CN107966487A - A kind of method that composite sensing coating is prepared based on electrophoresis codeposition - Google Patents
A kind of method that composite sensing coating is prepared based on electrophoresis codeposition Download PDFInfo
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- CN107966487A CN107966487A CN201711170175.7A CN201711170175A CN107966487A CN 107966487 A CN107966487 A CN 107966487A CN 201711170175 A CN201711170175 A CN 201711170175A CN 107966487 A CN107966487 A CN 107966487A
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- molecular recognition
- composite sensing
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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
Abstract
The invention discloses a kind of method that composite sensing coating is prepared based on electrophoresis codeposition, which includes the preparation of supporting molecular Recognition unit polymer nano-particle, the preparation of mixed deposit liquid, the three big step of preparation of composite sensing coating.Polymer nano-particle and inorganic conductive nano material are deposited on by electrode surface by a step electro-deposition at the same time in the present invention, polymer nano-particle can keep its identification activity for a long time while molecular recognition primitive fixed amount is improved；And coating preparation efficiency can be greatly improved while coating quality is ensured by being co-deposited technology of preparing, it is easy to accomplish mass industrial production；In addition, prepared composite sensing coating can be effectively with reference to " soft " of organic component and " hard " property of inorganic component, so that the composite coating has longer service life in practical applications, the sensor based on composite coating structure has extensive actual application value in fields such as food security, biological medicine and environment monitorings.
Description
Technical field
The present invention relates to self-assembling technique, electrophoretic deposition technique, function and service coating and electrochemical sensor field, especially
Be be related to it is a kind of by electrophoretic deposition that the polymer nano-particle of supporting molecular Recognition unit and inorganic conductive nano-particle is same
When be deposited on sensor electrode surface, and use it for the method for preparing composite sensing coating.
Background technology
Biology sensor is one kind by bioactive substance (such as enzyme, antibody, antigen, microorganism, cell, tissue, nucleic acid
Deng) recognition component is used as, the analysis and detection device formed with appropriate signal transducers and amplifier.With traditional detection side
Method is compared, and biology sensor has selectivity by force, the performance such as high sensitivity, good reliability, easy to operate, in clinical diagnosis, food
The numerous areas such as product safety, Pharmaceutical Analysis, Industry Control, environmental monitoring and biotechnology, biochip has wide answer
Use prospect.
Biomolecule Recognition unit is biology sensor core element, directly determines the function and quality of biology sensor.
The fixation of biomolecule primitive usually requires certain host material, and biomolecule primitive is combined as sensing with host material and applies
Layer becomes the core material of biology sensor.Therefore, the fixed form of biomolecule Recognition unit and fixed effect are biological biographies
Committed step in sensor preparation process.The process for fixation of biomolecule Recognition unit is varied, common classics immobilization
Method has：Investment, covalent bonding method, absorption method and LBL self-assembly method etc..However, these fixed forms are mainly by covalent
Or therefore molecular recognition primitive is fixed on membrane matrix surface by non-covalent fashion, molecular recognition primitive, which exists, is easy to leakage, enzyme activity
Property center be embedded, enzymatic activity be easy to loss the shortcomings of.
Polymer nano-particle has the advantages that preparation is simple, specific surface area is big, is commonly used as carrier and realizes to small molecule
The load and conveying of the function factors such as medicine.In recent years, our seminars looked for another way, and had developed a series of being based on polymer nano
Molecular engram sensor ([101776635 A of CN], [105241928 A of CN]) prepared by rice corpuscles, is realized in relative broad range
The low concentration of template molecule is detected, it is special thus to demonstrate advantage of the small size polymer nano-particle in sensitive coating field
Property.However, the molecular recognition polymer nano-particle for being concentrated mainly on electro-deposition independence of the preparation method of these sensitive coatings
On, therefore it has certain limitation in actual production.On the basis of early-stage study, we are ensureing the detection function of sensor
Property on the basis of, also more construct the more stable biography of comprehensive performance from the preparations controllability of sensitive coating and structural stability emphatically
Sensor system.At present, by a step electrophoresis codeposition by the polymer nano-particle and inorganic nano of supporting molecular Recognition unit
Conductive element modification prepares composite sensing coating in electrode surface, and the method for using it for construction biology sensor is not yet appeared in the newspapers
Road.
The content of the invention
In view of the above-mentioned problems existing in the prior art, the present invention is intended to provide a kind of will be loaded with point based on electrophoretic deposition technique
The polymer nano-particle of sub- Recognition unit is co-deposited with one step of inorganic conductive nano-particle and is prepared again in sensor electrode surface
Close sensitive coating and the method for using it for structure biology sensor.Fixed and divided as carrier using polymer nano-particle in the present invention
Sub- Recognition unit, can effectively improve the fixed amount of molecular recognition primitive；In addition, matrix material can be molecular recognition primitive
Excellent microenvironment is provided, so as to keep the activity of molecular recognition primitive for a long time.And it will be loaded and divided by a step co-electrodeposition method
The polymer nano-particle of sub- Recognition unit is deposited on electrode surface with inorganic conductive nano-particle, can be by adjusting inorganic lead
The content of nanoparticles optimizes regulation and control to the electric conductivity of sensitive coating.Prepared composite sensing coating can combine poly-
" soft " of compound nano-particle and " hard " of inorganic conductive nano material, stablizes so as to effectively improve the physical mechanical of coating
Property, sensitive coating is used to build sensor with high sensitivity, good long term stability.
Technical scheme is as follows：
A kind of method that composite sensing coating is prepared based on electrophoresis codeposition, supporting molecular Recognition unit polymer nanoparticle
The preparation of son, the preparation of mixed deposit liquid, the preparation of composite sensing coating comprise the following steps that：
(1) preparation of supporting molecular Recognition unit polymer nano-particle
Ionomer is dissolved in good solvent, obtains Ionomer solution；It is then that molecular recognition primitive is water-soluble
Liquid is added dropwise in Ionomer solution, and it is complete that 2~48h of stirring makes polymer be assembled with molecular recognition primitive；Then
Resulting solution is transferred to the dialysis of bag filter water proof to remove good solvent and unsupported molecular recognition primitive, is known up to supporting molecular
Other primitive polymer nano-particle solution.
The Ionomer is to contain polymer one or more in independent carboxyl, hydroxyl, amino group；Institute
Good solvent is stated as n,N-Dimethylformamide, dimethyl sulfoxide, dioxane, tetrahydrofuran, one or more mixed in acetonitrile
Bonding solvent；The molecular recognition primitive is one kind in enzyme, antibody, antigen, microorganism, cell, tissue, nucleic acid；The molecule
Recognition unit is supported on the inside or surface of polymer nano-particle；
(2) preparation of mixed deposit liquid
Certain density supporting molecular Recognition unit polymer nano-particle solution is prepared, adjusting pH makes its electrically charged, to
The inorganic conductive nano material that mass fraction is 0.1%~10% is wherein added, stirring makes polymer nano-particle be led with inorganic
Electric nano material is uniformly mixed, and obtains mixed deposit liquid stand for standby use；
The middle supporting molecular Recognition unit polymer nanocomposite of the supporting molecular Recognition unit polymer nano-particle solution
Particle concentration is 0.05mg/mL~10mg/mL；The inorganic conductive nano material is Nano silver grain, gold nanoparticle, platinum are received
One kind in rice corpuscles, graphene oxide, carbon nanotubes, carbon nano-fiber；The additive amount of the inorganic conductive nano material is
Mass fraction 0.01%~1.0%；The powered property in surface and polymer of inorganic conductive nano material in the mixed deposit liquid
The powered property in surface of nano-particle is consistent, to prevent component flocculating setting；
(3) preparation of composite sensing coating
Sensor electrode is immersed in step (2) the mixed deposit liquid, applies constant potential electricity using electro-deposition techniques
Pressure, makes the self-assembled nanometer particle of supporting molecular Recognition unit with inorganic nano conductive material co-deposition in electrode surface, shape
Into Organic inorganic film, natural drying at room temperature, is made composite sensing coating；
The sensor electrode is gold electrode, one kind in platinum electrode, glass-carbon electrode, ITO electrode, screen printing electrode；
The electrode needs preprocessed before use, and the method for pretreatment is：Successively with one in toluene, acetone, ethanol, deionized water
Kind or a variety of solution are ultrasonically treated 5min cleaning electrodes surface, nitrogen drying；The electrodeposition condition for deposition voltage 0.5V~
10V, sedimentation time are 2min~10min.
The present invention is beneficial to be had technical effect that：
1st, the present invention uses polymer nano-particle as carrier loaded molecular recognition primitive, polymer architecture designability
By force, effective protection to molecular recognition primitive can be realized by rational structure, so as to keep the long-term of molecular recognition primitive
Activity；In addition, polymer nano-particle has nano-scale, its big specific surface area can improve the load of molecular recognition primitive
Amount, so as to improve the molecule distinguishability of sensitive coating.
2nd, the present invention uses polymer nano-particle and the inorganic conductive nano material of small size to make to deposit liquid in electric field
Under, the not high inorganic conductive nanometer material of surface charge amount can be caused by orienting the polymer nano-particle of swimming and producing tractive force
Material is deposited on electrode base material surface at the same time, and the additive amount of inorganic conductive material is easily controllable, so as to simplify coating system
Standby mode, greatly improves the preparation efficiency of coating, it is easy to accomplish industrial mass production.
3rd, " soft " of composite sensing coating energy conjugated polymer prepared by the present invention and " hard " of inorganic conductive nano material
Property, so that the composite sensing coating prepared has similar " brick-mud " composite construction, therefore prepared composite sensing coating
Physical mechanical stability it is good so that the composite coating has longer service life in practical applications.
4th, it is of the invention by self-assembling technique, function and service coat preparing technology, electrochemical sensing technology and electrophoretic deposition skill
Art, which combines, to build diversified electrochemical copolymerization sensitive coating according to being actually needed, and then for building new chemical sensitisation
Device, is expected to be widely applied to the fields such as food security, biological medicine and environment monitoring, has extensive actual application value.
Brief description of the drawings
Fig. 1：The electrophoresis codeposition of the present invention prepares composite sensing coating process schematic diagram；
Fig. 2：The transmission electron microscope picture of HRP polymer nano-particles is loaded in the embodiment of the present invention 1；
Fig. 3：The SEM figures of composite sensing coating are made in the embodiment of the present invention 1；
Fig. 4：Chrono-amperometric response diagram of the obtained biology sensor to hydrogen peroxide in the embodiment of the present invention 1；
Embodiment
With reference to the accompanying drawings and examples, the present invention is specifically described.It should be appreciated that following embodiments are only this hair
Bright preferred embodiment, to more fully understand the present invention, thus should not be taken as limiting the scope of the invention.In the essence of the present invention
In god and scope of the claims, to any modifications and changes of the invention made, protection scope of the present invention is both fallen within
It is interior.
Embodiment 1
A kind of method that composite sensing coating is prepared based on electrophoresis codeposition, is comprised the following specific steps that：
(1) preparation of supporting molecular Recognition unit polymer nano-particle
The gamma-polyglutamic acid that Ionomer cumarin is modified is dissolved in good solvent dimethyl sulfoxide, cumarin is obtained and changes
The gamma-polyglutamic acid polymer solution of property；Then molecular recognition primitive horseradish peroxidase (HRP) aqueous solution is added dropwise
Into Ionomer solution, it is complete that stirring 12h makes polymer be assembled with molecular recognition primitive；Then resulting solution is transferred to
Bag filter water proof is dialysed to remove good solvent and unsupported molecular recognition primitive, is polymerize up to supporting molecular Recognition unit HRP
Thing nano-particle solution；TEM if figure is load HRP polymer nano-particles schemes, and as seen from the figure, gained nano-particle is
Spherical structure, its particle diameter are 100nm~200nm；
(2) preparation of mixed deposit liquid
The supporting molecular Recognition unit polymer nano-particle solution of 0.5mg/mL is prepared, adding mass fraction thereto is
0.5% silver nano-particle solution, stirring make polymer nano-particle be uniformly mixed with Nano silver grain, obtain mixed deposit liquid
Stand for standby use；
(3) preparation of composite sensing coating
Glass-carbon electrode is cleaned by ultrasonic 5min with ethanol, deionized water respectively, it is described that electrode then is immersed in step (2)
In mixed deposit liquid, apply constant potential voltage 1.5V, sedimentation time 3min using electro-deposition techniques, supporting molecular is identified base
The self-assembled nanometer particle of member is natural in electrode surface, formation Organic inorganic film, room temperature with inorganic nano-silver co-deposition
It is dry, composite sensing coating is made；Fig. 3 is that the SEM of composite sensing coating schemes, as seen from the figure, coprecipitated by a step electrophoresis
Product electrode surface form nano silver be uniformly dispersed, the composite coating of surfacing.The composite sensing coating is used to build
Hydrogen peroxide sensor is used to detect hydrogen peroxide, by Fig. 4 it can be found that with the increase of content of hydrogen peroxide, response current
Value is linearly increasing therewith, thus proves that the composite sensing coating can be used successfully to structure biology sensor.
Embodiment 2
A kind of method that composite sensing coating is prepared based on electrophoresis codeposition, is comprised the following specific steps that：
(1) preparation of supporting molecular Recognition unit polymer nano-particle
Ionomer is dissolved in good solvent n,N-Dimethylformamide, obtains poly- (acrylic acid-co- methacrylic acids
Different monooctyl ester-co- vinyl carbazoles) polymer solution；Then molecular recognition primitive lactate oxidase (LOD) aqueous solution is added dropwise
Enter into polymer solution, it is complete that stirring 2h makes polymer be assembled with molecular recognition primitive；Then resulting solution is transferred to dialysis
Bag water proof dialysis is to remove n,N-Dimethylformamide and unsupported LOD, up to the polymer of supporting molecular Recognition unit LOD
Nano-particle solution；
(2) preparation of mixed deposit liquid
The polymer nano-particle solution of the load LOD of 0.2mg/mL is prepared, it is 0.05% to add mass fraction thereto
Graphene oxide (GO) dispersion liquid, stirring polymer nano-particle is uniformly mixed with GO, obtain mixed deposit liquid standing it is standby
With；
(3) preparation of composite sensing coating
Gold electrode is cleaned by ultrasonic 5min with acetone, ethanol, deionized water respectively, electrode is then immersed in step (2)
In the mixed deposit liquid, apply constant potential voltage 3.0V using electro-deposition techniques, sedimentation time 5min, knows supporting molecular
The self-assembled nanometer particle of other primitive is with inorganic GO materials co-deposition in electrode surface, formation Organic inorganic film, room temperature
Spontaneously dry, composite sensing coating is made.
Embodiment 3
A kind of method that composite sensing coating is prepared based on electrophoresis codeposition, is comprised the following specific steps that：
(1) preparation of supporting molecular Recognition unit polymer nano-particle
The gamma-polyglutamic acid of Ionomer hydroxyethyl methacrylate-modified is dissolved in good solvent dimethyl sulfoxide, is obtained
To the gamma-polyglutamic acid polymer solution of hydroxyethyl methacrylate-modified；Then by molecular recognition primitive glucose oxidase
(GOx) aqueous solution is added dropwise in polymer solution, and it is complete that stirring 24h makes polymer be assembled with molecular recognition primitive；Then
Resulting solution is transferred to the dialysis of bag filter water proof to remove dimethyl sulfoxide and unsupported GOx, up to supporting molecular Recognition unit
The polymer nano-particle solution of GOx；
(2) preparation of mixed deposit liquid
The polymer nano-particle solution of the load GOx of 1.0mg/mL is prepared, it is 0.02% to add mass fraction thereto
Modified carbon nano-tube dispersion liquid, stirring polymer nano-particle is uniformly mixed with modified carbon nano-tube, obtain mixed deposit
Liquid stand for standby use；
(3) preparation of composite sensing coating
ITO electrode is cleaned by ultrasonic 5min with toluene, acetone, ethanol, deionized water respectively, electrode is then immersed in step
Suddenly in (2) described mixed deposit liquid, constant potential voltage 5.0V is applied using electro-deposition techniques, sedimentation time 4min, makes load
The self-assembled nanometer particle of molecular recognition primitive is with modified carbon nano tube tube material co-deposition in electrode surface, the organic-nothing of formation
Machine composite membrane, natural drying at room temperature, is made composite sensing coating.
Claims (9)
- A kind of 1. method that composite sensing coating is prepared based on electrophoresis codeposition, it is characterised in that supporting molecular Recognition unit polymerize The preparation of thing nano-particle, the preparation of mixed deposit liquid, the preparation of composite sensing coating comprise the following steps that：(1) preparation of supporting molecular Recognition unit polymer nano-particleIonomer is dissolved in good solvent, obtains Ionomer solution；Then by molecular recognition primitive aqueous solution by It is added dropwise in Ionomer solution, it is complete that stirring 2h~48h makes polymer be assembled with molecular recognition primitive；Then by institute Obtain solution and be transferred to the dialysis of bag filter water proof to remove good solvent and unsupported molecular recognition primitive, base is identified up to supporting molecular First polymer nano-particle solution；The good solvent is n,N-Dimethylformamide, dimethyl sulfoxide, dioxane, tetrahydrofuran, one kind in acetonitrile or more The mixed solvent of kind；(2) preparation of mixed deposit liquidCertain density supporting molecular Recognition unit polymer nano-particle solution is prepared, adjusting pH makes its electrically charged, thereto The inorganic conductive nano material that mass fraction is 0.1%~10% is added, stirring makes polymer nano-particle be received with inorganic conductive Rice material is uniformly mixed, and obtains mixed deposit liquid stand for standby use；The middle supporting molecular Recognition unit polymer nano-particle of the supporting molecular Recognition unit polymer nano-particle solution Concentration is 0.05mg/mL~10mg/mL；The additive amount of the inorganic conductive nano material is mass fraction 0.01%~1.0%；(3) preparation of composite sensing coatingSensor electrode is immersed in step (2) the mixed deposit liquid, applies constant potential voltage using electro-deposition techniques, makes The self-assembled nanometer particle of supporting molecular Recognition unit and inorganic nano conductive material co-deposition in electrode surface, formed with Machine-inorganic substances compound membrane, natural drying at room temperature, is made composite sensing coating.
- 2. the method according to claim 1 that composite sensing coating is prepared based on electrophoresis codeposition, it is characterised in that described Ionomer described in step (1) is to contain polymer one or more in independent carboxyl, hydroxyl, amino group.
- 3. the method according to claim 1 that composite sensing coating is prepared based on electrophoresis codeposition, it is characterised in that described Molecular recognition primitive described in step (1) is one kind in enzyme, antibody, antigen, microorganism, cell, tissue, nucleic acid.
- 4. the method according to claim 1 that composite sensing coating is prepared based on electrophoresis codeposition, it is characterised in that described Molecular recognition primitive is supported on the inside or surface of polymer nano-particle described in step (1)；Supporting molecular Recognition unit gathers The size of compound nano-particle is 20nm~1000nm.
- 5. the method according to claim 1 that composite sensing coating is prepared based on electrophoresis codeposition, it is characterised in that described Inorganic conductive nano material described in step (2) is Nano silver grain, gold nanoparticle, nano platinum particle, graphene oxide, carbon One kind in nanotube, carbon nano-fiber.
- 6. the method according to claim 1 that composite sensing coating is prepared based on electrophoresis codeposition, it is characterised in that described The powered property in surface of inorganic conductive nano material and the table of polymer nano-particle described in step (2) in mixed deposit liquid The powered property in face is consistent.
- 7. the method according to claim 1 that composite sensing coating is prepared based on electrophoresis codeposition, it is characterised in that described Sensor electrode described in step (3) is gold electrode, one kind in platinum electrode, glass-carbon electrode, ITO electrode, screen printing electrode.
- 8. the method according to claim 1 that composite sensing coating is prepared based on electrophoresis codeposition, it is characterised in that described Electrode needs preprocessed before use described in step (3), and the method for pretreatment is：Successively with toluene, acetone, ethanol, go from One or more solution in sub- water are ultrasonically treated 5min cleaning electrodes surface, nitrogen drying.
- 9. the method according to claim 1 that composite sensing coating is prepared based on electrophoresis codeposition, it is characterised in that described Electrodeposition condition described in step (3) is deposition voltage 0.5V~10V, and sedimentation time is 2min~10min.
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Cited By (1)
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| CN112080931A (en) * | 2020-08-21 | 2020-12-15 | 大连理工大学 | Method for preparing fiber pyrolytic carbon coating by utilizing electrophoretic deposition of dopamine |
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| CN105973962A (en) * | 2016-04-25 | 2016-09-28 | 陈前伟 | Preparation method of glucose sensor based on graphene nano wall |
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| CN104407140A (en) * | 2014-12-01 | 2015-03-11 | 江南大学 | Preparation method for immunosensor based on gamma-polyglutamic acid grafted dopamine and chitosan complex micelles |
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Application publication date: 20180427 |