CN114527183A - Photoinduced electrochemical sensor and preparation method and application thereof - Google Patents

Photoinduced electrochemical sensor and preparation method and application thereof Download PDF

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CN114527183A
CN114527183A CN202210050604.1A CN202210050604A CN114527183A CN 114527183 A CN114527183 A CN 114527183A CN 202210050604 A CN202210050604 A CN 202210050604A CN 114527183 A CN114527183 A CN 114527183A
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CN114527183B (en
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刘红艳
艾思敏
刘永伟
袁若
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Southwest University
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Abstract

The invention relates to a photoinduced electrochemical sensor which comprises a photoelectric anode and a photoelectric cathode, wherein the photoelectric anode comprises a first electrode and Bi positioned on the surface of the first electrode2WO6And/or sulfur doping of Bi2WO6The photoelectric cathode comprises a second electrode and PEDOT located on the surface of the second electrode. The photo-electrochemical sensing provided by the invention improves a high-performance stable self-powered cathode PEC sensing platform for detecting miRNA.

Description

Photoinduced electrochemical sensor and preparation method and application thereof
Technical Field
The invention belongs to the field of photoelectric materials and sensing, and particularly relates to a photoinduced electrochemical sensor and a preparation method and application thereof.
Background
In the self-powered cathode Photoelectrochemistry (PEC) sensor, an excitation signal of a photoelectrochemistry process is on a photoelectrode, and a target object identification process is on the photoelectrode, so that the interference of non-specific oxidation-reduction reaction on a photoelectricity active interface can be effectively prevented, the generation of false positive signals is avoided, and the anti-interference capability is strong. Compared with an optical detection method, the self-powered cathode PEC sensor has the advantages of simple equipment, low cost and no external power supply, so that the self-powered cathode PEC sensor becomes a simple, flexible, rapid and sensitive analysis technology suitable for molecular detection of tumor diseases and environmental pollutants.
Self-powered cathodic PEC sensors consist of a photoanode and a photocathode, which is used to identify a target and is typically constructed from P-type materials. And the photo-anode is used as a counter electrode/reference electrode for amplifying cathode photocurrent and is generally constructed by using an N-type material. P-type semiconductors used for constructing photocathodes currently used include NiO, PbS, Cu2O, BiOI and CuInS2And the like. However, most P-type semiconductor-based photocathodes have low photoelectric conversion efficiency, resulting in low cathode photocurrent generated. In order to enhance the cathode photocurrent signal, a sensitizer is usually needed to enhance the absorption of light by the N-type material of the photoanode and to improve the separation efficiency of the photo-generated electron-hole pairs, thereby improving the response sensitivity of the sensor to the substance to be measured. The traditional co-sensitization strategy is still difficult to find two cascade sensitization materials with matched energy levels, and the interface between different photoactive materials can also block charge transfer and limit the photoelectric conversion efficiency. In addition, the common cathode photoelectric material has the problems of poor conductivity, weak capability of attracting photogenerated electrons on an electrode interface, low charge migration speed and the like. Therefore, new strategies for improving photocurrent signals and further for high-sensitivity photoelectric sensors are urgently needed to be developed.
Disclosure of Invention
The invention designs a similar antenna strategy based on Bi2WO6Or S doping with Bi2WO6As a photo-anode material, a conductive polymer material poly (3, 4-ethylenedioxythiophene) (PEDOT) is used as a photo-cathode material, so that the conductivity of the photo-cathode is improved, the separation efficiency of photo-generated electron-hole pairs of an N-type semiconductor of the photo-anode is improved, and the cathode photocurrent is greatly enhanced. Thereby binding the targetInducing enzyme-assisted circulation amplification reaction, constructing a self-powered cathode photo-electrochemical sensor, and realizing ultra-sensitive detection of a tumor marker miRNA-141 (such as microRNA-141).
The invention provides a photoinduced electrochemical sensor which comprises a photoelectric anode and a photoelectric cathode, wherein the photoelectric anode comprises a first electrode and Bi positioned on the surface of the first electrode2WO6And/or sulfur doped Bi2WO6The photoelectric cathode comprises a second electrode and PEDOT positioned on the surface of the second electrode.
According to some embodiments of the inventive photo-electrochemical sensor, the sulfur is doped with Bi2WO6In the formula (II), thiourea and Bi2WO6The mass ratio of (0.1-3): 100, preferably (0.5-2.5): 100, most preferably (0.8-1.5): 100.
according to some embodiments of the inventive photo-electrochemical sensor, the sulfur is doped with Bi2WO is synthesized by a hydrothermal method, and the hydrothermal method synthesis preferably comprises the steps of mixing bismuth salt and tungstate in an alcohol solution to obtain a first mixed solution; adding thiourea into the mixed solution to obtain a second mixed solution; the second mixed solution is subjected to a closed reaction at the temperature of 150 ℃ and 200 ℃ for 12 to 36 hours to obtain a precipitate.
According to some embodiments of the photo-electrochemical sensor of the present invention, the feeding mass ratio of the thiourea (in terms of the mass of the sulfur element) to the bismuth salt (in terms of the mass of the bismuth element) is (0.07-2.1): 100, preferably (0.4-1.8): 100, most preferably (0.6-1.1): 100.
according to some embodiments of the photo-electrochemical sensor of the invention, the bismuth salt is Bi (NO)3)3Or a hydrate thereof.
According to some embodiments of the photo-electrochemical sensor of the invention, the tungstate is Na2WO4Or a hydrate thereof.
According to some embodiments of the photo-electrochemical sensor of the invention, the alcohol solution is a glycol solution.
According to some embodiments of the photo-induced electrochemical sensor of the present invention, the first electrode and the second electrode are glassy carbon electrodes.
The invention also provides a construction method of the photo-induced electrochemical sensor, which comprises the following steps:
loading PEDOT on the first electrode to obtain a PEDOT photocathode;
depositing gold nanoparticles on a PEDOT photocathode to serve as a working electrode;
adding Bi2WO6Or sulfur doped with Bi2WO6And loading the second electrode to prepare the photoanode as a counter/reference electrode.
Further, the invention also provides application of the photo-induced electrochemical sensor in detection of tumor markers. In particular, the tumor marker can be miRNA-141.
The invention provides an antenna strategy, wherein a photocathode is constructed by poly 3, 4-ethylenedioxythiophene (PEDOT) conducting polymer, the PEDOT has very good conductivity, photo-generated holes generated by a photo-anode can be attracted through an external circuit, the separation of photo-generated electron hole pairs of an anode N-type semiconductor is accelerated, a cathode photocurrent signal is amplified by more than 10 times, and a high-performance stable self-powered cathode PEC sensing platform is improved for detecting miRNA.
Drawings
Fig. 1 shows a construction process of a self-powered cathode photo-electrochemical sensor, wherein a is an electron transfer mechanism of the sensor, B is a target miRNA-141 induced enzyme-assisted single-signal amplification process, and C is a construction process of a photocathode on a self-powered cathode PEC sensor.
Fig. 2 shows the testing process of the self-powered cathode PEC sensor in the test case, where a is the linear relationship of photocurrent response, B is the calibration curve of the self-powered cathode PEC sensor at different concentrations of miRNA-141, C is the stability of the self-powered cathode PEC sensor at 1pM miRNA-141, and D is the selectivity of the sensor.
Fig. 3 shows the effect of S doping amount on the photoelectric properties of the material.
Fig. 4 shows the effect of amplifying the cathode photocurrent signal under the antenna strategy in example 2 of the present invention.
Detailed Description
For easy understanding of the present invention, the present invention will be described in detail with reference to examples, which are provided for illustrative purposes only and are not intended to limit the scope of the present invention.
The starting materials or components used in the present invention may be commercially or conventionally prepared unless otherwise specified.
Example 1
The S doped Bi of the invention2WO6(S:Bi2WO6) Prepared by simple hydrothermal reaction: first, 0.9701g of hydrated Bi (NO)3)3Dissolving in 20mL of ethylene glycol solution, stirring for 30min while adding 0.3297g of Na2WO4·2H2Dissolving O in 20mL of glycol solution, continuously stirring for 30min, mixing the two solutions, and ultrasonically dispersing until the solution is uniform. Then, thiourea was added as a sulfur source to the above mixed solution, and stirring was continued for 1 hour. Finally, the mixed solution was transferred to a 50mL teflon-lined autoclave and reacted at 180 ℃ for 24 hours in a digitally temperature-controlled reaction furnace. Naturally cooling the autoclave to room temperature, centrifuging to collect a gray precipitate, washing with distilled water and 95% ethanol for several times, and freeze-drying for later use.
A series of S-doped Bi are synthesized by the same method2WO6Defective nano material named S Bi2WO6X (X is 0, 1%, 3%, 5%, 10%) represents the mass ratio of thiourea/bismuth tungstate of 0 (without thiourea) and 1% (namely thiourea and Bi)2WO6The mass ratio of (1): 100) 3% ((i.e., thiourea and Bi)2WO6The mass ratio of (A) to (B) is 3: 100) 5% ((i.e., thiourea and Bi))2WO6The mass ratio of (A) to (B) is 5: 100) and 10%.
Test example
Test example 1
The photoelectrochemical test method is adopted to measure the photoelectric property of the photoanode material in the example 1 under the excitation of a 400nm light source, and the specific result is shown in table 1.
TABLE 1
Photocurrent muA
S:Bi2WO6-1％ 4.681
S:Bi2WO6-3％ 2.149
S:Bi2WO6-5％ 1.740
S:Bi2WO6-10％ 1.685
S:Bi2WO6-0(Bi2WO6) 3.568
Example 2
And (3) constructing a sensor:
firstly, polishing and grinding a glassy carbon electrode by using alumina powder, and alternately and ultrasonically washing the glassy carbon electrode by using ethanol and ultrapure water. Then, PEDOT is dripped on the surface of a clean and dry glassy carbon electrode, gold nanoparticles (AuNPs) are deposited on a PEDOT photocathode as a working electrode through an electrodeposition method after the PEDOT is naturally aired to form a film, and S: Bi is added2WO6Dropping 1% solution on the surface of glassy carbon electrode, which is also clean and dry, and using the photo-anode as counter/reference electrode to amplify the photo-current signal (PEC signal in "on" state), as can be seen in FIG. 4。
Next, the 5' -thiol-modified capture chain HP2 was assembled at the GCE/PEDOT/Dep Au photocathode interface via Au-S coordination bond, at which time the non-specific adsorption sites of the cathode interface were blocked with Hexanethiol (HT), followed by addition of the target-mediated enzyme-assisted single-signal amplification reaction product output DNA. Through the catalytic hairpin assembly amplification technology, output DNA opens hairpin DNA HP2 incubated on the electrode, wherein HP2 can be combined with HP3-S1-SiO2HP3 on the complex is hybridized and combined through strand displacement reaction, output DNA released in the process can circularly act on other hairpins on an electrode interface, and in addition, S2-SiO added2The complex can be assembled on the above modified electrode interface by hybridization of S2 and S1. Since DNAs-SiO2A large number of structures are assembled and fixedly carried on the photocathode interface, so that the doping of Bi into the photo-anode S by the PEDOT/dep Au photocathode is prevented2WO6The absorption of the generated photo-generated electrons, and the electron transport at the electrode surface, effect quenching of the cathodic PEC signal (the "off" state). In the process, the PEC signal quenching degree is in direct proportion to the concentration of the target miRNA-141, so that the sensor can be successfully used for miRNA-141 detection.
Example 3
1. The sensor is adopted to detect the miRNA-141 standard solution, and the specific method is as follows:
3) formation of miRNA-141 mediated enzyme assisted cyclic amplification reaction product output DNA: first, 120. mu.L, 2. mu.M hairpin DNA (HP1) was combined with Fe3O4Mixing and stirring the-Au solution at the temperature of 4 ℃ overnight to obtain Fe3O4-Au-HP 1. Subsequently, the mixture was magnetically separated and washed and then re-dispersed in 120. mu.L of phosphoric acid buffer solution in Fe3O4Hexanethiol was added to the Au-HP1 mixture to block non-specific binding sites. Next, 20. mu.L of miRNA-141, 0.5. mu.L of double strand specific nuclease (DSN, 0.1U) and 0.5. mu.L of 1 XDSN Master buffer were added to the Fe3O4The reaction was continued for 40 minutes in the Au-HP1-HT complex at 60 ℃. In the process, the target miRNA-141 can react with Fe3O4Hybridization of HP1 on Au to form a DNA-RNA hybrid strand, a double-strand specific nuclease capable of specificityRecognizing and digesting the DNA part in the DNA-RNA mixed chain, using the released RNA for the next cycle, finally adding DSN stop solution, heating at 60 ℃ for 10min to inactivate enzyme so as to stop the reaction, and obtaining a large amount of product output DNA through magnetic separation.
4) Hybridizing the released product output DNA with hairpin DNA (HP2) modified on the surface of an electrode, incubating for 2h, rinsing in ultrapure water, and adding SiO modified with a quenching group 210 μ L of each of HP3, S1, and S2 was incubated for 2h to complete the catalytic hairpin assembly strand displacement reaction.
3) The photo-electrochemical detection adopts a novel self-powered cathode PEC sensor system: GCE/PEDOT as working electrode, GCE/Bi2WO6-xSxInstead of a platinum wire counter electrode as counter/reference electrode, no bias voltage is supplied. In the presence of hydrogen peroxide (H)2O2) In Phosphate Buffer Solution (PBS), 400nm LED light is used as an excitation light source, a potential scanning fast light source mode is an off-on-off mode of 10-20-10, continuous scanning is carried out for 5 circles, and a stable photocurrent value is recorded.
4) The PEC signal of the sensor decreased with increasing miRNA-141 concentration and was proportional to the log of miRNA-141 concentration. The linear response ranged from 1fM to 10 nM.
2. Selective detection of the sensor
1) In the process of target-mediated displacement of the trigger strand, miRNA-141 was replaced with 100pM of interfering molecule. The output product is then reacted on the electrode according to the same procedure.
2) During target-mediated displacement of the trigger strand, the concentration of the target miRNA-141 was 10 pM.
3) During target-mediated displacement of the trigger strand, the blank is no target added and the subsequent reaction steps are unchanged.
4) PEC signals of the respective interferon molecules were measured by the same procedure, and the PEC signal intensities were averaged three times, in contrast to the PEC intensity of 10pM miRNA-141, and the results are shown in FIG. 2 (D).
3. Preparation of phosphate buffer solution (PBS, pH 7.0)
From 0.1 mol. L-1K2HPO4，0.1mol·L-1NaH2PO4And 0.1 mol. L-1KCl mixed solution.
The invention provides a high-performance and stable platform for detecting miRNA-141 by a self-powered cathode PEC sensor, and the sensor has excellent analysis performance and ultra-sensitivity. The innate strategy provides a new method for amplifying cathode photocurrent, is helpful for further understanding the defect structure and the basic function of a conductive polymer in the process of constructing a self-powered cathode PEC sensor, and is applied to other tumor marker miRNA molecules to guide clinical diagnosis.
It should be noted that the above-mentioned embodiments are only for explaining the present invention, and do not constitute any limitation to the present invention. The present invention has been described with reference to exemplary embodiments, but the words which have been used herein are words of description and illustration, rather than words of limitation. The invention can be modified, as prescribed, within the scope of the claims and without departing from the scope and spirit of the invention. Although the invention has been described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, but rather extends to all other methods and applications having the same functionality.

Claims (10)

1. A photo-induced electrochemical sensor comprises a photo-anode and a photo-cathode, wherein the photo-anode comprises a first electrode and Bi on the surface of the first electrode2WO6And/or sulfur doped Bi2WO6The photoelectric cathode comprises a second electrode and PEDOT positioned on the surface of the second electrode.
2. The photo-electrochemical sensor of claim 1, wherein the sulfur is doped with Bi2WO6In the formula (II), thiourea and Bi2WO6The mass ratio of (0.1-3): 100, preferably (0.5-2.5): 100, most preferably (0.8-1.5): 100.
3. the photo-electrochemical sensor according to claim 1 or 2, wherein the sulfur is doped with Bi2WO is synthesized by a hydrothermal method, and the hydrothermal method synthesis preferably comprises the steps of mixing bismuth salt and tungstate in an alcohol solution to obtain a first mixed solution; adding thiourea into the mixed solution to obtain a second mixed solution; the second mixed solution is subjected to a closed reaction at the temperature of 150 ℃ and 200 ℃ for 12 to 36 hours to obtain a precipitate.
4. The photo-electrochemical sensor according to claim 3, wherein the mass ratio of the thiourea (in terms of the mass of the sulfur element) to the bismuth salt (in terms of the mass of the bismuth element) is (0.07-2.1): 100, preferably (0.4-1.8): 100, most preferably (0.6-1.1): 100.
5. the photo-induced electrochemical sensor according to claim 3 or 4, wherein the bismuth salt is Bi (NO)3)3Or a hydrate thereof, the tungstate is Na2WO4Or a hydrate thereof, and the alcohol solution is an ethylene glycol solution.
6. The photo-induced electrochemical sensor according to any one of claims 1 to 5, wherein the first electrode and the second electrode are glassy carbon electrodes.
7. The method of making a photo-electrochemical sensor according to any one of claims 1-6, comprising the steps of:
loading PEDOT on the first electrode to obtain a PEDOT photocathode;
depositing gold nanoparticles on a PEDOT photocathode to serve as a working electrode;
adding Bi2WO6Or sulfur doped with Bi2WO6And loading the second electrode to prepare the photoanode as a counter/reference electrode.
8. Use of the photo-electrochemical sensor according to any one of claims 1-6 in the detection of a tumor marker.
9. The use of claim 8, wherein the tumor marker is miRNA-141.
10. A method for detecting miRNA comprises the following steps:
1) forming a target-mediated enzyme-assisted cyclic amplification reaction product output DNA;
2) hybridizing output DNA with hairpin DNA (HP2) modified on the surface of the electrode, and adding SiO modified with a quenching group2HP3, S1 and S2, and incubating to complete the catalytic hairpin assembly strand displacement reaction;
3) the photoelectrochemical sensor according to any one of claims 1 to 5, which is used for detecting a photocurrent value by using a photocathode as a working electrode, a photoanode as a reference electrode, and an LED light having a wavelength of 300 nm to 660 nm as an excitation light source, preferably 400nm, as an excitation light source in a phosphate buffer solution containing hydrogen peroxide.
CN202210050604.1A 2022-01-17 2022-01-17 Photoelectrochemical sensor and preparation method and application thereof Active CN114527183B (en)

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CN110323521A (en) * 2019-06-17 2019-10-11 北京大学 A kind of photoelectrochemistrpool pool of perovskite semiconductor
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