CN114371200A - MXene-ERHG electrochemical sensor with high pollution resistance and preparation method thereof - Google Patents
MXene-ERHG electrochemical sensor with high pollution resistance and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-pollution 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 method3AlC2MXene; (2) by means of H2O2Preparing a porous graphite oxide solution (HGO) by an etching method; (3) uniformly mixing MXene and HGO by ultrasonic to obtain MXene-HGO; (4) dripping the solution obtained in the step (3) on the pre-treated GCE to obtain MXene-HGO/GCE, and draining for later use; (5) and (3) performing electrochemical reduction on the MXene-HGO/GCE obtained in the step (4) in a 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 be enhanced and stabilizedAn electrochemical signal.
Description
Technical Field
The invention belongs to the technical field of analysis and test, and relates to a high-pollution 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, significant degradation of electrochemical performance such as current response and detection sensitivity is often encountered when coexisting species (e.g., biological macromolecules, proteins, and cells) bind to the electrode surface in a non-specific manner. In addition, non-specific binding of proteins (e.g., fibrinogen) to the tissue implantable sensing interface can induce an adverse immune response cascade. To overcome these problems, chemical modification of the sensing interface by various hydrophilic coatings is one of the main strategies.
MXene is a novel two-dimensional material that is of particular interest due to its unique hydrophilicity, electrical conductivity, and biocompatibility, but is highly susceptible to oxidation. Electrochemical reduction porous graphene (ERHG) is one of important derivatives of graphene-based materials, the electron transfer capacity and mass transfer capacity of the sensor can be effectively improved due to the existence of abundant reticular micropores and the increase of the specific surface area, but the graphene has good protein adsorption capacity and is not beneficial to biological anti-fouling. Therefore, the materials have obvious defects in the aspects of anti-fouling performance and the like. The present invention has been made to solve the above problems.
Disclosure of Invention
The invention aims to provide an MXene-ERHG electrochemical sensor with high pollution resistance and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
one of the technical schemes of the invention provides a high-pollution-resistance MXene-ERHG electrochemical sensor which is formed by compounding MXene and ERHG.
MXene and HGO are compounded, so that MXene is effectively protected, and an MXene-ERHG interface obtained through electrochemical reduction meets the requirement of hydrophilicity and has good electron transfer capacity, so that the MXene-ERHG biological interface can resist non-specific combination of proteins in complex biological fluid, and the electron transfer capacity of the interface is also enhanced.
The second technical scheme of the invention provides a preparation method of the MXene-ERHG electrochemical sensor with high pollution resistance, which comprises the following steps:
(1) mixing the MXene solution with the HGO solution and performing ultrasonic treatment to obtain an MXene-HGO solution;
(2) dripping MXene-HGO solution on a GCE electrode, and drying to obtain MXene-HGO/GCE;
(3) placing MXene-HGO/GCE in a PBS solution, and carrying out electrochemical reduction to obtain MXene-ERHG/GCE, namely the target product.
Furthermore, 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 0.5-5 mg/mL.
Furthermore, in the step (1), the adding volume ratio of the MXene solution to the HGO solution is 0.8-1.2: 1, and preferably 1: 1.
Further, in the step (1), the MXene solution is Ti3AlC2MXene suspension prepared by liquid etching method.
Further, in the step (1), the HGO solution used is H2O2And etching to obtain the final product.
Further, in the step (2), the GCE electrode is also pretreated, and the pretreatment process specifically comprises: firstly, polishing GCE electrodes (the diameter of the GCE electrodes is generally 3mm) by adopting aluminum oxide with the particle size of 1 micron, 0.3 micron and 0.05 micron in sequence, then placing the GCE electrodes in ethanol and ultrapure water in sequence for ultrasonic cleaning after polishing, and finally blowing the GCE electrodes by using nitrogen flow to dry.
Further, in step (3), the pH of the PBS solution is adjusted to 9.23, and oxygen removal treatment is performed.
Further, in the step (3), the electrochemical reduction adopts cyclic voltammetry, the scanning range is-1.5V-0.5V, and the scanning rate is 20mV · s-1。
The MXene-ERHG is reduced by an electrochemical reduction method to obtain the MXene-ERHG, firstly, the surfaces of the HGO and the MXene simultaneously contain rich oxygen-containing functional groups, the MXene can be coated by the HGO under the chemical combination action, the MXene is effectively protected, secondly, the electrochemical reduction of the ERHG has a micropore structure which provides guarantee for the good electron transfer capability of an electrochemical sensor, and finally, the synergistic effect of the HG and the MXene-ERHG provides guarantee for the detection of disease markers 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 method has a good linear range, a low detection limit and remarkable anti-fouling performance.
(2) The invention has simple and easy operation process and stable material performance.
Drawings
Fig. 1 is a schematic flow chart of the operation of the electrochemical sensor of the present invention.
Fig. 2 is a DA detection performance test chart of the electrochemical sensor, in which 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 antifouling property test effects of ERHG and MXene-ERHG.
FIG. 4 shows the effect of MXene-ERHG in the reproducibility and long-term stability test in artificial cerebrospinal fluid.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
In the following examples, Ti was prepared by liquid etching3AlC2Of MXene suspensionsThe procedures are specifically described 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.)
H2O2The etching process for preparing porous graphite oxide solution (HGO) is described in 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.
Otherwise, unless otherwise specified, all the materials or processing techniques are conventional commercial products or conventional processing techniques in the art.
Example 1:
a preparation method of a high-pollution resistance MXene-ERHG electrochemical sensor is shown in figure 1:
(1) preparation of Ti by liquid etching method3AlC2MXene suspension, and configured to 0.5 mg/ml;
(2) by means of H2O2Preparing a porous graphite oxide solution (HGO) by an etching method, and preparing the solution to be 0.5 mg/ml;
(3) mixing MXene and HGO in a 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 draining for later use
(5) And (3) performing electrochemical reduction on the obtained MXene-HGO/GCE in a PBS solution by adopting a cyclic voltammetry (CV scanning range is-1.5V-0.5V, and scanning speed is 20mV s < -1 >) to obtain MXene-ERHG/GCE.
Example 2:
a preparation method of a high-pollution resistance MXene-ERHG electrochemical sensor is shown in figure 1:
(1) preparing Ti3AlC2 MXene suspension by liquid etching method to 1.5 mg/ml;
(2) by means of H2O2Preparing a porous graphite oxide solution (HGO) by an etching method, and preparing the solution to be 1.5 mg/ml;
(3) mixing MXene and HGO in a 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 draining for later use
(5) And (3) performing electrochemical reduction on the obtained MXene-HGO/GCE in a PBS solution by adopting a cyclic voltammetry (CV scanning range is-1.5V-0.5V, and scanning speed is 20mV s < -1 >) to obtain MXene-ERHG/GCE.
Example 3:
a preparation method of a high-pollution resistance MXene-ERHG electrochemical sensor is shown in figure 1:
(1) preparing Ti3AlC2 MXene suspension by liquid etching method to 5.0 mg/ml;
(2) by means of H2O2Preparing a porous graphite oxide solution (HGO) by an etching method, and preparing the solution to be 5.0 mg/ml;
(3) mixing MXene and HGO in a 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 draining for later use
(5) And (3) performing electrochemical reduction on the obtained MXene-HGO/GCE in a PBS solution by adopting a cyclic voltammetry (CV scanning range is-1.5V-0.5V, and scanning speed is 20mV s < -1 >) to obtain MXene-ERHG/GCE.
Comparative example 1:
a preparation method of an ERHG electrochemical sensor comprises the following steps:
(1) by means of H2O2Preparing a porous graphite oxide solution (HGO) by an etching method, and preparing the solution to be 1.5 mg/ml;
(2) dripping the obtained HGO on a pre-treated GCE electrode to obtain HGO/GCE, and draining for later use;
(3) and (3) carrying out electrochemical reduction on the obtained HGO/GCE in a PBS solution by adopting cyclic voltammetry (CV scanning range is-1.5V-0.5V, and scanning speed is 20mV s < -1 >) 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 method3AlC2MXene suspension prepared to be 1.5 mg/ml;
(2) and (3) dripping the obtained MXene on a pretreated GCE electrode to obtain MXene/GCE, and draining for later use.
The anti-fouling performance test of the MXene-ERHG electrochemical sensor prepared in this example 1 shows that when 10 μ M DA is detected, the current signal is 6.55 μ A, and after the electrochemical sensor is soaked in 10mg/ml BSA solution for 30min, the current signal is 3.99 μ A, and the current response is reduced by 39.08%, which indicates that the MXene-ERHG has a certain anti-fouling performance.
The anti-fouling performance test of the MXene-ERHG electrochemical sensor prepared in this example 2 shows that when 10 μ M DA is detected, the current signal is 28.48 μ A, and after the electrochemical sensor is soaked in 10mg/ml BSA solution for 30min, the current signal is 24.46 μ A, and the current response is reduced by 14.10%, which indicates that the anti-fouling performance of the electrochemical sensor can be effectively improved by increasing the concentration.
The anti-fouling performance test of the MXene-ERHG electrochemical sensor prepared in this example 3 shows that when 10 μ M DA is detected, the current signal is 19.50 μ A, and after the electrochemical sensor is soaked in 10mg/ml BSA solution for 30min, the current signal is 14.74 μ 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.
The anti-fouling performance test of the ERHG electrochemical sensor prepared in the comparative example 1 shows that when 10 mu M DA is detected, the current signal is 8.29 mu A, after the electrochemical sensor is soaked in 10mg/ml BSA solution for 30min, the current signal is 1.47 mu A, the current response is reduced by 82.25%, and the ERHG electrochemical sensor basically has no anti-fouling performance.
When the MXene electrochemical sensor prepared in comparative example 2 is subjected to DA detection performance test, it can be seen that when 10 μ M DA is detected by using DPV, no corresponding current signal exists, which indicates that the MXene electrochemical sensor does not have DA detection performance (see FIG. 2).
From the current change bar chart before and after soaking of the MXene-ERHG/GCE and the ERHG/GCE electrodes (fig. 3, which shows the current response comparison of 10 μ M DA detection before and after soaking of the MXene-ERHG and the ERHG electrochemical sensor in BSA), it can be seen that compared with the ERHG/GCE (the current reduction rate is 82.25%), the current reduction rate of the MXene-ERHG/GCE electrode after soaking of 10mg/ml BSA is only (14.10%), which indicates that the MXene-ERHG/GCE has stronger anti-fouling capability.
From the histograms of long-term stability, reproducibility and reproducibility of MXene-ERHG/GCE (see FIG. 4, where (a)1 MXene-ERHG was tested 10 times in duplicate, (b)5 MXene-ERHG, (c) PDV response of 1 MXene-ERHG every 3 days in artificial cerebrospinal fluid containing 10. mu.M DA), it can be seen that MXene-ERHG/GCE has good long-term stability and reproducibility.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, 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 embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. An MXene-ERHG electrochemical sensor with high pollution resistance is characterized in that the MXene-ERHG electrochemical sensor is formed by compounding MXene and ERHG.
2. The method for preparing the MXene-ERHG electrochemical sensor with high anti-pollution performance as claimed in claim 1, wherein the method comprises the following steps:
(1) mixing the MXene solution with the HGO solution and performing ultrasonic treatment to obtain an MXene-HGO solution;
(2) dripping MXene-HGO solution on a GCE electrode, and drying to obtain MXene-HGO/GCE;
(3) placing MXene-HGO/GCE in a PBS solution, and carrying out electrochemical reduction to obtain MXene-ERHG/GCE, namely the target product.
3. The method for preparing the MXene-ERHG electrochemical sensor with high anti-pollution performance according to claim 2, wherein in the step (1), the concentration of the MXene solution is 0.5-5 mg/mL.
4. The method for preparing the MXene-ERHG electrochemical sensor with high anti-pollution performance according to claim 2, wherein in the step (1), the concentration of the HGO solution is 0.5-5 mg/mL.
5. The method for preparing the MXene-ERHG electrochemical sensor with high anti-pollution performance according to claim 2, wherein in the step (1), the addition volume ratio of the MXene solution to the HGO solution is 0.8-1.2: 1.
6. The method for preparing the MXene-ERHG electrochemical sensor with high anti-pollution performance according to claim 2, wherein in the step (1), the MXene solution is Ti3AlC2MXene suspension prepared by liquid etching method.
7. The method for preparing the MXene-ERHG electrochemical sensor with high anti-pollution performance according to claim 2, wherein in the step (1), the HGO solution is H2O2And etching to obtain the final product.
8. The method for preparing the MXene-ERHG electrochemical sensor with high anti-pollution performance according to claim 2, wherein in the step (2), the GCE electrode is further pretreated, and the pretreatment process specifically comprises the following steps: firstly, polishing the GCE electrode by adopting alumina with the particle size of 1 mu m, 0.3 mu m and 0.05 mu m in sequence, then placing the polished GCE electrode in ethanol and ultrapure water in sequence for ultrasonic cleaning, and finally blowing the polished GCE electrode by using nitrogen flow to finish the operation.
9. The method for preparing the MXene-ERHG electrochemical sensor with high anti-pollution performance according to claim 2, wherein in the step (3), the pH value of the PBS solution is up to 9.23, and oxygen removal treatment is performed.
10. The method for preparing the MXene-ERHG electrochemical sensor with high anti-pollution performance according to claim 2, wherein in the step (3), the electrochemical reduction adopts cyclic voltammetry, the scanning range is-1.5V-0.5V, and the scanning rate is 20 mV.s-1。
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