CN108088881A - A kind of preparation method based on polymer-carbon nanotube enzyme-free glucose sensor - Google Patents
A kind of preparation method based on polymer-carbon nanotube enzyme-free glucose sensor Download PDFInfo
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- CN108088881A CN108088881A CN201711370560.6A CN201711370560A CN108088881A CN 108088881 A CN108088881 A CN 108088881A CN 201711370560 A CN201711370560 A CN 201711370560A CN 108088881 A CN108088881 A CN 108088881A
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- polymer
- enzyme
- carbon nanotube
- glucose sensor
- free glucose
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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
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
- G01N27/3275—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction
- G01N27/3278—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction involving nanosized elements, e.g. nanogaps or nanoparticles
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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
- G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
Abstract
The invention discloses a kind of carbon nano-tube hybridization body being modified based on amphiphilic polymers for carrier, carried metal nanocatalyst particles, and it is applied to the method for making glucose sensor.This method includes the preparation of polymer carbon nano tube hybrid, the two big step of structure of enzyme-free glucose sensor.It realizes that macromolecular assembles altogether with one step of carbon nanotubes using the assembling driving force of amphiphilic macromolecular, prepares polymer carbon nano tube hybrid.While this hybrid has excellent stability, the advantages of combining two kinds of materials, has good electric conductivity and larger surface area；Therefore, electrode modified material is used as, energy payload has the metal nanoparticle of catalytic activity, and the wide enzyme-free glucose sensor of good stability, high sensitivity, detection range is made.In addition, the enzyme-free glucose sensor is easily integrated applied to microelectronic component, the fields such as biological medicine, life and health can be expected to be used for.
Description
Technical field
The present invention relates to electrochemical sensor field and Macromolecular self-assembly fields, and parents are based on more particularly, to one kind
Property polymer modification carbon nano-tube hybridization body for carrier, carried metal nanocatalyst particles, and be applied to making nothing
The method of enzymatic glucose sensor.
Background technology
Diabetes are the health problems of getting worse in world wide, may be with a variety of serious complication.According to
The report of world health organization, there are about 0.35 hundred million people in the world at present to suffer from diabetes.A large amount of evidences show diabetic
Glucose in Blood by Cyclic is higher than normal level, and excreting glucose on the other hand, in urine can also reflect seriously
Kidney trouble, therefore, the accurate content for detecting glucose in body fluid will be particularly important.The method of detection glucose has at present：
Chromatography, spectroscopic methodology and electrochemical method etc., and glucose sensor have miniaturization, low cost, it is quick the advantages that.Therefore,
Glucose sensor plays important role in the monitoring and control of diabetes.The glucose being most widely used at present passes
Sensor is the sensor based on enzymatic, however, since enzyme is easily subject to the shadow of temperature, pH, humidity and chemical substance in itself
It rings, this allows for the stability of glucolase sensor and recycling rate of waterused is poor.Therefore, development is a kind of quick, simply, can
The enzyme-free glucose sensor leaned on has important practical significance.
Carbon nanotubes is that a kind of have special construction (radial dimension is nanoscale, and axial dimension is micron dimension, pipe two
End group this sealing) One-dimensional Quantum material, there is larger specific surface area, higher chemical stability, stronger adsorption capacity
With excellent electric conductivity.Therefore during dressing agent of the carbon nanotubes as electrochemical reaction electrode, show outstanding electron transfer
Tenability, and have preferable electrochemistry and chemical stability in aqueous solution and non-aqueous solution.
Metal nano material is subject to that people's is extensive since it has higher specific surface area and higher catalytic activity
Concern.Using nanometer technology, it is expected to improve sensibility, detection range and the response time of sensor.It is passed commonly used in glucose
The metal electrode material of sensor has the noble metals such as Pt, Au, Rd, Ru and NiO, MnO2, the transiting metal oxidations such as CoO, ZnO, CuO
Object.However the catalytic activity of nano material is strongly dependent upon the size of itself and its distribution on carrier, therefore select to close
Suitable carrier is important for the catalytic performance for improving sensor.
In order to make full use of both nano materials, people have further attempted to receive by the use of carbon nanotubes as support metal
The template of rice catalyst, but since the special construction of carbon nanotubes causes its dissolubility is not good enough, easy entanglement is reunited etc..It needs pair
CNTs carries out surface modification, and homodisperse nano particle is obtained by covalently or non-covalently acting on, carbon pipe can be improved and exist
Dispersiveness in various organic solvents and the compatibility with macromolecule matrix, so as to enhance the performance of composite material.
Amphiphilic polymers are had rule by hydrophilic, hydrophobic segment or are randomly arranged and formed, therefore can in selective solvent
Self assembly is carried out, forms variously-shaped such as spherical, rodlike, bowl-shape, vesica nanoscale structures, and with surface-active
Matter.In amphiphilic polymers self assembling process, if can utilize between carbon nanotubes and polymer π-π effect, hydrogen bond action or
Intermolecular force between hydrophobe action breaks down carbon nanotubes is expected to obtain uniform and stable nanotube dispersion, from
And cause carbon nanotubes has in no enzyme sensor field to be more widely applied.
The content of the invention
In view of the problems of the existing technology, it is modified object of the present invention is to provide one kind based on amphiphilic polymers
Carbon nano-tube hybridization body for carrier, carried metal nanocatalyst particles, and be applied to and make glucose sensor
Method.The present invention by amphiphilic macromolecular main chain introduce can with carbon nanotubes interact monomeric building blocks,
Conductive carbon nanotubes is introduced during amphiphilic Macromolecular self-assembly simultaneously, utilizes the assembling driving force of amphiphilic macromolecular
It realizes that macromolecular assembles altogether with one step of carbon nanotubes, prepares polymer-carbon nanotube hybrid.Prepared polymer-carbon
" soft " and " hard " of carbon nanotubes of the effectively comprehensive polymer of nanotube hydridization physical efficiency, so as to excellent stability；In addition,
This polymer carbon nano tube hybrid is the carbon nano-tube modified structure of polymer nano-particle, and carbon nanotubes can improve hydridization
The electric conductivity of body, and polymer nano-particle can greatly improve the specific surface area of hybrid.Therefore, by the polymerization of this electric conductivity
Object-carbon nano-tube hybridization body is used as electrode modified material, and energy payload has the metal nanoparticle of catalytic activity, so as to make
Obtain the wide enzyme-free glucose sensor of good stability, high sensitivity, detection range.
Technical scheme is as follows：
A kind of preparation method based on polymer-carbon nanotube enzyme-free glucose sensor, polymer-carbon nanotube hydridization
The preparation of body, the structure of enzyme-free glucose sensor are as follows：
(1) preparation of polymer-carbon nanotube hybrid
Amphiphilic polymers are dissolved in organic solvent, addition carbon nanotubes, ultrasonic disperse 1h~for 24 hours, make amphiphilic poly-
It closes object and carbon nanotubes fully acts on, obtain homodisperse amphiphilic polymers/carbon nano tube dispersion liquid；Delay in dispersion liquid
Slow 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
To polymer-carbon nanotube hydridization liquid solution.
The amphiphilic polymers are block copolymer, graft copolymer, random copolymer, branched polymer, conjugation are poly-
One kind in object is closed, the organic solvent is one in n,N-Dimethylformamide, tetrahydrofuran, dimethyl sulfoxide, dioxane
Kind；The initial solubility of amphiphilic polymers is 0.1mg/mL~200mg/mL；The amphiphilic polymers and carbon nanotubes matter
Amount is than being 1:0.01~1:1, the active force between the amphiphilic polymers and carbon nanotubes includes hydrogen for non-covalent bond effect
One or more of key effect, electrostatic interaction, π-π effects, coordination.
(2) structure of enzyme-free glucose sensor
Modified electrode is pre-processed, then polymer-carbon nanotube hydridization liquid solution in step (1) is passed through into drop coating, spin coating
Or the method for electrophoretic deposition is modified to electrode surface, obtains polymer-carbon nanotube hybrid modified electrode, drying at room temperature.With
Afterwards by the method for vacuum sputtering or electrochemical reduction metal nano catalyst precursor, uniformly divide in modified electrode Surface Creation
The metal nano catalyst particle of cloth is to get to enzyme-free glucose sensor.
The electrode is gold electrode, one kind in glass-carbon electrode, ITO electrode, carbon paste electrode；The polymer-carbon nanometer
Amphiphilic polymers concentration is 0.1mg/mL~200mg/mL, amphiphilic polymers and carbon nanotube mass in pipe hydridization liquid solution
Than for 1:0.01~1:1；The drop coating method is pipettes the μ L polymer-carbon nanotube hydridization liquid solution drop coatings of 5 μ L~30 in electricity
Pole surface；Electrode is is immersed in polymer-carbon nanotube hydridization liquid solution by the electrophoretic deposition method, by controlling voltage
In electrode surface, specific electrophoretic deposition process condition is with the modification of polymer-carbon nanotube hybrid is made with the time：Deposition voltage
0.5V~10V, sedimentation time 1min~10min；The metal nano catalyst is Pt, Pb, Ni, Cu, Au, Ag, NiO, MnO2、
One kind in CoO, ZnO, CuO；The precursor solution concentration be 0.01mmol/L~10mmol/L, the electrochemical reduction side
Method is cyclic voltammetry, one kind in potentiostatic method, galvanostatic method.
The present invention is beneficial to be had technical effect that：
1st, the present invention prepares polymer-carbon nanotube hybrid using amphiphilic macromolecular is carbon nano-tube modified, is used
Make carrier to load metal nanocatalyst particles and be applied to structure enzyme-free glucose sensor.Prepared hybrid is organic poly-
Object and inorganic carbon nano tube compound material are closed, the unique advantage of the two can be combined, there is excellent comprehensive performance；Polymer is to receive
Rice corpuscles form modifies the specific surface area that in carbon nano tube surface, can effectively improve composite material, and the introducing of carbon nanotubes is then
The electric conductivity of material can be greatly improved；Using this hybrid as carrier to load metal nanocatalyst particles, gold can be improved
Belong to the load capacity of nanocatalyst particles, and can play carbon nanotubes and metal nano catalyst particle and concerted catalysis make
With so as to assign the superior sensing capabilities of sensor and stability.
2nd, the amphiphilic polymers structure designability that the present invention uses is strong, synthesis is simple, and carbon nanotubes is as a kind of excellent
Different conductive material is cheap, and the combination of organic polymer and inorganic carbon nanotubes can be solved effectively to sense in sensor and applied
The problem of layer and stability, it is easy to accomplish industrialized production and application.
3rd, enzyme-free glucose sensor prepared by the present invention can be with response is fast, detection range is wide, high sensitivity, stabilization
The advantages that property is good.
4th, the present invention, can be in glucose sensor application by polymer material science and electrochemical sensing field reasonable combination
On the basis of expand be applied to structure other biological, chemical sensor, so as to be widely used in food security, biological medicine and life
Order the fields such as health.
Description of the drawings
Fig. 1：The enzyme-free glucose sensor of the present invention prepares schematic diagram；
Fig. 2：The number of pure nano-carbon tube (a) and polymer-carbon nanotube hybrid (b) solution in the embodiment of the present invention 1
Photo；
Fig. 3：The transmission electron microscope picture of prepared polymer-carbon nanotube hybrid in the embodiment of the present invention 1；
Fig. 4：The chronoa mperometric plot of enzyme-free glucose sensor detection glucose in the embodiment of the present invention 1.
Specific embodiment
It is explained further the present invention With reference to embodiment, but the invention is not limited in used in following instance
Condition.
Embodiment 1
A kind of preparation method based on polymer-carbon nanotube enzyme-free glucose sensor, it is characterised in that preparation process
It is as follows：
(1) preparation of polymer-carbon nanotube hybrid
Amphiphilic polymers are dissolved in n,N-Dimethylformamide, are made into the polymer solution of 5mg/mL, carbon is added in and receives
Mitron, for 24 hours, obtaining homodisperse amphiphilic polymers/carbon nano tube dispersion liquid, (concentration of carbon nanotubes is ultrasonic disperse
1mg/mL)；Ultra-pure water is slowly dropped into dispersion liquid and carries out self assembly, dialysis 2d obtains polymer-carbon nanotube after stirring 4h
Hydridization liquid solution；The digital photograph of pure nano-carbon tube (a) and polymer-carbon nanotube hybrid (b) solution is as shown in Fig. 2, can
See that pure nano-carbon tube is gathered in the bottom of solution, and polymer-carbon nanotube hydridization liquid solution is then uniform mass colour, performance
Go out good dispersion stabilization；And this result also has performance in transmission electron microscope, as shown in figure 3, Polymer adsorption is received in carbon
Nanotube surface prevents entanglement and reunion between carbon nanotubes, so as to form beading structure, shows polymer-carbon nanotube
The successful preparation of hybrid.
(2) structure of enzyme-free glucose sensor
By pretreatment of glassy carbon electrode, and the 10 μ L of polymer-carbon nanotube hydridization liquid solution in removing step (1) are in glass carbon
On electrode, polymer-carbon nanotube hybrid modified electrode is obtained, is immersed after drying at room temperature in silver nitrate solution, passes through permanent electricity
Position reduction silver nitrate is in the equally distributed Nano silver grain of modified electrode Surface Creation, and the concentration of silver nitrate is 1mmol/L, deposition
Voltage is -0.2V, and sedimentation time is 90s to get to enzyme-free glucose sensor.Fig. 4 is the meter that the sensor detects glucose
When current curve, it can be seen that with the increase of glucose content, current value linearly increases, show the enzyme-free glucose sense
The successful structure of device.
Embodiment 2
A kind of preparation method based on polymer-carbon nanotube enzyme-free glucose sensor, it is characterised in that preparation process
It is as follows：
(1) preparation of polymer-carbon nanotube hybrid
Amphiphilic polymers are dissolved in n,N-Dimethylformamide, are made into the polymer solution of 5mg/mL, carbon is added in and receives
Mitron, for 24 hours, obtaining homodisperse amphiphilic polymers/carbon nano tube dispersion liquid, (concentration of carbon nanotubes is ultrasonic disperse
1mg/mL)；Ultra-pure water is slowly dropped into dispersion liquid and carries out self assembly, dialysis 2d obtains polymer-carbon nanotube after stirring 4h
Hydridization liquid solution.
(2) structure of enzyme-free glucose sensor
Electrode table is electrodeposited in by pretreatment of glassy carbon electrode, and by the polymer-carbon nanotube hybrid in step (1)
Face, deposition voltage 0.7V, sedimentation time 5min obtain polymer-carbon nanotube hybrid modified electrode, after drying at room temperature
It immerses in silver nitrate solution, silver nitrate is reduced in the equally distributed Nano silver grain of modified electrode Surface Creation by constant potential,
The concentration of silver nitrate is 1mmol/L, and deposition voltage is -0.2V, and sedimentation time is 90s to get to enzyme-free glucose sensor.
Embodiment 3
A kind of preparation method based on polymer-carbon nanotube enzyme-free glucose sensor, it is characterised in that preparation process
It is as follows：
(1) preparation of polymer-carbon nanotube hybrid
Amphiphilic polymers are dissolved in n,N-Dimethylformamide, are made into the polymer solution of 5mg/mL, carbon is added in and receives
Mitron, for 24 hours, obtaining homodisperse amphiphilic polymers/carbon nano tube dispersion liquid, (concentration of carbon nanotubes is ultrasonic disperse
2mg/mL)；Ultra-pure water is slowly dropped into dispersion liquid and carries out self assembly, dialysis 2d obtains polymer-carbon nanotube after stirring 4h
Hydridization liquid solution.
(2) structure of enzyme-free glucose sensor
Electrode table is electrodeposited in by pretreatment of glassy carbon electrode, and by the polymer-carbon nanotube hybrid in step (1)
Face, deposition voltage 0.7V, sedimentation time 5min, obtains the electrode of polymer-carbon nanotube hybrid modified, and room temperature is done
It is immersed after dry in silver nitrate solution, silver nitrate is reduced in the equally distributed nano grain of silver of modified electrode Surface Creation by constant potential
Son, the concentration of silver nitrate is 1mmol/L, and deposition voltage is -0.2V, and sedimentation time senses for 90s to get to enzyme-free glucose
Device.
Claims (10)
1. a kind of preparation method based on polymer-carbon nanotube enzyme-free glucose sensor, it is characterised in that polymer-carbon is received
Prepared by mitron hybrid, the structure of enzyme-free glucose sensor, is as follows：
(1) prepared by polymer-carbon nanotube hybrid：Amphiphilic polymers are dissolved in organic solvent, add in carbon nanotubes, are surpassed
Sound disperses 1h~for 24 hours, obtains homodisperse amphiphilic polymers/carbon nano tube dispersion liquid；It is slowly dropped into dispersion liquid super
Pure water, stirring 1h~for 24 hours, mixed liquor is then placed in dialysis 1d~7d in bag filter, obtains polymer-carbon nanotube hybrid
Solution；
(2) structure of enzyme-free glucose sensor：Modified electrode is pre-processed, then by the polymer-carbon nanotube in step (1)
Hydridization liquid solution is modified by the method for drop coating, spin coating or electrophoretic deposition to electrode surface, obtains polymer-carbon nanotube hydridization
Body modified electrode, drying at room temperature；Then by the method for vacuum sputtering or electrochemical reduction metal nano catalyst precursor,
The equally distributed metal nano catalyst particle of modified electrode Surface Creation is to get to enzyme-free glucose sensor.
2. the preparation method of polymer-carbon nanotube enzyme-free glucose sensor according to claim 1, it is characterised in that institute
It is block copolymer, graft copolymer, random copolymer, branched polymer, conjugated polymers to state amphiphilic polymers in step (1)
One kind in object.
3. the preparation method of polymer-carbon nanotube enzyme-free glucose sensor according to claim 1, it is characterised in that institute
It is one kind in N,N-dimethylformamide, tetrahydrofuran, dimethyl sulfoxide, dioxane to state organic solvent in step (1).
4. the preparation method of polymer-carbon nanotube enzyme-free glucose sensor according to claim 1, it is characterised in that institute
It is 0.1mg/mL~200mg/mL, amphiphilic polymers and carbon nanotubes matter to state the initial solubility of amphiphilic polymers in step (1)
Amount is than being 1:0.01~1:1.
5. the preparation method of polymer-carbon nanotube enzyme-free glucose sensor according to claim 1, it is characterised in that institute
State the active force in step (1) between amphiphilic polymers and carbon nanotubes includes hydrogen bond action, electrostatic for non-covalent bond effect
One or more of effect, π-π effects, coordination.
6. the preparation method of polymer-carbon nanotube enzyme-free glucose sensor according to claim 1, it is characterised in that institute
It is one kind in gold electrode, glass-carbon electrode, ITO electrode, carbon paste electrode to state modified electrode in step (2).
7. the preparation method of polymer-carbon nanotube enzyme-free glucose sensor according to claim 1, it is characterised in that institute
It is 0.1mg/mL~200mg/mL to state in step (2) amphiphilic polymers concentration in polymer-carbon nanotube hydridization liquid solution, double
Parent's property polymer is 1 with carbon nanotube mass ratio:0.01~1:1.
8. the preparation method of polymer-carbon nanotube enzyme-free glucose sensor according to claim 1, it is characterised in that institute
Drop coating method is stated in step (2) to pipette the μ L polymer-carbon nanotubes hydridization liquid solution drop coatings of 5 μ L~30 in electrode surface, electricity
Electrode is is immersed in polymer-carbon nanotube hydridization liquid solution by swimming deposition method, by controlling voltage and making to gather with the time
Object-carbon nano-tube hybridization body modification is closed in electrode surface, specific electrophoretic deposition process condition is：Deposition voltage 0.5V~10V sinks
Product time 1min~10min.
9. the preparation method of polymer-carbon nanotube enzyme-free glucose sensor according to claim 1, it is characterised in that institute
It is Pt, Pb, Ni, Cu, Au, Ag, NiO, MnO to state metal nano catalyst in step (2)2, one kind in CoO, ZnO, CuO.
10. according to the preparation method of polymer-carbon nanotube enzyme-free glucose sensor described in claim 9, metal nano is urged
The preparation of agent derives from corresponding precursor solution, and precursor solution concentration is 0.01mmol/L~10mmol/L.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101315345A (en) * | 2008-07-15 | 2008-12-03 | 四川大学 | Modified electrode and production method for detecting grape-sugar concentration in non-enzyme condition |
| CN102046517A (en) * | 2008-05-28 | 2011-05-04 | 株式会社百奥尼 | Nanocomposites consisting of carbon nanotube and metal and a process for preparing the same |
| CN105670444A (en) * | 2016-04-12 | 2016-06-15 | 江南大学 | Carbon-nanometer-tube/gold-nanometer-particle composite function coating prepared based on amphiphilic polymer |
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2017
- 2017-12-19 CN CN201711370560.6A patent/CN108088881A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102046517A (en) * | 2008-05-28 | 2011-05-04 | 株式会社百奥尼 | Nanocomposites consisting of carbon nanotube and metal and a process for preparing the same |
| CN101315345A (en) * | 2008-07-15 | 2008-12-03 | 四川大学 | Modified electrode and production method for detecting grape-sugar concentration in non-enzyme condition |
| CN105670444A (en) * | 2016-04-12 | 2016-06-15 | 江南大学 | Carbon-nanometer-tube/gold-nanometer-particle composite function coating prepared based on amphiphilic polymer |
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Application publication date: 20180529 |