CN108169298A - A kind of preparation method for the disposable sensor for detecting dopamine - Google Patents
A kind of preparation method for the disposable sensor for detecting dopamine Download PDFInfo
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- CN108169298A CN108169298A CN201711370559.3A CN201711370559A CN108169298A CN 108169298 A CN108169298 A CN 108169298A CN 201711370559 A CN201711370559 A CN 201711370559A CN 108169298 A CN108169298 A CN 108169298A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
Polymer/carbon Nanotubes Composites are prepared based on amphiphilic polymers modified carbon nano-tube the invention discloses one kind and are used as electrode modified material, modify the method for preparing the disposable sensor that can detect dopamine in screen printing electrode surface.Macroscopic single crystal is simple for process in Polymer/carbon Nanotubes Composites prepared by the present invention, and conductive carbon nanotube is of low cost, therefore conducive to mass production, is of very high actual application value.The combination of organic polymer and inorganic carbon nanotube can assign sensitive coating excellent comprehensive performance, had based on sensor prepared by the composite material to the detection of dopamine it is highly selective with it is highly sensitive.In addition, the sensor has throwing property, portability, the problem of meeting the requirement of safety and health aspect, while avoid cross contamination in practical application.The combination of functional high molecule material and electrochemical sensing technology is expected to widely develop applied to numerous areas such as biological medicine, life and healths.
Description
Technical field
The present invention relates to electrochemical sensor and polymeric material fields, and in particular to one kind is changed based on amphiphilic polymers
Property carbon nanotube prepare Polymer/carbon Nanotubes Composites and be used as electrode modified material, modify in silk-screen printing electricity
Pole surface preparation can detect the method for the disposable sensor of dopamine.
Background technology
Dopamine is a kind of important catechu amine neurotransmitters, is used to help cell and sends pulsed chemical substance, with
The information such as desire, the feeling and excitement of brain are transmitted closely related.The deficiency of dopamine can make us the ability of muscle out of hand,
Even result in a variety of mental disorders such as Parkinson's disease, schizophrenia, bipolar disorder, alzheimer's disease.At present,
The method for measuring dopamine has chromatography, fluorescence spectrophotometry, mass spectrography and spectrophotometry, but these conventional methods exist
Detection device is expensive, it is complicated for operation, a series of shortcomings such as need professional operator, detection time-consuming.
Compared to the above, electrochemical sensing technology has response fast, high sensitivity, at low cost and easily operated
The advantages that, it is therefore widely used in the fields such as biological medicine, food security.Dopamine molecule is easily oxidised there are two including
Phenolic hydroxyl group, have very high electro-chemical activity, therefore using electrochemical sensing technology to dopamine detection have it is very strong
Feasibility.However, since the oxidizing potential of the oxidizing potential and dopamine of uric acid and ascorbic acid is very close, pass through electricity
Chemical method, which directly detects dopamine, has the problem of detecting and selecting property is poor.Therefore, development has both highly sensitive and strong selectivity
Dopamine Sensor it is significant.
Carbon nanotube (CNTs) be it is a kind of on nanoscale have complete molecular structure One-dimensional Quantum material, have with
Lamellar structure as graphite-phase.Carbon nanotube has great draw ratio, excellent mechanical strength and good conductive and heat-conductive
Ability is a kind of ideal conductive material, so as to be widely used in electrochemical sensor field.In recent years, by carbon nanotube
Gradually cause the concern of people as electrode modified material structure Dopamine Sensor, this is mainly due to the delocalizations of carbon nanotube
Pi bond can be interacted with dopamine by π-π, so as to realize the selection to dopamine in the presence of uric acid and ascorbic acid
Property identification.However, the special construction of carbon nanotube causes, its dissolubility is not good enough, easy entanglement is reunited, therefore in actual production, base
Still there is very big challenge in the Dopamine Sensor that carbon nanotube structure performance is stablized.
Invention content
In view of the problems of the existing technology, the present invention provides one kind to be based on amphiphilic polymers modified carbon nano tube control
Standby Polymer/carbon Nanotubes Composites are simultaneously used as electrode modified material, modify that prepared in screen printing electrode surface can
To detect the method for the disposable sensor of dopamine.Polymer/carbon Nanotubes Composites prepared by the present invention are in water
With good dispersion stabilization, it is used as that there is large specific surface area, good conductivity during electrode modified material, based on this
Sensor prepared by Polymer/carbon Nanotubes Composites have to the detection of dopamine it is highly selective with highly sensitive, and
This sensor is disposable sensor, so as to have the advantages that portable, no cross contamination in actual use.
Technical scheme is as follows：
A kind of preparation method for the disposable sensor for detecting dopamine, the synthesis of amphiphilic polymers, polymer/carbon are received
The preparation of mitron composite material, the preparation of disposable sensor are as follows：
(1) synthesis of amphiphilic polymers
Under condition of normal pressure, acrylic monomer, photosensitive monomer, acrylic ester monomer are dissolved in dioxane；It adds in few
Amount initiator simultaneously makes its dissolving；12h~48h is reacted under the conditions of nitrogen protection, 60 DEG C~90 DEG C；After reaction, with oil
Ether is precipitating reagent, and tetrahydrofuran is solvent, and products therefrom is dried in vacuo to get amphiphilic polymerization by repeated precipitation dissolving
Object.
The acrylic monomer is acrylic acid, one kind in methacrylic acid；The photosensitive monomer for 2- methylols-
(4- methylcoumarins) oxygen ethyl-methacrylate, 7- (4- vinyl benzyls oxygroup) -4- methylcoumarins, 2- cinnamic acid acyls
One or both of oxygen ethyl-methacrylate；The acrylic ester monomer is Isooctyl acrylate monomer, methacrylic acid
One or both of different monooctyl ester, isodecyl methacrylate, lauryl methacrylate；The initiator is two isobutyl of azo
One kind in nitrile, azobisisoheptonitrile；The synthetic method of polymers be free radical polymerization, acrylic monomer, photosensitive monomer,
The molar ratio of acrylic ester monomer is 5:1:4~5:5:5, initiator amount is the 0.5%~3% of total moles monomer.
(2) preparation of Polymer/carbon Nanotubes Composites
Above-mentioned amphiphilic polymers are dissolved in organic solvent, addition carbon nanotube, ultrasonic disperse 1h~for 24 hours, it obtains
The Polymer/carbon Nanotubes Composites of even dispersion；Be slowly dropped into dispersion liquid ultra-pure water carry out self assembly, stirring 1h~
For 24 hours, mixed liquor is placed in dialysis 1d~7d in bag filter after assembling, obtains Polymer/carbon Nanotubes Composites.
The carbon nanotube is single-walled carbon nanotube, one kind in double-walled carbon nano-tube, multi-walled carbon nanotube, and the carbon is received
Mitron caliber is 5nm~20nm, and length is 10 μm~100 μm；The organic solvent is N,N-dimethylformamide, tetrahydrochysene furan
It mutters, one kind in dimethyl sulfoxide, dioxane；The initial solubility of amphiphilic polymers is 0.1mg/mL~200mg/mL, double
Parent's property polymer is 1 with carbon nanotube mass ratio:0.01~1:1, the effect between the amphiphilic polymers and carbon nanotube
Power includes one or more of hydrogen bond action, electrostatic interaction, π-π effects, coordination for non-covalent bond effect.
(3) preparation of disposable sensor
Polymer/carbon Nanotubes Composites described in step (2) are coated in sensor electrode surface, N2It is done under environment
It is dry to obtain disposable sensor.
The sensor electrode be screen printing electrode, the screen printing electrode collection working electrode, to electrode, reference electricity
Pole is whole in one；The working electrode host material of the screen printing electrode is gold, one kind in glass carbon, graphite, ITO, carbon slurry；
The painting method is drop-coating, one kind in spray coating method, spin-coating method, bar coating method, electrophoretic deposition；The electrophoretic deposition
Method condition is deposition voltage 0.5V~15.0V, and sedimentation time is 1min~15min.
The advantage of the invention is that：
1st, the present invention has both the poly- of Investigation of stabilized dispersion of nano and electric conductivity using the preparation of amphiphilic polymers modified carbon nano-tube
Object/carbon nano tube compound material is closed, amphiphilic polymers synthesis technology is simple, and carbon nanotube is as a kind of excellent conductive material
Cheap, the combination of organic polymer and inorganic carbon nanotube assigns sensitive coating excellent comprehensive performance, therefore is conducive to criticize
Quantization production, is of very high actual application value.
2nd, the present invention builds Dopamine Sensor using Polymer/carbon Nanotubes Composites as electrode modified material, this
Kind composite material has big specific surface area and since the protonation of acrylic monomer in polymer so that composite material is whole
Bear electricity, therefore quick, a large amount of enrichments to lotus dopamine on schedule are easily achieved, so as to realize, selection quick to dopamine
Property detection；And the introducing of carbon nanotube can enhance the electric conductivity of sensor, so that prepared sensor is for dopamine
Detection have high sensitivity.
3rd, the present invention is based on the design of the disposable sensor of screen printing electrode, there is small, light weight, portable
Band, the characteristics of can detecting in real time, the problem of avoiding cross contamination in practical application, while meet safety and health aspect
It is required that contribute to the foundation of portable medical detection system.
4th, polymer material science and electrochemical sensing field reasonable combination are expected to be widely applied to food and pacified by the present invention
Entirely, the fields such as biological medicine, life movement.
Description of the drawings
Fig. 1：The disposable sensor of the present invention prepares schematic diagram；
Fig. 2：The digital photograph and dimensional drawing of the disposable sensor prepared in the embodiment of the present invention 1；
Fig. 3：The SEM figures of the disposable working sensor electrode surface pattern prepared in the embodiment of the present invention 1；
Fig. 4：Differential pulse voltammetry of the disposable sensor in dopamine and ascorbic acid solution in the embodiment of the present invention 1
Curve；
Fig. 5：The linear relationship curve graph of disposable sensor detection dopamine in test case of the present invention.
Specific embodiment
The present invention is explained further, but the invention is not limited in used in following instance With reference to embodiment
Condition.
Embodiment 1
A kind of preparation method for the disposable sensor for detecting dopamine, specific preparation process are as follows：
(1) synthesis of amphiphilic polymers
Under condition of normal pressure, by acrylic acid, 7- (4- vinyl benzyls oxygroup) -4- methylcoumarins, Isooctyl acrylate monomer to rub
That ratio 5:5:5 are dissolved in dioxane；Add in initiator azodiisobutyronitrile (by monomer total moles than 2%) and make its dissolving；
It is reacted for 24 hours under the conditions of nitrogen protection, 65 DEG C；After reaction, using petroleum ether as precipitating reagent, tetrahydrofuran is solvent, repeatedly
Precipitation dissolving, products therefrom is dried in vacuo to get amphiphilic polymers PAVE.
(2) preparation of Polymer/carbon Nanotubes Composites
The above-mentioned amphiphilic polymers PAVE of 5mg are dissolved in 10mL n,N-Dimethylformamide, are made into the polymerization of 5mg/mL
Object solution, adds in 2mg carbon nanotubes, and ultrasonic disperse for 24 hours, obtains homodisperse amphiphilic polymers/carbon nano tube dispersion liquid
(a concentration of 0.2mg/mL of carbon nanotube)；Ultra-pure water is slowly dropped into dispersion liquid and carries out self assembly, stirs the 2d that dialyses afterwards for 24 hours
Obtain Polymer/carbon Nanotubes Composites.
(3) preparation of disposable sensor
By Polymer/carbon Nanotubes Composites drop coating described in step (2) in screen printing electrode surface, drop coating dispersion
Liquid is 10 μ L.In N2Disposable sensor is dried to obtain under environment.Fig. 2 be prepared working electrode digital photograph and dimensional drawing,
Prepared Dopamine Sensor size is smaller as can be seen from Fig., has portability, and sensor electrode is screen printing electrode,
It is of low cost therefore with throwing property.Fig. 3 is the SEM figures of sensor electrode surface pattern, it can be seen that polymer/carbon nano-tube
Composite sensing coating is interlaced beading network structure, this configuration increases the specific surface area of electrode, so as to
The adsorption capacity of dopamine molecule when improving detection, so as to improve sensor detection performance.
Embodiment 2
A kind of preparation method for the disposable sensor for detecting dopamine, it is characterised in that preparation process is as follows：
(1) synthesis of amphiphilic polymers
With 1 step 1 of embodiment
(2) preparation of Polymer/carbon Nanotubes Composites
The above-mentioned amphiphilic polymers PAVE of 5mg are dissolved in 10mL n,N-Dimethylformamide, are made into the polymerization of 5mg/mL
Object solution adds in 5mg carbon nanotubes, and ultrasonic disperse for 24 hours, obtaining homodisperse Polymer/carbon Nanotubes Composites, (receive by carbon
A concentration of 0.5mg/mL of mitron)；Ultra-pure water is slowly dropped into dispersion liquid and carries out self assembly, dialysis 2d is obtained afterwards for 24 hours for stirring
Polymer/carbon Nanotubes Composites.
(3) preparation of disposable sensor
Polymer/carbon Nanotubes Composites described in step (2) are electrodeposited in screen printing electrode surface, deposition electricity
1.0V, sedimentation time 180s is pressed to obtain disposable sensor.
Test case
Disposable sensor is to the Electrochemical Detection of dopamine (DA)
(1) anti-interference test
It is 1.0 × 10 that the disposable sensor that embodiment 1 prepares is immersed concentration-3mol·L-1Dopamine and anti-
Bad hematic acid phosphate delays in solution (pH 7.0), sample is tested using differential pulse voltammetry, impulse amplitude 50mV,
Pulse period is 0.5s, pulse width 50mS, voltage increment 4mV.Fig. 4 is dopamine and ascorbic acid in 7.0 phosphoric acid of pH
Differential pulse voltammetry curve in salt buffer, as seen from the figure, prepared disposable sensor only have sound to dopamine
It should.
(2) differential pulse voltammetry (DPV) is tested
The disposable sensor that embodiment 1 prepares is immersed into concentration respectively and is followed successively by (a) 1.0 × 10-6mol·L-1,
(b)5.0×10-6mol·L-1, (c) 1.0 × 10-5mol·L-1, (d) 3.0 × 10-5mol·L-1, (e) 5.0 × 10-5mol·L-1, (f) 1.0 × 10-4mol·L-1, (g) 3.0 × 10-4mol·L-1, (h) 5.0 × 10-4mol·L-1, (i) 8.0 × 10- 4mol·L-1, (j) 1.0 × 10-3mol·L-1DOPA amine phosphate delay in solution (pH 7.0), using differential pulse voltammetry
Sample is tested, impulse amplitude 50mV, pulse period 0.5s, pulse width 50mS, voltage increment 4mV.Fig. 5
To detect the linear relationship curve graph of dopamine, as seen from the figure, in 1 μM~300 μM and 300 μM~1000 μM concentration ranges
With relatively good linear relationship.
Claims (8)
1. a kind of preparation method for the disposable sensor for detecting dopamine, it is characterised in that prepare and condition is as follows：
(1) synthesis of amphiphilic polymers:It is under condition of normal pressure, acrylic monomer, photosensitive monomer, acrylic ester monomer is molten
In dioxane；It adds in a small amount of initiator and makes its dissolving；12h~48h is reacted under the conditions of nitrogen protection, 60 DEG C~90 DEG C；
After reaction, using petroleum ether as precipitating reagent, tetrahydrofuran is solvent, and products therefrom progress vacuum is done in repeated precipitation dissolving
It is dry to get amphiphilic polymers；
(2) prepared by Polymer/carbon Nanotubes Composites：Above-mentioned amphiphilic polymers are dissolved in organic solvent, carbon is added in and receives
Mitron, ultrasonic disperse 1h~for 24 hours, obtain homodisperse amphiphilic polymers/carbon nano tube dispersion liquid；In dispersion liquid slowly
Instillation ultra-pure water progress self assembly, stirring 1h~for 24 hours, mixed liquor is placed in dialysis 1d~7d in bag filter after assembling, is obtained
Polymer/carbon Nanotubes Composites；
(3) preparation of disposable sensor：Polymer/carbon Nanotubes Composites described in step (2) are coated in screen printing
Brush electrode surface, N2Disposable sensor is dried to obtain under environment.
2. a kind of preparation method for the disposable sensor for detecting dopamine according to claim 1, it is characterised in that described
The synthetic method of amphiphilic polymers is free radical polymerization in step (1), and the acrylic monomer is acrylic acid, metering system
One kind in acid, the photosensitive monomer is 2- methylols-(4- methylcoumarins) oxygen ethyl-methacrylate, 7- (4- ethylene
Base benzyloxy) -4- methylcoumarins, one or both of 2- cinnamic acids acyloxyethyl-methacrylate, the acrylic acid
Esters monomer is Isooctyl acrylate monomer, in isooctyl methacrylate, isodecyl methacrylate, lauryl methacrylate
One or two, acrylic monomer, photosensitive monomer, acrylic ester monomer molar ratio be 5:1:4~5:5:5, initiator
Dosage is the 0.5%~3% of total moles monomer.
3. a kind of preparation method for the disposable sensor for detecting dopamine according to claim 1, it is characterised in that described
Acrylic monomer is hydrophilic monomer in step (1), and photosensitive monomer contains conjugated structure, and acrylic ester monomer is hydrophobicity
Monomer.
4. a kind of preparation method for the disposable sensor for detecting dopamine according to claim 1, it is characterised in that described
The initial solubility of amphiphilic polymers is 0.1mg/mL~200mg/mL, amphiphilic polymers and carbon nanotube mass in step (2)
Than being 1:0.01~1:1；The carbon nanotube is single-walled carbon nanotube, one kind in double-walled carbon nano-tube, multi-walled carbon nanotube,
The carbon nanotube caliber is 5nm~20nm, and length is 10 μm~100 μm.
5. a kind of preparation method for the disposable sensor for detecting dopamine according to claim 1, it is characterised in that described
Active force in step (2) between amphiphilic polymers and carbon nanotube includes hydrogen bond action for non-covalent bond effect, electrostatic is made
With one or more of, π-π effect, coordination.
6. a kind of preparation method for the disposable sensor for detecting dopamine according to claim 1, it is characterised in that described
Sensor electrode is screen printing electrode, and the screen printing electrode collects working electrode, whole in one to electrode, reference electrode；
The working electrode host material of the screen printing electrode is gold, one kind in glass carbon, graphite, ITO, carbon slurry.
7. a kind of preparation method for the disposable sensor for detecting dopamine according to claim 1, it is characterised in that described
Painting method described in step (3) is drop-coating, one kind in spray coating method, spin-coating method, bar coating method, electrophoretic deposition.
8. a kind of preparation method for the disposable sensor for detecting dopamine according to claim 7, it is characterised in that described
Electrophoretic deposition method condition is deposition voltage 0.5V~10.0V, and sedimentation time is 1min~15min.
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| CN110470715A (en) * | 2019-09-11 | 2019-11-19 | 江南大学 | A kind of preparation method of the screen printing electrode of composite nano materials modification |
| CN110470716A (en) * | 2019-09-11 | 2019-11-19 | 江南大学 | A kind of preparation method of the screen printing electrode of composite nano materials modification |
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Application publication date: 20180615 |