene nanocolloid solution prepared in the step 3, standing for 3 hours at room temperature, unfreezing the refrigerating fluid,
5. taking out 1 ml of unfrozen SI @ graphene nano coil solution, dropwise adding the solution on a glassy carbon electrode, and carrying out vacuum drying for 1h at the temperature of 30 ℃ to enable colloidal particles to be adsorbed on the glassy carbon electrode;
6. continuously dropwise adding 12 drops of clenbuterol hydrochloride antibody solution (50 mg/L) into the adsorption film on the glassy carbon electrode, uniformly coating by rotating at a medium speed, and then drying in vacuum for 12 hours at the temperature of 30 ℃ to obtain the clenbuterol hydrochloride electrochemical sensor.
Claims (3)
1. A preparation method of a graphene nano-roll cured clenbuterol hydrochloride sensor is characterized by comprising the following steps:
1) purification of graphene oxide
Adding 5-8 g of graphene oxide into 20 ml of hydrogen peroxide, stirring for 10 minutes, filtering, leaching, and freeze-drying to obtain purified graphene oxide;
2) preparation of SI @ graphene solution
Weighing 0.01-0.1 g of purified graphene oxide, adding 50 ml of deionized water, and ultrasonically dispersing in an ultrasonic device for 60 minutes; continuously adding 3-5 g of water glass, 1-3 ml of ammonia water and 0.03-0.08 g of hexadecyl trimethyl ammonium chloride, performing ultrasonic dispersion for 60 minutes again to obtain an SI @ graphene solution, and standing for 48 hours at 4 ℃ after 2 times of dispersion;
3) preparation of SI @ graphene nanocolloid solution
Taking out 10 ml of SI @ graphene solution, dropwise adding 0.2-2 g of hydrazine hydrate, stirring for 60 minutes, quickly immersing a reactor into liquid nitrogen, and quickly freezing to obtain an SI @ graphene nano roll for later use;
4) taking out the SI @ graphene nano roll prepared in the step 3, standing for 4 hours at room temperature, and naturally thawing;
5) taking out 1-2 ml of unfrozen SI @ graphene nano roll solution, dropwise adding the solution on a glassy carbon electrode, and performing vacuum drying for 1h at the temperature of 30 ℃ to enable colloidal particles to be adsorbed on the glassy carbon electrode to form an adsorption adhesive film;
6) and continuously dropwise adding 5-12 drops of clenbuterol hydrochloride antibody solution into the adsorption film on the glassy carbon electrode, uniformly coating by rotating at a medium speed, and then drying in vacuum for 5-12 hours at the temperature of 30 ℃ to obtain the clenbuterol hydrochloride electrochemical sensor.
2. The method for preparing the graphene nanocolloid-cured clenbuterol hydrochloride sensor according to claim 1, wherein the method comprises the following steps: the filtration elution is 2 times of filtration elution by using 20 ml of deionized water.
3. The method for preparing an electrochemical sensor by using the graphene nanocolloid solidified clenbuterol hydrochloride antibody according to claim 1, wherein the content of the clenbuterol hydrochloride antibody solution is 50 mg/L.
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