CN113511686B - Carbon quantum dot@MnFe 2 O 4 Is used for preparing and electrochemical sensing application of the same - Google Patents

Carbon quantum dot@MnFe 2 O 4 Is used for preparing and electrochemical sensing application of the same Download PDF

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CN113511686B
CN113511686B CN202110357825.9A CN202110357825A CN113511686B CN 113511686 B CN113511686 B CN 113511686B CN 202110357825 A CN202110357825 A CN 202110357825A CN 113511686 B CN113511686 B CN 113511686B
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吴海燕
闫煜
王子威
夏芯
桑敏
张国华
周文娟
邱凤仙
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Abstract

The invention discloses a carbon quantum dot @ MnFe 2 O 4 Is prepared from the raw materials by a chemical method, and is applied to electrochemical sensing, and belongs to the field of material science. The invention is realized by mixing MnCl 2 ·4H 2 O、FeCl 3 ·6H 2 O, naAc and shaddock peel powder are mixed in glycol and heated for 6 to 12 hours at 160 to 200 ℃ to prepare the carbon quantum dot@MnFe 2 O 4 . The invention uses a simple one-step solvothermal reaction to lead the carbon quantum dots to be in contact with ferrite material (MnFe 2 O 4 ) The composite, the CQDs@MnFe with excellent electrochemical performance is prepared by utilizing good water solubility and higher specific surface area of the carbon quantum dots, and solving the problem of agglomeration of ferrite materials 2 O 4 . The material can be used as an electrochemical modification material, combines a molecular imprinting technology, realizes quantitative detection of glucose content by a synergistic effect, and has strong anti-interference performance.

Description

Carbon quantum dot@MnFe 2 O 4 Is used for preparing and electrochemical sensing application of the same
Technical Field
The invention relates to a carbon quantum dot @ MnFe 2 O 4 Is prepared from the raw materials by a chemical method, and is applied to electrochemical sensing, and belongs to the field of material science.
Background
MnFe 2 O 4 Is a ferrite nano material, and has relatively stable chemical property, relative specific surface area, saturation magnetization and better dielectric property. MnFe 2 O 4 The material has been widely used in electrocatalytic oxygen evolution reaction, adsorption of environmental pollutants and as lightCatalysts, etc., but there has been little attention paid to their electrochemical performance. The single ferrite nano material has various defects, such as reduced conductivity caused by easy agglomeration of nano particles, reduced specific surface area and the like, so that the application of the ferrite nano material is greatly restricted.
Carbon Quantum Dots (CQDs) are nano materials with the size smaller than 10nm, and are widely focused by researchers due to the excellent optical performance, low toxicity, good water solubility, good biocompatibility and simple preparation method.
How to solve the agglomeration of the ferrite nano material and improve the electrochemical performance of the ferrite nano material has important significance for the development of the ferrite nano material.
Disclosure of Invention
The invention aims to provide a preparation method and application of a carbon quantum dot coated magnetic ferrite. The invention uses a simple one-step solvothermal reaction to lead the carbon quantum dots to be in contact with ferrite material (MnFe 2 O 4 ) The composite, the CQDs@MnFe with excellent electrochemical performance is prepared by utilizing good water solubility and higher specific surface area of the carbon quantum dots, and solving the problem of agglomeration of ferrite materials 2 O 4 . The material can be used as an electrochemical modification material, and combines with a molecular imprinting technology to realize quantitative detection of the glucose content under the synergistic effect.
Specifically, the invention firstly provides a carbon quantum dot@MnFe 2 O 4 The preparation method of (2), the method comprises the following steps: dissolving a manganese source and an iron source in ethylene glycol according to the molar ratio of elements Mn to Fe of 4:1-1:5, then adding NaAc and a carbon source, mixing, transferring the mixture into a reactor, reacting for 6-12h at 160-200 ℃, cooling, washing and drying after the reaction is finished, thus obtaining the carbon quantum dot@MnFe 2 O 4 。
In one embodiment of the invention, the manganese source comprises MnCl 2 ·4H 2 O、MnSO 4 、Mn(CH 3 COO) 2 ·4H 2 Any one or more of O; the iron source comprises FeCl 3 ·6H 2 O、Fe 2 (SO 4 ) 3 、Fe(NO 3 ) 3 Any one or more of the following.
In one embodiment of the invention, the carbon source comprises any one or more of shaddock peel powder, peanut shells and willow leaves.
In one embodiment of the invention, the molar ratio of the elements Mn and Fe is preferably 1:2.
In one embodiment of the present invention, the mass g molar ratio of the carbon source to the elemental Fe in the iron source is 1:0.001-0.01.
In one embodiment of the present invention, the mass ratio of the NaAc to the carbon source is 1 to 5:1.
In one embodiment of the invention, the preparation temperature is preferably 200℃for 12h.
In one embodiment of the invention, the reactor is a high pressure reactor.
In one embodiment of the present invention, the washing is performed with ultrapure water and ethanol, respectively, several times.
In one embodiment of the present invention, the drying is preferably vacuum drying, and the drying conditions are: drying at 40-80 deg.c for 18-36 hr.
Secondly, the invention also provides the carbon quantum dot@MnFe prepared by the preparation method 2 O 4 。
Again, the invention provides a molecularly imprinted sensor, which is prepared by the following method:
(1) Taking the prepared carbon quantum dot @ MnFe 2 O 4 Diluting with ultrapure water, adding a film forming agent, dripping on a polished glassy carbon electrode, and drying at 30-80 ℃ for 5-60min to obtain an electrochemical sensing matrix;
(2) Placing the electrochemical sensing matrix prepared in the step (1) into a phosphoric acid buffer solution containing 3-aminophenylboric acid and glucose, and performing electropolymerization for 10-40 circles within the potential range of 0-1.2V at the sweeping speed of 0.01-0.2V S -1 ；
(3) Eluting the template molecules by using the eluent to obtain the modified electrode prepared in the step (2).
In one embodiment of the present invention, the film forming agent is any one of chitosan, cellulose acetate or Nafion, preferably chitosan.
In one embodiment of the invention, the film former is combined with carbon quantum dots @ MnFe 2 O 4 The volume ratio of the addition amount of (2) is 1:1 to 5:1.
in one embodiment of the present invention, the concentrations of the 3-aminophenylboronic acid and glucose are 1.0 to 1.5mmol L, respectively -1 And 0.645 to 3.87mmol L -1 。
In one embodiment of the invention, the phosphate buffer solution has a ph=9.
In one embodiment of the invention, the eluent in step (3) is acetic acid/sodium acetate buffer (ph=4), and the elution is performed by immersing the modified electrode in the eluent for 5 to 30min, preferably 15min.
Finally, the invention also provides application of the molecular imprinting sensor in glucose detection.
The invention has the beneficial effects that:
the invention combines the advantages of good dielectric property of ferrite material and the advantages of larger specific surface area, water solubility and better conductivity of carbon quantum dots, and prepares the carbon quantum dots @ MnFe by a one-step solvothermal method 2 O 4 Is not susceptible to agglomeration. The material is used as an electrode modification material, and the molecular imprinting sensor is prepared by combining a molecular imprinting technology, so that the material can be applied to quantitative detection of glucose. In the invention, the carbon quantum dot@MnFe 2 O 4 The preparation method is simple and the cost is low; the material is used as an electrode modification material, so that the conductivity of a commercial electrode matrix is improved, and the detection performance of glucose as a target is effectively improved by combining a molecular imprinting technology.
Drawings
FIG. 1 carbon Quantum dot @ MnFe prepared in example 1 2 O 4 Electron microscope characterization map of (2).
FIG. 2 different modified electrodes in potassium ferricyanide solutionComprises a Bare glass carbon electrode (Bare GCE), a chitosan modified electrode (CS/GCE), mnFe 2 O 4 Modified electrode (MnFe) 2 O 4 CQDs modified electrode (CQDs/CS/GCE) and CQDs@MnFe 2 O 4 Modified electrode (CQDs@MnFe) 2 O 4 /CS/GCE)。
FIG. 3 is a linear plot of the response of the molecularly imprinted sensing electrode prepared in example 3 to glucose at different concentrations.
FIG. 4 shows the results of interference resistance studies of the molecularly imprinted sensing electrode prepared in example 3.
Detailed Description
The present invention is further described below with reference to examples, but embodiments of the present invention are not limited thereto.
Example 1
CQDs@MnFe 2 O 4 Is prepared from
MnCl is added to 2 ·4H 2 O and FeCl 3 ·6H 2 O was dissolved in 60mL of ethylene glycol at a molar ratio of 1:2 (mass 0.49g:1.35g, respectively) to form a clear solution. Subsequently, naAc (4.1 g) and shaddock peel powder (1.0 g) were added to the above solution, followed by vigorous stirring at 300r/min at room temperature. The mixture was then transferred to a 100mL stainless steel autoclave lined with polytetrafluoroethylene and heated at 200 ℃ for 12h. After the reaction was completed, the autoclave was naturally cooled to room temperature. The black product is washed by ultrapure water and ethanol for several times, and then dried in a vacuum oven at 60 ℃ for 24 hours, and the prepared material is CQDs@MnFe 2 O 4 Fig. 1 is an electron microscope image of a ferrite material coated with the prepared carbon quantum dots, and the composite material is spherical and has a particle size of 300-800 nm.
Example 2
CQDs@MnFe 2 O 4 Modifying the electrochemical properties of the electrode:
10mg/mLCQDs@MnFe of the material prepared in example 1 2 O 4 The electrode substrate modifying material is prepared by mixing the electrode substrate modifying material with 1% chitosan solution according to the volume ratio of 3:1, uniformly mixing, then dripping the mixture on a polished glassy carbon electrode, and placing the polished glassy carbon electrode at 60 DEG CDrying in an oven for 20min to obtain an electrochemical sensing matrix, which is marked as CQDs@MnFe 2 O 4 /CS/GCE。
CQDs and MnFe prepared in comparative examples 1 and 2 were prepared according to the method of this example 2 O 4 The electrochemical sensing matrix prepared is also respectively marked as CQDs/CS/GCE and MnFe 2 O 4 /CS/GCE。
Comparing the cyclic voltammetry properties of the different modified electrodes in potassium ferricyanide solution, see FIG. 2 (where Bare GCE represents Bare glassy carbon electrode and CS/GCE represents chitosan modified electrode), it can be seen that CQDs/CS/GCE has almost no current, and when CQDs@MnFe is used 2 O 4 After modification, the prepared CQDs@MnFe 2 O 4 The electrochemical performance of the/CS/GCE is optimal, and the measured current value is the largest and is obviously higher than that of MnFe 2 O 4 /CS/GCE. Therefore, the CQDs@MnFe provided by the invention 2 O 4 The material is used as an electrode modification material, so that the conductivity of a commercial electrode matrix is greatly improved.
Example 3 preparation of a molecularly imprinted sensor
The electrochemical sensing matrix prepared in example 2 is used as a working electrode, an Ag/AgCl electrode is used as a reference electrode, a platinum wire is used as an auxiliary electrode, and the electrochemical sensing matrix is placed in a molar ratio of 1:1 in a phosphate buffer solution (ph=9) of 3-aminophenylboronic acid and glucose, electropolymerized for 20 cycles at a potential ranging from 0V to 1.2V, and a sweep rate of 0.05V S -1 Eluting the template molecules by using eluent to obtain the molecular imprinting sensor with recognition performance on glucose.
(1) Investigation of glucose detection Performance
The detection performance of the blotting membrane electrode on glucose was studied by Differential Pulse Voltammetry (DPV). The results of the study are shown in FIG. 3, which shows that the logarithmic value of the glucose concentration is in linear relation with the variation value of the peak current in the concentration range of 0.1-600 mu M, R 2 The = 0.9602 indicates that the molecular imprinting sensor prepared by the method can accurately measure the glucose content.
CQDs prepared in comparative example 1 were prepared according to the method of this example to prepare corresponding molecularly imprinted sensors without detection of dextranGlucose function. MnFe prepared in comparative example 2 2 O 4 A molecular imprinting sensor was prepared according to the method of this example for detecting glucose, and it was found that only glucose with a concentration of 80. Mu.M to 300. Mu.M could be detected. The CQDs@MnFe prepared by the invention 2 O 4 The sensitivity of the CS/GCE molecularly imprinted sensor is high, and the linear range is wider for detecting glucose.
(2) Anti-interference study
The blotting membrane electrode prepared in example 2 was used as a working electrode, an Ag/AgCl electrode was used as a reference electrode, and a platinum wire was used as an auxiliary electrode. Glucose, fructose, lactose and sucrose were detected at a concentration of 100. Mu.M by using DPV as a detection means. The research result is shown in fig. 4, and shows that the prepared imprinted membrane electrode has higher response to glucose and relatively lower response value to other test objects. The prepared imprinted membrane electrode has specific recognition performance on glucose.
Example 4
(1) Preparation of modified electrode: mnCl is added to 2 ·4H 2 O and FeCl 3 ·6H 2 O is in a molar ratio of 1:1 (MnCl) 2 ·4H 2 O was 0.49 g) dissolved in 60mL of ethylene glycol to form a clear solution. Subsequently, naAc (4.1 g) and shaddock peel powder (1.0 g) were added to the above solution, followed by vigorous stirring at room temperature. The mixture was then transferred to a 100mL stainless steel autoclave lined with polytetrafluoroethylene and heated at 160 ℃ for 12h. After the reaction was completed, the autoclave was naturally cooled to room temperature. The resulting black product was washed several times with ultrapure water and ethanol, and then dried in a vacuum oven at 60 ℃ for 24 hours. Mixing the material with 1% chitosan solution in a volume ratio of 3:1, after uniformly mixing, dripping the mixture on a polished glassy carbon electrode, and drying the mixture at 60 ℃ for 20 minutes to obtain the modified electrode.
(2) Molecular imprinting electrochemical sensor: placing the modified electrode prepared in the step (1) as a working electrode, an Ag/AgCl electrode as a reference electrode and a platinum wire as an auxiliary electrode in a molar ratio of 1:1 in a phosphate buffer solution (pH=9) of 3-aminophenylboronic acid and glucose, electropolymerization is carried out for 20 cycles at a potential ranging from 0V to 1.2V, with a sweeping speed of 0.1V S -1 Eluting the template molecules by using eluent to obtain the molecular imprinting sensor with recognition performance on glucose.
Example 5
(1) Preparation of modified electrode: mnSO is carried out 4 And FeCl 3 ·6H 2 O was dissolved in 60mL of ethylene glycol at a molar ratio of 1:2 (mass of 0.18g:1.35g, respectively) to form a clear solution. Subsequently, naAc (2.05 g) and peanut hulls (2.0 g) were added to the above solution, followed by vigorous stirring at room temperature. The mixture was then transferred to a 100mL stainless steel autoclave lined with polytetrafluoroethylene and heated at 200 ℃ for 12h. After the reaction was completed, the autoclave was naturally cooled to room temperature. The resulting black product was washed several times with ultrapure water and ethanol, and then dried in a vacuum oven at 60 ℃ for 24 hours. The material and 1% chitosan solution are mixed according to the volume ratio of 3:1, after uniformly mixing, dripping the mixture on a polished glassy carbon electrode, and drying the mixture at 60 ℃ for 20 minutes to obtain the modified electrode.
(2) Molecular imprinting electrochemical sensor: placing the modified electrode prepared in the step (1) as a working electrode, an Ag/AgCl electrode as a reference electrode and a platinum wire as an auxiliary electrode in a molar ratio of 1:1 in a phosphate buffer solution (pH=9) of 3-aminophenylboronic acid and glucose, electropolymerization is carried out for 10 cycles at a potential ranging from 0V to 1.2V, with a sweeping speed of 0.1V S -1 Eluting the template molecules by using eluent to obtain the molecular imprinting sensor with recognition performance on glucose.
Comparative example 1 preparation of CQDs
NaAc (4.1 g) and shaddock peel powder (1.0 g) were added to 60mL of ethylene glycol, followed by vigorous stirring at room temperature, and the mixture was transferred to a 100mL polytetrafluoroethylene-lined stainless steel autoclave and heated at 200℃for 12 hours. After the reaction was completed, the autoclave was naturally cooled to room temperature, washed several times with ultrapure water and ethanol, and then dried in a vacuum oven at 60℃for 24 hours, and the prepared material was CQDs.
Comparative example 2 MnFe 2 O 4 Is prepared from
MnCl is added to 2 ·4H 2 O and FeCl 3 ·6H 2 O is dissolved according to the mol ratio of 1:2 (the mass is 0.49g to 1.35g respectively)NaAc (4.1 g) was added simultaneously to 60mL of ethylene glycol and vigorously stirred to form a clear solution. The mixture was then transferred to a 100mL stainless steel autoclave lined with polytetrafluoroethylene and heated at 200 ℃ for 12h. After the reaction was completed, the autoclave was naturally cooled to room temperature. Washing the obtained product with ultrapure water and ethanol for several times, and drying in a vacuum oven at 60deg.C for 24 hr to obtain MnFe material 2 O 4 。
Comparative example 3
CQDs@MnFe 2 O 4 Preparation of the Material
MnCl is added to 2 ·4H 2 O and FeCl 3 ·6H 2 O was dissolved in 60mL of ethylene glycol at a molar ratio of 1:2 to form a clear solution. Subsequently, naAc (4.1 g) and shaddock peel powder (1.0 g) were added to the above solution, followed by vigorous stirring at 300r/min at room temperature. The mixture was then transferred to a 100mL stainless steel autoclave lined with polytetrafluoroethylene and heated at 120 ℃ for 6h. After the reaction was completed, the autoclave was naturally cooled to room temperature. The black product is washed by ultrapure water and ethanol for several times, and then dried in a vacuum oven at 60 ℃ for 24 hours, and the prepared material is CQDs@MnFe 2 O 4 . The prepared CQDs@MnFe 2 O 4 CQDs@MnFe material prepared according to example 2 2 O 4 The electrochemical response of the modified electrode is lower than that of the bare electrode, and is 40% of the electrochemical response signal of the bare electrode.
While the invention has been described with reference to the preferred embodiments, it is not limited thereto, and various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (7)

1. Carbon quantum dot@MnFe containing material 2 O 4 Characterized in that the carbon quantum dot @ MnFe 2 O 4 The preparation of the composition comprises the following steps:
dissolving a manganese source and an iron source in ethylene glycol according to the mol ratio of elements Mn to Fe of 4:1-1:5, and then addingAdding NaAc and a carbon source, mixing, transferring the mixture into a reactor, reacting for 12 hours at 200 ℃, cooling, washing and drying after the reaction is finished, thus obtaining the carbon quantum dot@MnFe 2 O 4 The method comprises the steps of carrying out a first treatment on the surface of the The carbon source is shaddock peel powder.
2. A carbon quantum dot @ MnFe-containing material as claimed in claim 1 2 O 4 Characterized in that the carbon quantum dot @ MnFe 2 O 4 Manganese source in the preparation of (a) comprises MnCl 2 ·4H 2 O、MnSO 4 、Mn(CH 3 COO) 2 ·4H 2 Any one or more of O; the iron source comprises FeCl 3 ·6H 2 O、Fe 2 (SO 4 ) 3 、Fe(NO 3 ) 3 Any one or more of the following.
3. A carbon quantum dot @ MnFe-containing material as claimed in claim 1 2 O 4 Characterized in that the carbon quantum dot @ MnFe 2 O 4 In the preparation of (1), the mass ratio of NaAc to carbon source is 1-5:1.
4. The molecular imprinting sensor is characterized by being prepared by the following steps:
(1) Taking the carbon quantum dot @ MnFe of claim 1 2 O 4 After dilution, adding a film forming agent, dripping on a polished glassy carbon electrode, and drying for 5-60min at 30-80 ℃ to obtain an electrochemical sensing matrix;
(2) The electrochemical sensing matrix prepared in the step (1) is placed in a phosphoric acid buffer solution containing 3-aminophenylboric acid and glucose, and is subjected to electropolymerization for 10-40 circles within the potential range of 0V-1.2V, and the sweeping speed is 0.01-0.2V S -1 ；
(3) Eluting the template molecules by using the eluent to obtain the modified electrode prepared in the step (2).
5. The molecular imprinting sensor according to claim 4, wherein the film-forming agent is any one of chitosan, cellulose acetate or Nafion.
6. Use of a molecularly imprinted sensor according to claim 4 or 5 for glucose detection.
7. A composition comprising carbon quantum dots @ MnFe as defined in claim 1 2 O 4 The electrode of (2) is used for detecting glucose.
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