CN114371200B - High-stain-resistance MXene-ERHG electrochemical sensor and preparation method thereof - Google Patents
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
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Abstract
The invention relates to a high-stain-resistance MXene-ERHG electrochemical sensor and a preparation method thereof, wherein the preparation method comprises the following steps: (1) Preparation of Ti by liquid etching 3 AlC 2 MXene; (2) By H 2 O 2 Preparing a porous graphite oxide solution (HGO) by an etching method; (3) uniformly mixing MXene and HGO by ultrasonic waves to obtain MXene-HGO; (4) Dripping the solution obtained in the step (3) on the pretreated GCE to obtain MXene-HGO/GCE, and draining for later use; (5) And (3) carrying out electrochemical reduction on the MXene-HGO/GCE obtained in the step (4) in PBS solution by adopting a Cyclic Voltammetry (CV) method to obtain the MXene-ERHG/GCE. The prepared MXene-ERHG sensor is expected to be used as an anti-fouling substrate to enhance and stabilize electrochemical signals. Compared with the prior art, the MXene-ERHG sensor prepared by the method is expected to be used as an anti-fouling substrate to strengthen and stabilize electrochemical signals.
Description
Technical Field
The invention belongs to the technical field of analysis and test, and relates to a high-stain-resistance MXene-ERHG electrochemical sensor and a preparation method thereof.
Background
Electrochemical detection of disease markers in complex biological fluids (e.g., serum, whole blood, and interstitial fluid) is widely used for early diagnosis, prevention, and treatment of disease. However, when coexisting species (e.g., biomacromolecules, proteins, and cells) bind to the electrode surface in a non-specific manner, significant decreases in electrochemical properties such as current response and detection sensitivity are often encountered. In addition, non-specific binding of proteins (e.g., fibrinogen) to tissue implantable sensing interfaces can induce adverse immune response cascades. To overcome these problems, chemical modification of the sensing interface by various hydrophilic coatings is one of the main strategies.
While MXene is of great interest as a novel two-dimensional material, due to its unique hydrophilicity, conductivity and biocompatibility, it is extremely susceptible to oxidation. Electrochemical reduction porous graphene (ERHG) is taken as one of important derivatives of graphene-based materials, has abundant netlike micropores and increased specific surface area, and can effectively improve the electron transfer capability and mass transfer capability of the sensor, but the graphene has good protein adsorption capability, and is unfavorable for biological anti-fouling. Therefore, the material has obvious defects in aspects of anti-fouling performance and the like. The present invention has been made to solve the above-described problems.
Disclosure of Invention
The invention aims to provide an MXene-ERHG electrochemical sensor with high pollution resistance and a preparation method thereof, and an electrochemical sensor which resists the nonspecific binding of proteins in complex biological fluid and simultaneously meets the requirements of better interface electron transfer capacity and sensitivity is prepared by utilizing the synergistic effect of MXene and ERHG.
The aim of the invention can be achieved by the following technical scheme:
one of the technical schemes of the invention provides a high-stain-resistance MXene-ERHG electrochemical sensor, which is formed by compounding MXene and ERHG.
Through compounding MXene and HGO, the MXene-ERHG interface obtained through electrochemical reduction can not only meet the hydrophilicity, but also have good electron transfer capability, so that the MXene-ERHG biological interface can resist the nonspecific combination of proteins in complex biological fluid, and also enhance the interface electron transfer capability.
The second technical scheme of the invention provides a preparation method of the high-stain-resistance MXene-ERHG electrochemical sensor, which comprises the following steps:
(1) Mixing an MXene solution with an HGO solution and performing ultrasonic treatment to obtain an MXene-HGO solution;
(2) Dropping the MXene-HGO solution on the GCE electrode, and drying to obtain the MXene-HGO/GCE;
(3) And (3) placing the MXene-HGO/GCE in a PBS solution, and performing electrochemical reduction to obtain the MXene-ERHG/GCE, namely the target product.
Further, in the step (1), the concentration of the MXene solution is 0.5-5 mg/mL.
Further, in the step (1), the concentration of the HGO solution is 0.5 to 5mg/mL.
Further, in the step (1), the addition volume ratio of the MXene solution to the HGO solution is 0.8-1.2:1, preferably 1:1.
Further, in the step (1), the MXene solution used is Ti 3 AlC 2 The MXene suspension is prepared by a liquid etching method.
Further, in the step (1), the HGO solution is H 2 O 2 And (5) preparing by an etching method.
Further, in the step (2), the GCE electrode is further subjected to a pretreatment, and the pretreatment process specifically includes: firstly, sequentially polishing GCE electrodes (the diameter of which is generally 3 mm) by adopting alumina with the particle diameters of 1 mu m,0.3 mu m and 0.05 mu m, then sequentially placing the GCE electrodes in ethanol and ultrapure water for ultrasonic cleaning after polishing, and finally, drying by using nitrogen flow to finish the GCE electrodes.
Further, in the step (3), the PBS solution was adjusted to pH 9.23, and subjected to oxygen removal treatment.
Further, in the step (3), the electrochemical reduction is carried out by cyclic voltammetry, the scanning range is-1.5V-0.5V, and the scanning rate is 20 mV.s -1 。
The invention adopts the electrochemical reduction method to reduce the MXene-HGO to obtain the MXene-ERHG, firstly, the HGO and the MXene surface simultaneously contain rich oxygen-containing functional groups, the chemical combination effect enables the HGO to coat the MXene, thereby effectively protecting the MXene, secondly, the microporous structure of the ERHG subjected to electrochemical reduction provides a guarantee for good electron transfer capability of an electrochemical sensor, and finally, the synergistic effect of the two provides a guarantee for detecting the disease marker of the MXene-ERHG in complex biological liquid.
Compared with the prior art, the invention has the following advantages:
(1) The MXene-ERHG electrochemical sensor prepared by the invention has good linear range, lower detection limit and remarkable anti-fouling performance.
(2) The invention has simple and feasible operation process and stable material performance.
Drawings
FIG. 1 is a schematic diagram of the workflow of an electrochemical sensor of the present invention.
Fig. 2 is a DA detection performance test chart of an electrochemical sensor, wherein 2 (a) and 2 (d) are CV and DPV charts of example 2, 2 (b) and 2 (e) are CV and DPV charts of comparative example 1, and 2 (c) and 2 (f) are CV and DPV charts of comparative example 2.
FIG. 3 shows the anti-fouling performance test effect of ERHG and MXene-ERHG.
FIG. 4 is a graph showing the effect of MXene-ERHG in reproducibility and long-term stability testing in artificial cerebrospinal fluid.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples. The present embodiment is implemented on the premise of the technical scheme of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to the following examples.
In the following examples, ti was prepared by liquid etching 3 AlC 2 The procedure for MXene suspensions is described in detail in the following references ([ 1 ]]G.Jia,A.Zheng,X.Wang,L.Zhang,L.Li,C.Li,Y.Zhang,L.Cao,Flexible,biocompatible and highly conductive MXene-graphene oxide film for smart actuator and humidity sensor,Sens Actuators B Chem.,346(2021)130507.)
H 2 O 2 Process for preparing porous graphite oxide solution (HGO) by etching methodSee in particular the following references: [2]Z.Chen,Y.Zhang,Y.Yang,X.Shi,L.Zhang,G.Jia,Hierarchical nitrogen-doped holey graphene as sensitive electrochemical sensor for methyl parathion detection,Sens.Actuators B Chem,336(2021)129721;[3]Y.Xu,C.Y.Chen,Z.Zhao,Z.Lin,C.Lee,X.Xu,C.Wang,Y.Huang,M.I.Shakir,X.Duan,Solution processable holey graphene oxide and its derived macrostructures for high-15 performance supercapacitors,Nano Lett.,15(2015)4605-4610.
The remainder, unless specifically stated, is indicative of a conventional commercial product or conventional processing technique in the art.
Example 1:
a preparation method of a high-stain-resistance MXene-ERHG electrochemical sensor is shown in FIG. 1:
(1) Preparation of Ti by liquid etching 3 AlC 2 An MXene suspension, and was prepared at 0.5mg/ml;
(2) By H 2 O 2 Preparing a porous graphite oxide solution (HGO) by an etching method, and preparing the solution into 0.5mg/ml;
(3) MXene and HGO are mixed according to the volume ratio of 1:1, uniformly mixing by ultrasonic waves to obtain MXene-HGO;
(4) Dripping the obtained MXene-HGO on a pretreated GCE electrode to obtain MXene-HGO/GCE, and pumping for standby
(5) And (3) carrying out electrochemical reduction on the obtained MXene-HGO/GCE in PBS solution by adopting a cyclic voltammetry (CV scanning range is-1.5V-0.5V, and scanning speed is 20 mV.s-1), so as to obtain the MXene-ERHG/GCE.
Example 2:
a preparation method of a high-stain-resistance MXene-ERHG electrochemical sensor is shown in FIG. 1:
(1) Preparing Ti3AlC2 MXene suspension by adopting a liquid etching method, and preparing the suspension into 1.5mg/ml;
(2) By H 2 O 2 Preparing a porous graphite oxide solution (HGO) by an etching method, and configuring the solution to be 1.5mg/ml;
(3) MXene and HGO are mixed according to the volume ratio of 1:1, uniformly mixing by ultrasonic waves to obtain MXene-HGO;
(4) Dripping the obtained MXene-HGO on a pretreated GCE electrode to obtain MXene-HGO/GCE, and pumping for standby
(5) And (3) carrying out electrochemical reduction on the obtained MXene-HGO/GCE in PBS solution by adopting a cyclic voltammetry (CV scanning range is-1.5V-0.5V, and scanning speed is 20 mV.s-1), so as to obtain the MXene-ERHG/GCE.
Example 3:
a preparation method of a high-stain-resistance MXene-ERHG electrochemical sensor is shown in FIG. 1:
(1) Preparing Ti3AlC2 MXene suspension by adopting a liquid etching method, and preparing the suspension into 5.0mg/ml;
(2) By H 2 O 2 Preparing a porous graphite oxide solution (HGO) by an etching method, and configuring to be 5.0mg/ml;
(3) MXene and HGO are mixed according to the volume ratio of 1:1, uniformly mixing by ultrasonic waves to obtain MXene-HGO;
(4) Dripping the obtained MXene-HGO on a pretreated GCE electrode to obtain MXene-HGO/GCE, and pumping for standby
(5) And (3) carrying out electrochemical reduction on the obtained MXene-HGO/GCE in PBS solution by adopting a cyclic voltammetry (CV scanning range is-1.5V-0.5V, and scanning speed is 20 mV.s-1), so as to obtain the MXene-ERHG/GCE.
Comparative example 1:
a preparation method of an ERHG electrochemical sensor comprises the following steps:
(1) By H 2 O 2 Preparing a porous graphite oxide solution (HGO) by an etching method, and configuring the solution to be 1.5mg/ml;
(2) Dropping the obtained HGO on the pretreated GCE electrode to obtain HGO/GCE, and draining for later use;
(3) And (3) carrying out electrochemical reduction on the obtained HGO/GCE in PBS solution by adopting a cyclic voltammetry (CV scanning range is-1.5V-0.5V, and scanning speed is 20 mV.s-1), so as to obtain ERHG.
Comparative example 2:
a preparation method of an MXene electrochemical sensor comprises the following steps:
(1) Preparation of Ti by liquid etching 3 AlC 2 An MXene suspension, and was prepared at 1.5mg/ml;
(2) And (3) dripping the obtained MXene on the pretreated GCE electrode to obtain the MXene/GCE, and draining for later use.
As can be seen from the anti-fouling performance test of the MXene-ERHG electrochemical sensor prepared in the embodiment 1, when 10 mu M DA is detected, the current signal is 6.55 mu A, and after the electrochemical sensor is soaked in 10mg/ml BSA solution for 30min, the current signal is 3.99 mu A, and the current response is reduced by 39.08%, which indicates that the MXene-ERHG has certain anti-fouling performance.
As can be seen from the anti-fouling performance test of the MXene-ERHG electrochemical sensor prepared in the embodiment 2, when 10 mu M DA is detected, the current signal is 28.48 mu A, and after the electrochemical sensor is soaked in 10mg/ml BSA solution for 30min, the current signal is 24.46 mu A, and the current response is reduced by 14.10%, so that the anti-fouling performance of the electrochemical sensor can be effectively improved by increasing the concentration.
As can be seen from the anti-fouling performance test of the MXene-ERHG electrochemical sensor prepared in the example 3, when 10. Mu.M DA is detected, the current signal is 19.50. Mu.A, and after the electrochemical sensor is soaked in 10mg/ml BSA solution for 30min, the current signal is 14.74. Mu.A, and the current response is reduced by 24.41%, which indicates that the anti-fouling performance of the electrochemical sensor cannot be improved by continuously increasing the concentration.
As can be seen from the anti-fouling performance test of the ERHG electrochemical sensor prepared in comparative example 1, when 10 mu M DA is detected, the current signal is 8.29 mu A, and after the electrochemical sensor is soaked in 10mg/ml BSA solution for 30min, the current signal is 1.47 mu A, and the current response is reduced by 82.25%, which indicates that the ERHG electrochemical sensor has no anti-fouling performance basically.
DA detection performance test was performed on the MXene electrochemical sensor prepared in comparative example 2, and it can be seen that when 10. Mu.M DA was detected using DPV, there was no corresponding current signal, indicating that the MXene electrochemical sensor did not have the performance of detecting DA (see FIG. 2).
As can be seen from the histogram of current change before and after soaking of the MXene-ERHG/GCE and ERHG/GCE electrodes (FIG. 3, which shows comparison of current response of 10. Mu.M DA before and after soaking BSA in the MXene-ERHG and ERHG electrochemical sensors), the current drop rate of the MXene-ERHG/GCE electrode after soaking in 10mg/ml BSA was only (14.10%) compared with that of the ERHG/GCE (current drop rate of 82.25%), indicating that the MXene-ERHG/GCE has a stronger fouling resistance.
From a histogram of long term stability, repeatability and reproducibility of the MXene-ergg/GCE (see fig. 4, where (a) 1 MXene-ergg was tested repeatedly 10 times, (b) 5 MXene-ergg, (c) 1 MXene-ergg responded every 3 days to PDV of artificial cerebrospinal fluid containing 10 μm DA), it can be seen that MXene-ergg/GCE has good long term stability and reproducibility.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (4)
1. The high-stain-resistance MXene-ERHG electrochemical sensor is characterized by being formed by compounding MXene and ERHG;
the electrochemical sensor is prepared by the following steps:
(1) Mixing an MXene solution with an HGO solution and performing ultrasonic treatment to obtain an MXene-HGO solution;
(2) Dropping the MXene-HGO solution on the GCE electrode, and drying to obtain the MXene-HGO/GCE;
(3) Placing the MXene-HGO/GCE in a PBS solution for electrochemical reduction to obtain the MXene-ERHG/GCE, namely the target product;
in the step (1), the concentration of the MXene solution is 0.5-5 mg/mL;
in the step (1), the concentration of the HGO solution is 0.5-5 mg/mL;
in the step (1), the adding volume ratio of the MXene solution to the HGO solution is 0.8-1.2:1;
in the step (3), the electrochemical reduction adopts cyclic voltammetry, and the scanning range thereofis-1.5V-0.5V, and the scanning rate is 20 mV.s -1 。
2. The high stain resistant MXene-ERHG electrochemical sensor of claim 1, wherein in step (1), the MXene solution used is Ti 3 AlC 2 The MXene suspension is prepared by a liquid etching method.
3. The high stain resistant MXene-ERHG electrochemical sensor according to claim 1, wherein in step (1), the HGO solution is H 2 O 2 And (5) preparing by an etching method.
4. The high stain resistant MXene-ergg electrochemical sensor of claim 1, wherein in step (2), the GCE electrode is further subjected to a pretreatment process, specifically: firstly, sequentially polishing the GCE electrode by adopting alumina with the particle diameters of 1 mu m,0.3 mu m and 0.05 mu m, then sequentially placing the GCE electrode in ethanol and ultrapure water for ultrasonic cleaning after polishing, and finally, drying by using nitrogen flow to finish the process.
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三维石墨烯/MXene复合材料的制备及电化学性能;李子成;《中国优秀硕士论文全文数据库》》;全文 * |
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