CN107064264B - A kind of construction method of the optical electro-chemistry sensor for no enzyme detection dopamine - Google Patents
A kind of construction method of the optical electro-chemistry sensor for no enzyme detection dopamine Download PDFInfo
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- CN107064264B CN107064264B CN201710351559.2A CN201710351559A CN107064264B CN 107064264 B CN107064264 B CN 107064264B CN 201710351559 A CN201710351559 A CN 201710351559A CN 107064264 B CN107064264 B CN 107064264B
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Abstract
The present invention provides a kind of construction methods of optical electro-chemistry sensor for no enzyme detection dopamine, and steps are as follows: step 1 prepares azepine graphene quantum dot (N-GQDs) solution；Step 2 prepares presoma pucherite (BiVO4)；Step 3 prepares ternary complex BiOCl/BiVO4/N-GQDs；The optical electro-chemistry sensor of step 4, building without enzyme detection dopamine.Compared with traditional detection method, the optical electro-chemistry detection method of DA proposed in the present invention has the features such as operation is easier flexibly, and instrument and equipment is simpler, and reagent dosage is few, and testing cost is cheap.
Description
Technical field
The invention belongs to field of electrochemical detection, refer to a kind of optical electro-chemistry biography detected for dopamine in human body without enzymeization
The construction method and purposes of sensor.
Background technique
Dopamine (dopamine, DA) is the important neurotransmitter of one of central nervous system of human body, and
Important role is also played in kidney and angiocarpy.Researchers, which are devoted to develop simple, quick, sensitive method, to be used for
The detection of dopamine.The method for the detection dopamine that there is now includes electrophoresis, liquid chromatography and spectrofluorimetry
Etc. research methods deposited in terms of practical application although these methods can satisfy sensitivity and the requirement of specific detection
In certain limitation.For example, chromatography can be used in qualitative and quantitative analysis, and testing result is relatively accurate, reliable, sensitive
Degree is high, favorable reproducibility, but instrument equipment is expensive, complicated for operation, needs technical professional, thus is not suitable for large quantities of
The processing and analysis and the quick detection at scene of amount sample.Optical electro-chemistry (PEC) technology, as a kind of emerging electroanalysis skill
Art has received widespread attention in various fields, such as biological field, field of medicaments and environmental science etc..PEC sensing
Technology has the advantages that much cannot or to be difficult to realize on Conventional electrochemical platform as a kind of novel analytical technology.
Since PEC is to use two different form of excitation and detection signal, and the technical background signal is low, therefore has higher
Sensitivity.
The present invention prepares BiOCl/BiVO4/ N-GQDs nano-complex is successfully established photoelectrochemical as photoelectric activity material
Learn sensing platform, for the optical electro-chemistry detection without enzyme of dopamine in human serum, construct it is a kind of quickly, Sensitive Detection it is more
The optical electro-chemistry sensor of bar amine, establishes the corresponding relationship between DA concentration and photocurrent response value, realizes simple, clever
The purpose of quick, quick detection DA.Therefore, prepared sensor can be used for detecting the DA content in human serum.
Summary of the invention
The present invention is intended to provide the optical electro-chemistry that a kind of the advantages that highly sensitive, highly selective, Wide measuring range is integrated
Sensor.Sensor preparation process is simple, at low cost, realizes the purpose of rapid quantitative detection DA.
Used scheme is summarized are as follows:
With the BiOCl/BiVO of preparation4/ N-GQDs nano-complex creates overdelicate photoelectricity as photoelectric activity material
Chemical sensitisation platform.Utilize BiOCl/BiVO4/ N-GQDs nano-complex is to the property such as the larger absorption of visible light and quick response
Matter plays the role of a signal amplification to detection system.As addition object DA, BiOCl/BiVO in solution4/ N-GQDs receives
Excitation of the rice compound by visible light, the hole of generation is aoxidized to by DA, produced by the oxidation product of DA can be prevented effectively
Electron-hole pair it is compound again so that its photocurrent response enhanced strength, is established between photocurrent response value and DA concentration
Relationship, with achieve the purpose that it is quick to DA content in human serum, sensitive, selectively detect.
The present invention is realized by following specific technical solution:
A kind of construction method of the optical electro-chemistry sensor for no enzyme detection dopamine, steps are as follows:
Step 1 prepares azepine graphene quantum dot (N-GQDs) solution:
It after ammonium citrate is dissolved in water, is transferred in oil bath, heating reaction is carried out under conditions of constant pressure airtight, has been reacted
Azepine graphene quantum dot solution is obtained after finishing；
Step 2 prepares presoma pucherite (BiVO4):
Five nitric hydrate bismuths are dissolved in concentrated nitric acid, solution A is obtained；Ammonium metavanadate is dissolved in sodium hydroxide solution, is obtained
To solution B；Solution A is added drop-wise in solution B dropwise, is stirred evenly, obtains mixed liquor C, then hydroxide is added dropwise into mixed liquor C
Sodium solution adjusts pH to 11~12, obtains mixed liquor D, mixed liquor D is transferred in stainless steel autoclave and carries out solvent thermal reaction,
After completion of the reaction, the solid product obtained is pucherite；
Step 3 prepares ternary complex BiOCl/BiVO4/ N-GQDs:
The pucherite that step 2 is obtained is scattered in hydrochloric acid, is stirred evenly, and the azepine graphene amount in step 1 is added
Son point solution, stirs evenly, obtains mixed liquor E, mixed liquor E is transferred in stainless steel autoclave and carries out solvent thermal reaction, instead
After answering, obtained solid product is ternary complex BiOCl/BiVO4/N-GQDs；
The optical electro-chemistry sensor of step 4, building without enzyme detection dopamine:
By ternary complex BiOCl/BiVO4/ N-GQDs is scattered in ultrapure water, obtains BiOCl/BiVO4/ N-GQDs points
Dispersion liquid, by BiOCl/BiVO4/ N-GQDs dispersant liquid drop is applied in ITO electrode, using ITO electrode as working electrode, is saturated calomel
Electrode is as reference electrode, and platinum filament, which is used as, constitutes the optical electro-chemistry sensor without enzyme detection dopamine to electrode, by electrochemistry
Work station three-electrode system under the irradiation of xenon source and carries out photoelectrochemical assay in nitrogen atmosphere.
In step 1, the amount ratio of the ammonium citrate and water is 1~2g:30~60mL；Temperature in the oil bath is
140~200 DEG C.
In step 2, in the solution A, the amount ratio of five nitric hydrate bismuths and concentrated nitric acid is 4~5g:10mL；In solution B,
The amount ratio of ammonium metavanadate and sodium hydroxide solution is 1~2g:10mL；In the mixed liquor C, the volume ratio of solution A and solution B
For 1:1；The sodium hydroxide solution is 6mol/L；The temperature of the solvent thermal reaction is 140~200 DEG C, the reaction time 8
~12h.
In step 3, in the mixed liquor E, pucherite, hydrochloric acid, azepine graphene quantum dot solution amount ratio be 0.05
~0.1g:20mL:1~5mL, the concentration of hydrochloric acid are 8mmol/L；The temperature of the solvent thermal reaction is 140~200 DEG C, reaction
Time is 8~12h.
In step 4, the intensity of the xenon source is 25%~100%.
The utility model has the advantages that the present invention prepares BiOCl/BiVO4/ N-GQDs nano-complex is as photoelectric activity material, success
Optical electro-chemistry sensing platform is established, a kind of optical electro-chemistry detection method without enzyme of dopamine in human serum is established,
Characteristic and advantage are expressed as follows:
(1) present invention preparation BiOCl/BiVO4/ N-GQDs nano-complex constructs photoelectrochemical as photoelectric activity material
Learn sensor, dual amplification photocurrent response signal.
(2) present invention is using N-GQDs to BiOCl/BiVO4Hetero-junctions is further adulterated, on the one hand, N-GQDs
Have the function of that excellent electric conductivity can play signal amplification；On the other hand, pi-conjugated using the intermolecular π-of N-GQDs and DA
Effect, further increases stability and is more advantageous to the transfer of electronics.
(3) method for amplifying signal proposed by the invention and detection pattern realize the super sensitivity detection to DA, 1pM~
In 10 μM of concentration ranges, the logarithm (lgC of DA concentrationDA) and the good linear relationship of photocurrent response value presentation, detection limit
Up to 0.3pM.
(4) compared with traditional detection method, the optical electro-chemistry detection method of DA proposed in the present invention has operation more
The features such as simplicity is flexible, and instrument and equipment is simpler, and reagent dosage is few, and testing cost is cheap.
Detailed description of the invention
Fig. 1 (A) is the BiOCl/BiVO of preparation4The transmission electron microscope picture of/N-GQDs nano-complex；(B) for DA concentration with
The corresponding relationship of photocurrent response value (embedded figure is its linear relationship chart).
Specific embodiment
The present invention will be further described below with reference to examples:
Preparation step is as follows:
Step 1, preparation BiOCl/BiVO4/ N-GQDs nano-complex；
The optical electro-chemistry sensor of step 2, building dopamine (DA) sensitively without enzyme detection；
In step 1,1~2g ammonium citrate and 30 the step of preparing azepine graphene quantum dot (N-GQDs): are weighed first
After the mixing of~60mL water, it is transferred in three-neck flask, three-neck flask is placed in 140~200 DEG C of oil bath pans and is heated, on three-neck flask
Be connected to spherical condensation tube, condenser pipe gas outlet is tied with balloon, with ensure whole process in relatively closed, constant pressure environment into
Row.With the progress of heating reaction, balloon starts to expand slightly, and solution colour also becomes faint yellow or else disconnected intensification extremely by colourless
Yellow illustrates that N-GQDs is successfully synthesized.
In step 1, presoma pucherite (BiVO is prepared4) the step of: 4~5g, five nitric hydrate bismuth is weighed first to be dissolved in
In 10mL concentrated nitric acid, solution A is obtained, then weighs 1~2g ammonium metavanadate and is dissolved in 10mL sodium hydroxide solution (6mol/L), is obtained
To solution B.Then solution A is added drop-wise in solution B dropwise, obtains orange-yellow suspension, and continue to stir 1h.Then toward outstanding
Sodium hydroxide solution (6mol/L) is added dropwise in supernatant liquid dropwise and adjusts pH to 11~12.Mixed solution is finally added to sealing
In stainless steel autoclave, the temperature of calcination is 140~200 DEG C, and the reaction time is 8~12h, obtains presoma pucherite.
In step 1, ternary complex BiOCl/BiVO is prepared4The step of/N-GQDs: it is molten to weigh 0.05~0.1g pucherite
Solution stirs 0.5h, adds 1~5mL N-GQDs solution, be again stirring for 0.5h in 20mL hydrochloric acid (8mmol/L).Gained
Mixed solution be added in the stainless steel autoclave of sealing, the temperature of calcination is 140~200 DEG C, and the reaction time is 8~12h,
Obtain BiOCl/BiVO4/ N-GQDs nano-complex.
In step 2, BiOCl/BiVO is prepared with ultrapure water4/ N-GQDs dispersion liquid, takes quantitative BiOCl/BiVO4/N-
GQDs dispersion liquid is modified in ITO electrode, and using ITO electrode as working electrode, saturated calomel electrode is as reference electrode, platinum filament
As to electrode, by electrochemical workstation three-electrode system, under the irradiation of xenon source and photoelectricity is carried out in nitrogen atmosphere
Chemical analysis.After the photocurrent response of material tends towards stability, it is added dropwise into the quartzy photocell containing phosphate buffer solution
Configured dopamine solution successively carries out photoelectric analysis by concentration.In addition, in step 2, the intensity of the xenon source is
25%~100%, the ionic strength of the phosphate buffer solution is 0.02M~0.2M.When the photocurrent response of material tends to be steady
After fixed, configured dopamine solution is added dropwise into the quartzy photocell containing phosphate buffer solution, is successively carried out by concentration
Photoelectric analysis.In addition, the intensity of the xenon source is 25%~100%, the ion of the phosphate buffer solution in step 2
Intensity is 0.02M~0.2M.
Embodiment 1:
BiOCl/BiVO4The preparation of/N-GQDs nano-complex
Weigh a certain amount of BiVO4It is dissolved in 20mL hydrochloric acid, stirs 0.5h, add 1~5mL N-GQDs solution, then
Secondary stirring 0.5h.Resulting mixed solution is added in the stainless steel autoclave of sealing, the temperature of calcination is 140~200 DEG C,
Reaction time is 8~12h, obtains BiOCl/BiVO4/ N-GQDs nano-complex.
Embodiment 2:
The building of optical electro-chemistry sensor
Prepare BiOCl/BiVO4/ N-GQDs (2mg/mL) dispersion liquid takes quantitative dispersion liquid to modify processed
In ITO electrode, using ITO electrode as working electrode, as reference electrode, platinum filament is used as to electrode saturated calomel electrode, is passed through
Electrochemical workstation three-electrode system under the irradiation of xenon source and carries out photoelectrochemical assay in nitrogen atmosphere.Work as material
Photocurrent response tend towards stability after, be added dropwise and configure into the quartzy photocell containing phosphate buffer solution (pH=7.4)
Dopamine solution, successively carry out photoelectric analysis by concentration.
Fig. 1 (A) is the BiOCl/BiVO that the present embodiment obtains4The transmission electron microscope picture of/N-GQDs nano-complex, You Tuke
Know, hence it is evident that there are three kinds of different lattices, show successfully to prepare BiOCl/BiVO4/ N-GQDs nano-complex；Fig. 1 (B) is
The corresponding relationship (embedded figure is its linear relationship chart) for the DA concentration and photocurrent response value that the present embodiment obtains, can from figure
To find out, with the increase of DA concentration, BiOCl/BiVO4The photoelectric current of/N-GQDs/ITO is gradually increased, and photoelectric current size
Good linear relationship is presented between DA concentration.If Fig. 1 (B) is embedded in figure, in the concentration ranges of 1pM~10 μM, DA is dense
Logarithm (the lgC of degreeDA) and the good linear relationship of photocurrent response value presentation, detection limit is up to 0.3pM.
Claims (4)
1. a kind of construction method of the optical electro-chemistry sensor for no enzyme detection dopamine, which is characterized in that steps are as follows:
Step 1 prepares azepine graphene quantum dot solution:
It after ammonium citrate is dissolved in water, is transferred in oil bath, heating reaction is carried out under conditions of constant pressure airtight, after completion of the reaction
Obtain azepine graphene quantum dot solution；
Step 2 prepares presoma pucherite:
Five nitric hydrate bismuths are dissolved in concentrated nitric acid, solution A is obtained；Ammonium metavanadate is dissolved in sodium hydroxide solution, is obtained molten
Liquid B；Solution A is added drop-wise in solution B dropwise, is stirred evenly, mixed liquor C is obtained, then dropwise addition sodium hydroxide is molten into mixed liquor C
Liquid adjusts pH to 11~12, obtains mixed liquor D, mixed liquor D is transferred in stainless steel autoclave and carries out solvent thermal reaction, reacts
After, obtained solid product is pucherite；
Step 3 prepares ternary complex BiOCl/BiVO4/ N-GQDs:
The pucherite that step 2 is obtained is scattered in hydrochloric acid, is stirred evenly, and the azepine graphene quantum dot in step 1 is added
Solution stirs evenly, and obtains mixed liquor E, and mixed liquor E is transferred in stainless steel autoclave and carries out solvent thermal reaction, has been reacted
Bi Hou, obtained solid product are ternary complex BiOCl/BiVO4/N-GQDs；
The optical electro-chemistry sensor of step 4, building without enzyme detection dopamine:
By ternary complex BiOCl/BiVO4/ N-GQDs is scattered in ultrapure water, obtains BiOCl/BiVO4/ N-GQDs dispersion liquid,
By BiOCl/BiVO4/ N-GQDs dispersant liquid drop is applied in ITO electrode, using ITO electrode as working electrode, saturated calomel electrode
As reference electrode, platinum filament, which is used as, constitutes the optical electro-chemistry sensor without enzyme detection dopamine to electrode, by electrochemical operation
It stands three-electrode system, under the irradiation of xenon source and carries out photoelectrochemical assay in nitrogen atmosphere.
2. a kind of construction method of optical electro-chemistry sensor for no enzyme detection dopamine according to claim 1,
It is characterized in that, in step 1, the amount ratio of the ammonium citrate and water is 1~2g:30~60mL；Temperature in the oil bath is
140~200 DEG C.
3. a kind of construction method of optical electro-chemistry sensor for no enzyme detection dopamine according to claim 1,
It is characterized in that, in step 2, in the solution A, the amount ratio of five nitric hydrate bismuths and concentrated nitric acid is 4~5g:10mL；Solution B
In, the amount ratio of ammonium metavanadate and sodium hydroxide solution is 1~2g:10mL；In the mixed liquor C, the body of solution A and solution B
Product is than being 1:1；The sodium hydroxide solution is 6mol/L；The temperature of the solvent thermal reaction is 140~200 DEG C, when reaction
Between be 8~12h.
4. a kind of construction method of optical electro-chemistry sensor for no enzyme detection dopamine according to claim 1,
Be characterized in that, in step 3, in the mixed liquor E, pucherite, hydrochloric acid, azepine graphene quantum dot solution amount ratio be 0.05
~0.1g:20mL:1~5mL, the concentration of hydrochloric acid are 8mmol/L；The temperature of the solvent thermal reaction is 140~200 DEG C, reaction
Time is 8~12h.
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| CN108490057A (en) * | 2018-04-02 | 2018-09-04 | 中国科学院海洋研究所 | A kind of optical electro-chemistry detection method of sulfate reducing bacteria (SRB) |
| CN109142493B (en) * | 2018-07-17 | 2020-06-26 | 江苏大学 | Construction method of photoelectrochemical sensor for non-labeled detection of 4-chlorophenol |
| CN111380935B (en) * | 2018-12-28 | 2022-03-01 | Tcl科技集团股份有限公司 | Method for quantitatively detecting content of thiol ligand on surface of quantum dot |
| CN110297022A (en) * | 2019-06-28 | 2019-10-01 | 济南大学 | Natrium doping pucherite/graphene paste electrode sensor preparation method |
| CN112522862B (en) * | 2020-11-13 | 2022-02-01 | 南通大学 | Visible light driven antibacterial nanofiber and preparation method and application thereof |
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| CN113877632B (en) * | 2021-11-16 | 2023-08-01 | 江西省科学院应用化学研究所 | Preparation method of 2D bismuth vanadate@PDA core-shell structure composite material loaded by noble metal nanoparticles |
| CN113877631B (en) * | 2021-11-16 | 2023-08-11 | 江西省科学院应用化学研究所 | Preparation method of graphene quantum dot-supported bismuth vanadate nanocomposite capable of efficiently degrading heavy metal ions |
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