CN104569093B - A kind of electrochemical detection test strip is starched and preparation method thereof and a kind of electrochemical detection test strip and preparation method thereof with carbon - Google Patents
A kind of electrochemical detection test strip is starched and preparation method thereof and a kind of electrochemical detection test strip and preparation method thereof with carbon Download PDFInfo
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- CN104569093B CN104569093B CN201510034134.XA CN201510034134A CN104569093B CN 104569093 B CN104569093 B CN 104569093B CN 201510034134 A CN201510034134 A CN 201510034134A CN 104569093 B CN104569093 B CN 104569093B
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Abstract
Starched the invention provides a kind of electrochemical detection test strip with carbon, including：10.8wt%~38.3wt% graphite, 1.8wt%~17.0wt% conductive black, 4.5wt%~7.5wt% polyester resin, 0.2wt%~5.0wt% surfactant and 45.0wt%~69.8wt% solvent.The present invention makes carbon starch to be formed in effective electronics conduction pathway, conductive black and add graphite and be conducive to black dispersion, improves electrode conductivity by the compounding of graphite and conductive black；Also, the non-porous sandwich construction of graphite can promote the generation of electrochemical reaction, the sensitivity of electrode is improved.Meanwhile, electrode prepared by carbon slurry provided by the present invention has preferable hydrophily, is uniformly spread in electrode surface beneficial to enzyme liquid, improves the reappearance of sensor.
Description
Technical field
The invention belongs to biosensor technology field, and in particular to a kind of electrochemical detection test strip is starched and its made with carbon
Preparation Method and a kind of electrochemical detection test strip and preparation method thereof.
Background technology
The analysis detection of biomolecule is to obtaining chemistry and biological information in life process, understanding biomolecule and its knot
Relation, the mechanism of elaboration vital movement and the efficient diagnosis to disease of structure and function and treatment all have highly important meaning
Justice.How efficiently, these biomolecule are enzyme rapidly and sensitively detected, is face in current life scientific domain one very heavy
The problem of wanting.The key for solving these problems is that the various new analysis and detection technologies of development.The appearance of biology sensor
Provide new instrument to efficiently solve these problems, for life science and its association area research provide it is many new
Method.
Electrochemical detection test strip be a kind of common electrochemica biological sensor, the test paper structure feature include base material,
Three electrochemical electrodes (working electrode, reference electrode and to electrode), one layer of electrochemical electrode region coating includes enzyme, polymer
The film layer of holder and pH cushions etc., when testing sample is with above-mentioned electrode contact, the electrochemical signals using its generation are true
Its fixed concentration.And carbon is starched for constituting test paper conducting wire and test paper electrode reaction area, wherein, test paper electrode reaction area refers to be measured
Electroactive chemical substance is aoxidized or reduction reaction, and pass through electricity under certain overpotential in electrode reaction area in sample
Pole reaction zone realizes electric charge transfer and forms electric current, and test paper conducting wire then provides path for signal code.Therefore, carbon slurry performance
The wettability of the chemical characteristic, especially electrode surface of direct determining electrode reaction zone.Because the current signal of sensor is defeated
Go out value and electrochemical reaction area is proportional, electrochemical reaction area is then decided by the contact surface of liquid sample and electrode reaction area
Product, and its contact area is then relevant with the wettability of electrode surface, therefore the wettability of electrode surface has to signal code
Material impact.Existing carbon slurry mainly is made up of carbon black, electron mediator and organic solvent, but starched by the carbon electrode prepared and
The wetability of enzyme liquid is poor, causes the poor reproducibility of sensor, and sensitivity is relatively low.
The content of the invention
In view of this, the technical problem to be solved in the present invention be to provide a kind of electrochemical detection test strip carbon slurry and its
Preparation method and a kind of electrochemical detection test strip, the test strips favorable reproducibility for the carbon slurry preparation that the present invention is provided, sensitivity are high.
Starched the invention provides a kind of electrochemical detection test strip with carbon, including：
10.8wt%~38.3wt% graphite,
1.8wt%~17.0wt% conductive black,
4.5wt%~7.5wt% polyester resin,
0.2wt%~5.0wt% surfactant,
45.0wt%~69.8wt% solvent.
It is preferred that, the particle diameter of the graphite is 1000~20000 mesh.
It is preferred that, the solvent is 2-Butoxyethyl acetate, butyl acetate or cyclohexanone.
It is preferred that, the polyester resin is ES850, ES100, ES110, ES550 or DYNAPOLL411.
It is preferred that, said surface activating agent is triton x-100, Qula logical X-405, polysorbate40, Tween 80 and polyethylene
One or more in pyrrolidones.
Present invention also offers the preparation method that a kind of above-mentioned electrochemical detection test strip is starched with carbon, comprise the following steps：
Graphite, conductive black, polyester resin, surfactant and solvent are mixed, grinding obtains Electrochemical Detection
Test strips are starched with carbon.
It is preferred that, mixed as follows：
Polyester resin is mixed with solvent, heated, polyester resin solution is obtained；
Surfactant is mixed with solvent, surfactant solution is obtained；
Polyester resin solution is mixed with surfactant solution, graphite and conductive black, stirring is added.
Present invention also offers a kind of electrochemical detection test strip, including：
Base material；
It is compound in the carbon slurry film layer of base material；
It is compound in the insulating lacquer layer that carbon starches film layer；
It is compound in the film layer containing enzyme of insulating lacquer layer；
The carbon slurry film layer is prepared by above-mentioned electrochemical detection test strip carbon slurry.
It is preferred that, the film layer containing enzyme is the aqueous solution containing glucose oxidase or the aqueous solution of glucose dehydrogenase
After drying into film.
Present invention also offers a kind of preparation method of above-mentioned electrochemical detection test strip, comprise the following steps：
Carbon slurry and insulated paint are coated on successively by substrate surface by silk-screen printing, then coated on dry insulated paint surface
One layer of enzyme liquid, makes siphon passage and slitting after drying, obtains electrochemical detection test strip successively.
Compared with prior art, starched the invention provides a kind of electrochemical detection test strip with carbon, including：10.8wt%~
38.3wt% graphite, 1.8wt%~17.0wt% conductive black, 4.5wt%~7.5wt% polyester resin, 0.2wt%
~5.0wt% surfactant and 45.0wt%~69.8wt% solvent.The present invention is answered by graphite and conductive black
Match somebody with somebody, carbon is starched to be formed in effective electronics conduction pathway, conductive black and is added graphite and be conducive to black dispersion, improve electrode conductance
Rate；Also, the non-porous sandwich construction of graphite can promote the generation of electrochemical reaction, the sensitivity of electrode is improved.Meanwhile, this hair
Electrode prepared by bright provided carbon slurry has preferable hydrophily, uniformly spreads, improves in electrode surface beneficial to enzyme liquid
The reappearance of sensor.
As a result show, the sensitivity for the electrochemical detection test strip that the present invention is provided is 0.28~0.30 μ A/mmol/L.This
Invention provide carbon slurry prepare electrode enzyme liquid contact angle it is smaller, illustrate the present invention provide carbon slurry and enzyme liquid compatibility more
It is good, so as to ensure that the reappearance of electrode.
Brief description of the drawings
The preparation technology flow chart for the electrochemical detection test strip that Fig. 1 provides for the present invention；
Fig. 2 is the response current and the relation of blood sugar concentration of electrochemical detection test strip prepared by embodiment 1 and comparative example 1
Figure；
Fig. 3 is the response current and the relation of blood sugar concentration of electrochemical detection test strip prepared by embodiment 2 and comparative example 2
Figure；
Fig. 4 is the response current and the relation of blood sugar concentration of electrochemical detection test strip prepared by embodiment 3 and comparative example 3
Figure.
Embodiment
Starched the invention provides a kind of electrochemical detection test strip with carbon, including：
10.8wt%~38.3wt% graphite,
1.8wt%~17.0wt% conductive black,
4.5wt%~7.5wt% polyester resin,
0.2wt%~5.0wt% surfactant,
45.0wt%~69.8wt% solvent.
The electrochemical detection test strip that the present invention is provided includes conductive black with carbon slurry, wherein, conductive black is starched as carbon
Effective conductive compositions, it is ensured that the excellent conductance of carbon electrode.In the present invention, the addition of the conductive black is
1.8wt%~17.0wt%, preferably 2wt%~15wt%, more preferably 5wt%~10wt%.
The electrochemical detection test strip that the present invention is provided is starched with carbon also includes graphite, in the present invention, the conductive black
In must add a certain proportion of graphite, could so form effective electronics conduction pathway, wherein, the graphite is equivalent to electricity
Node in subchannel network.Graphite is added in conductive black and is conducive to the scattered of conductive black, conductive black is unlikely to reunite
And reduce electrical conductivity.Also, graphite is due to non-porous, sandwich construction, active as that can turn into electro transfer during electrode material
Point, it is beneficial to the electroactive material reacted on its surface that electro transfer to electrode/be transferred to electronics from electrode is electroactive
Material, promotes the generation of electrochemical reaction, improves the sensitivity of electrode.The addition of the graphite be 10.8wt%~
38.3wt%, preferably 12wt%~35wt%, more preferably 20wt%~30wt%.In addition, the different-grain diameter of graphite can be made
Into the different electrochemical properties of carbon electrode, when graphite particle diameter is larger, such as larger than 1000 mesh can substantially reduce the electrification of carbon electrode
Response sensitivity is learned, when particle diameter is too small, such as less than 20000 mesh can not then form effective conductive network together with conductive black
And the conductance of carbon electrode is reduced, therefore, the particle size range of graphite is the mesh of 1000 mesh~20000, preferably 5000 mesh~
The mesh of 15000 mesh, more preferably 7000 mesh~12000.
Carbon slurry provided by the present invention needs to be attached on the base materials such as PVC or PET when in use, and polyester resin is carbon black and stone
The dispersant and binding agent of ink, are fixed on test paper base material, it is ensured that carbon starches the adhesive force on base material, and forms one
Fixed figure.In the present invention, the polyester resin is preferably ES850, ES100, ES110, ES550 or DYNAPOL L411,
More preferably the trade mark of SK companies is ES550 polyester resin, and the addition of the polyester resin is 4.5wt%~7.5wt%,
Preferably 5wt%~7wt%, more preferably 5.5wt%~6.5wt%.
Carbon slurry of the present invention also includes surfactant, and the surfactant is preferably triton x-100, Qula
One or more in logical X-405, polysorbate40, Tween 80 and polyvinylpyrrolidone, more preferably triton x-100, tween
40 or polyvinylpyrrolidone.Wherein, the addition of the surfactant is 0.2wt%~5.0wt%, is preferably
0.5wt%~4.5wt%, more preferably 2wt%~4wt%.
The electrochemical detection test strip that the present invention is provided is starched with carbon also includes solvent, to prevent solvent volatilization is too fast from causing carbon
Premature solidification is starched, and ensures that carbon slurry can be dried effectively in 100~150 DEG C of baking oven, need to be from boiling point 200~300
DEG C organic solvent, preferably esters high boiling solvent, more preferably 2-Butoxyethyl acetate, butyl acetate
Or cyclohexanone.The addition of the solvent is 45.0wt%~69.8wt%, preferably 50wt%~65wt%, is more preferably
55wt%~60wt%.
Present invention also offers the preparation method that a kind of above-mentioned electrochemical detection test strip is starched with carbon, comprise the following steps：
Graphite, conductive black, polyester resin, surfactant and solvent are mixed, grinding obtains Electrochemical Detection
Test strips are starched with carbon.
The present invention is not specifically limited to the method for the mixing, and mixing is preferably carried out as follows and is stirred
Mix：
Polyester resin is mixed with solvent, heated, polyester resin solution is obtained；
Surfactant is mixed with solvent, surfactant solution is obtained；
Polyester resin solution is mixed with surfactant solution, graphite and conductive black, stirring is added.
Wherein, polyester resin is mixed with solvent, heated, wherein the temperature of the heating is preferably 70~90 DEG C, more preferably
For 80 DEG C.Polyester resin solution is mixed with surfactant solution, the speed that addition graphite and conductive black are stirred is
3000~5000rpm, the time of stirring is 3~5h.
Present invention also offers a kind of electrochemical detection test strip, including：
Base material；
It is compound in the carbon slurry film layer of base material；
It is compound in the insulating lacquer layer that carbon starches film layer；
It is compound in the film layer containing enzyme of insulating lacquer layer；
The carbon slurry film layer is prepared by above-mentioned electrochemical detection test strip carbon slurry.
Electrochemical detection test strip provided by the present invention includes base material, and the base material is preferably PET base material or PVC bases
Material.
The electrochemical detection test strip also includes being starched with carbon by electrochemical detection test strip provided by the present invention preparing
Obtained carbon slurry film layer.
Wherein, the electrochemical detection test strip carbon slurry includes：
10.8wt%~38.3wt% graphite,
1.8wt%~17.0wt% conductive black,
4.5wt%~7.5wt% polyester resin,
0.2wt%~5.0wt% surfactant,
45.0wt%~69.8wt% solvent.
In the present invention, the addition of the conductive black be 1.8wt%~17.0wt%, preferably 2wt%~
15wt%, more preferably 5wt%~10wt%.The addition of the graphite is 10.8wt%~38.3wt%, is preferably
12wt%~35wt%, more preferably 20wt%~30wt%.The particle size range of the graphite is the mesh of 1000 mesh~20000, excellent
Elect the mesh of 5000 mesh~15000 as, the mesh of more preferably 7000 mesh~12000.The polyester resin be preferably ES850, ES100,
ES110, ES550 or DYNAPOLL411；More preferably the trade mark of SK companies is ES550 polyester resin, the polyester resin
Addition is 4.5wt%~7.5wt%, more preferably preferably 5wt%~7wt%, 5.5wt%~6.5wt%.The surface
Activating agent is preferably one kind or many in triton x-100, Qula logical X-405, polysorbate40, Tween 80 and polyvinylpyrrolidone
Plant, more preferably triton x-100, polysorbate40 or polyvinylpyrrolidone.Wherein, the addition of the surfactant is
0.2wt%~5.0wt%, preferably 0.5wt%~4.5wt%, more preferably 2wt%~4wt%.The solvent need to be from boiling
O'clock in 200~300 DEG C of organic solvent, preferably esters or ketone high boiling solvent, more preferably 2-Butoxyethyl acetate,
Butyl acetate or cyclohexanone.The addition of the solvent is 45.0wt%~69.8wt%, preferably 50wt%
~65wt%, more preferably 55wt%~60wt%.
The test paper also includes insulating lacquer layer, and the present invention is not specifically limited to the species of the insulated paint and source,
It is commercially available.
After the film layer containing enzyme is the aqueous solution containing glucose oxidase or the drying of the aqueous solution of glucose dehydrogenase
Into film.
Present invention also offers a kind of preparation method of above-mentioned electrochemical detection test strip, comprise the following steps：
Carbon slurry and insulated paint are coated on successively by substrate surface by silk-screen printing, then coated on dry insulated paint surface
One layer of enzyme liquid, makes siphon passage and slitting after drying, obtains electrochemical detection test strip successively.
Electrochemical detection test strip provided by the present invention uses disposable test strip manufacture craft, and technological process is shown in
The preparation technology flow chart for the electrochemical detection test strip that Fig. 1, Fig. 1 provide for the present invention.Specifically, using be screen printed onto through
The PET or PVC base surface carbon coating slurry of pretreatment are crossed, carbon electrode is obtained after drying, using being screen printed onto carbon electrodes
Insulated paint is coated, in insulated paint surface printing or drop coating enzyme liquid after drying, siphon passage is made after drying and is cut, after packaging
To electrochemical detection test strip.
The present invention makes carbon starch to form effective electronics conduction pathway, conductive black by the compounding of graphite and conductive black
Middle addition graphite is conducive to black dispersion, improves electrode conductivity；Also, the non-porous sandwich construction of graphite can promote electrochemistry
The generation of reaction, improves the sensitivity of electrode.Meanwhile, electrode prepared by carbon slurry provided by the present invention has preferably hydrophilic
Property, uniformly spread in electrode surface beneficial to enzyme liquid, improve the reappearance of sensor.
As a result show, the sensitivity for the electrochemical detection test strip that the present invention is provided is 0.28~0.30 μ A/mmol/L.This
Invention provide carbon slurry prepare electrode enzyme liquid contact angle it is smaller, illustrate the present invention provide carbon slurry and enzyme liquid compatibility more
It is good, so as to ensure that the reappearance of electrode.
For a further understanding of the present invention, the electrochemical detection test strip carbon provided with reference to embodiment the present invention
Slurry and preparation method thereof and electrochemical detection test strip and preparation method thereof are illustrated, and protection scope of the present invention is not by following
The limitation of embodiment.
Embodiment 1
1st, in three-necked flask, 2-Butoxyethyl acetate and polyester resin are added in the following proportions, 80 DEG C are heated to, fully
Stirring mixing, obtains the mixed liquor that resin is completely dissolved, and is transferred to container cooling stand-by；
2-Butoxyethyl acetate 70wt%；
Polyester resin 30wt%.
2nd, according to the form below adds the surfactant and 2-Butoxyethyl acetate of fixed proportion, stirring in stainless steel iron flask
It is uniformly dispersed, set aside for use；
3rd, resin mixture liquor according to the form below ratio prepared by step 1 is added in mixed liquor prepared by step 2, pressed simultaneously
Table adds the carbon black and graphite of fixed proportion, and high-speed stirred is scattered 3 hours, is transferred in grinder and grinds 2 times, electricity is finally made
Chemical detection test strips are starched with carbon.
| Component | Ratio/wt% |
| Conductive carbon black | 4.3 |
| 2000 mesh graphite | 38.3 |
| ES-100 resin mixture liquors | 25.0 |
| 2-Butoxyethyl acetate | 27.5 |
| Triton x-100 | 5.0 |
4th, by being screen printed onto the electrochemical detection test strip that the PVC base surface coating step 3 of cleaning is prepared
Starched with carbon, carbon electrode is obtained after drying.Insulated paint is coated by being screen printed onto carbon electrodes, in dry insulation after drying
The aqueous solution containing glucose oxidase that surface drop coating mass concentration is 5 ‰ is painted, after drying, is made in thin-film surface containing enzyme
Electrochemical detection test strip is obtained after siphon passage, slitting.
Comparative example 1
1st, the carbon slurry using the trade mark of ten chemical company's production of Japan as CH-10 is used as electrochemical detection test strip carbon
Slurry.
2nd, starched, dried with carbon by being screen printed onto the PVC base surface above-mentioned electrochemical detection test strip of coating of cleaning
After obtain carbon electrode.Insulated paint is coated by being screen printed onto carbon electrodes, in dry insulated paint surface drop coating after drying
Mass concentration is 5 ‰ aqueous solution containing glucose oxidase, after drying, and siphon passage is made in thin-film surface containing enzyme,
Electrochemical detection test strip is obtained after slitting.
3rd, the performance of electrochemical detection test strip is determined：
(1) sensitivity test：
The electrochemical detection test strip that embodiment 1 and comparative example 1 are obtained tests skill on electrochemical workstation using i-t
Art, test condition is to maintain electrode pressure difference 0.2V, and sensed current signal is changed over time, and takes 20S current values conduct after sample introduction
Balanced balanced current, balanced balanced current of the strip of embodiment 1 under different blood sugar concentrations, meet with a response electric current and blood sugar concentration curve, knot
Fruit sees the response current and the relation of blood sugar concentration that Fig. 2, Fig. 2 are electrochemical detection test strip prepared by embodiment 1 and comparative example 1
Figure, wherein, in Fig. 2,1 is response current and the blood sugar concentration relation of electrochemical detection test strip prepared by embodiment 1,2 for pair
The response current of electrochemical detection test strip prepared by ratio 1 and blood sugar concentration relation.
The sensitivity for calculating embodiment 1 is 0.28 μ A/mmol/L, and comparative example 1 is 0.22 μ A/mmol/L, it can be seen that made
Sensitivity of the Electrochemical Detection strip obtained with embodiment 1 to glucose solution is high compared with the test strips of comparative example 1 by 24%.
(2) carbon slurry and the compatibility of enzyme liquid：
It is spread condition of the test enzyme liquid in electrode surface, after completion silk-screen printing obtains carbon electrode, respectively in implementation
The electrode surface of example 1 and comparative example 1 carries out enzyme liquid contact angle test, and testing time is 4 times, and numbering is respectively 1~4.As a result see
Table 1, table 1 is embodiment 1 and the enzyme liquid contact angle test result of the electrode surface of comparative example 1.
The embodiment 1 of table 1 and the enzyme liquid contact angle test result of the electrode surface of comparative example 1
| Numbering | Embodiment 1 | Comparative example 1 |
| 1 | 13.7 | 106.0 |
| 2 | 17.0 | 110.8 |
| 3 | 10.2 | 109.8 |
| 4 | 18.0 | 112.2 |
The enzyme liquid contact angle of embodiment 1 is less than comparative example 1 as can be seen from Table 1, and enzyme liquid is easier in experimental group strip
Diffusion into the surface, illustrates that carbon slurry of the present invention and the compatibility of enzyme liquid are more preferable.
Embodiment 2
1st, in three-necked flask, 2-Butoxyethyl acetate and polyester resin are added in the following proportions, 80 DEG C are heated to, fully
Stirring mixing, obtains the mixed liquor that resin is completely dissolved, and is transferred to container cooling stand-by；
2-Butoxyethyl acetate 60wt%；
Polyester resin 40wt%.
2nd, according to the form below adds the surfactant and 2-Butoxyethyl acetate of fixed proportion, stirring in stainless steel iron flask
It is uniformly dispersed, set aside for use.
3rd, resin mixture liquor according to the form below ratio prepared by step 1 is added in mixed liquor prepared by step 2, pressed simultaneously
Table adds the carbon black and graphite of fixed proportion, and high-speed stirred is scattered 3 hours, is transferred in grinder and grinds 2 times, electricity is finally made
Chemical detection test strips are starched with carbon.
4th, by being screen printed onto the electrochemical detection test strip that the PVC base surface coating step 3 of cleaning is prepared
Starched with carbon, carbon electrode is obtained after drying.Insulated paint is coated by being screen printed onto carbon electrodes, in dry insulation after drying
The aqueous solution containing glucose dehydrogenase that surface drop coating mass concentration is 3 ‰ is painted, after drying, is made in thin-film surface containing enzyme
Electrochemical detection test strip is obtained after siphon passage, slitting.
Comparative example 2
1st, the carbon slurry using the trade mark of ten chemical company's production of Japan as CH-10 is used as electrochemical detection test strip carbon
Slurry.
2nd, starched, dried with carbon by being screen printed onto the PVC base surface above-mentioned electrochemical detection test strip of coating of cleaning
After obtain carbon electrode.Insulated paint is coated by being screen printed onto carbon electrodes, in dry insulated paint surface drop coating after drying
Mass concentration is 3 ‰ aqueous solution containing glucose dehydrogenase, after drying, and siphon passage is made in thin-film surface containing enzyme,
Electrochemical detection test strip is obtained after slitting.
3rd, the performance of electrochemical detection test strip is determined：
(1) sensitivity test：
The electrochemical detection test strip that embodiment 2 and comparative example 2 are obtained tests skill on electrochemical workstation using i-t
Art, test condition is to maintain electrode pressure difference 0.2V, and sensed current signal is changed over time, and takes 20S current values conduct after sample introduction
Balanced balanced current, balanced balanced current of the strip of embodiment 2 under different blood sugar concentrations, meet with a response electric current and blood sugar concentration curve, knot
Fruit sees the response current and the relation of blood sugar concentration that Fig. 3, Fig. 3 are electrochemical detection test strip prepared by embodiment 2 and comparative example 2
Figure, wherein, in Fig. 3,1 is response current and the blood sugar concentration relation of electrochemical detection test strip prepared by embodiment 2,2 for pair
The response current of electrochemical detection test strip prepared by ratio 2 and blood sugar concentration relation.
The sensitivity for calculating embodiment 2 is 0.28 μ A/mmol/L, and comparative example 2 is 0.23 μ A/mmol/L, it can be seen that made
Sensitivity of the Electrochemical Detection strip obtained with embodiment 2 to glucose solution is high compared with the test strips of comparative example 2 by 20%.
(2) carbon slurry and the compatibility of enzyme liquid：
It is spread condition of the test enzyme liquid in electrode surface, after completion silk-screen printing obtains carbon electrode, respectively in implementation
The electrode surface of example 2 and comparative example 2 carries out enzyme liquid contact angle test, and testing time is 4 times, and numbering is respectively 1~4.As a result see
Table 2, table 2 is embodiment 2 and the enzyme liquid contact angle test result of the electrode surface of comparative example 2.
The embodiment 2 of table 2 and the enzyme liquid contact angle test result of the electrode surface of comparative example 2
| Numbering | Embodiment 2 | Comparative example 2 |
| 1 | 9.0 | 106.4 |
| 2 | 12.8 | 109.4 |
| 3 | 12.4 | 110.4 |
| 4 | 19.3 | 113.4 |
The enzyme liquid contact angle of embodiment 2 is less than comparative example 2 as can be seen from Table 2, and enzyme liquid is easier in the strip of embodiment 2
Diffusion into the surface, illustrates that carbon slurry of the present invention and the compatibility of enzyme liquid are more preferable.
Embodiment 3
1st, in three-necked flask, 2-Butoxyethyl acetate and polyester resin are added in the following proportions, 80 DEG C are heated to, fully
Stirring mixing, obtains the mixed liquor that resin is completely dissolved, and is transferred to container cooling stand-by；
2-Butoxyethyl acetate 65wt%；
Polyester resin 35wt%.
2nd, according to the form below adds the surfactant and 2-Butoxyethyl acetate of fixed proportion, stirring in stainless steel iron flask
It is uniformly dispersed, set aside for use；
3rd, resin mixture liquor according to the form below ratio prepared by step 1 is added in mixed liquor prepared by step 2, pressed simultaneously
Table adds the carbon black and graphite of fixed proportion, and high-speed stirred is scattered 3 hours, is transferred in grinder and grinds 2 times, electricity is finally made
Chemical detection test strips are starched with carbon；
| Component | Ratio/wt% |
| Conductive carbon black | 6 |
| 10000 mesh graphite | 35.5 |
| ES-550 resin mixture liquors | 20 |
| 2-Butoxyethyl acetate | 38.5 |
| Polyvinylpyrrolidone | 3 |
4th, by being screen printed onto the electrochemical detection test strip that the PVC base surface coating step 3 of cleaning is prepared
Starched with carbon, carbon electrode is obtained after drying.Insulated paint is coated by being screen printed onto carbon electrodes, in dry insulation after drying
The aqueous solution containing glucose dehydrogenase that surface drop coating mass concentration is 1 ‰ is painted, after drying, is made in thin-film surface containing enzyme
Electrochemical detection test strip is obtained after siphon passage, slitting.
Comparative example 3
1st, the carbon slurry using the trade mark of ten chemical company's production of Japan as CH-10 is used as electrochemical detection test strip carbon
Slurry.
2nd, starched, dried with carbon by being screen printed onto the PVC base surface above-mentioned electrochemical detection test strip of coating of cleaning
After obtain carbon electrode.Insulated paint is coated by being screen printed onto carbon electrodes, in dry insulated paint surface drop coating after drying
Mass concentration is 1 ‰ aqueous solution containing glucose dehydrogenase, after drying, and siphon passage is made in thin-film surface containing enzyme,
Electrochemical detection test strip is obtained after slitting.
3rd, the performance of electrochemical detection test strip is determined：
(1) sensitivity test：
The electrochemical detection test strip that embodiment 3 and comparative example 3 are obtained tests skill on electrochemical workstation using i-t
Art, test condition is to maintain electrode pressure difference 0.2V, and sensed current signal is changed over time, and takes 20S current values conduct after sample introduction
Balanced balanced current, balanced balanced current of the strip of embodiment 3 under different blood sugar concentrations, meet with a response electric current and blood sugar concentration curve, knot
Fruit sees the response current and the relation of blood sugar concentration that Fig. 4, Fig. 4 are electrochemical detection test strip prepared by embodiment 3 and comparative example 3
Figure, wherein, in Fig. 4,1 is response current and the blood sugar concentration relation of electrochemical detection test strip prepared by embodiment 3,2 for pair
The response current of electrochemical detection test strip prepared by ratio 3 and blood sugar concentration relation.
The sensitivity for calculating embodiment 3 is 0.30 μ A/mmol/L, and comparative example 3 is 0.24 μ A/mmol/L, it can be seen that made
The Electrochemical Detection strip that the embodiment 3 starched with carbon of the present invention is obtained is high compared with the strip of comparative example 3 to the sensitivity of glucose solution
22%.
(2) carbon slurry and the compatibility of enzyme liquid：
It is spread condition of the test enzyme liquid in electrode surface, after completion silk-screen printing obtains carbon electrode, respectively in implementation
The electrode surface of example 3 and comparative example 3 carries out enzyme liquid contact angle test, and testing time is 4 times, and numbering is respectively 1~4.As a result see
Table 3, table 3 is embodiment 3 and the enzyme liquid contact angle test result of the electrode surface of comparative example 3.
The embodiment 3 of table 3 and the enzyme liquid contact angle test result of the electrode surface of comparative example 3
| Numbering | Embodiment 3 | Comparative example 3 |
| 1 | 13.2 | 116.1 |
| 2 | 12.3 | 100.5 |
| 3 | 10.6 | 112.1 |
| 4 | 17.5 | 107.6 |
The enzyme liquid contact angle of embodiment 3 is less than comparative example 3 as can be seen from Table 3, and enzyme liquid is easier in the strip of embodiment 3
Diffusion into the surface, illustrates that carbon slurry of the present invention and the compatibility of enzyme liquid are more preferable.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of electrochemical detection test strip is starched with carbon, it is characterised in that including：
10.8wt%~38.3wt% graphite,
1.8wt%~17.0wt% conductive black,
4.5wt%~7.5wt% polyester resin,
0.2wt%~5.0wt% surfactant, the surfactant is selected from triton x-100, Qula and leads to X-405, tells
One or more in temperature 40, Tween 80 and polyvinylpyrrolidone；
45.0wt%~69.8wt% solvent.
2. carbon slurry according to claim 1, it is characterised in that the particle diameter of the graphite is 1000~20000 mesh.
3. carbon slurry according to claim 1, it is characterised in that the solvent is 2-Butoxyethyl acetate or diethylene glycol
Monobutyl ether acetate or cyclohexanone.
4. carbon according to claim 1 slurry, it is characterised in that the polyester resin be ES850, ES100, ES110,
ES550 or DYNAPOL L411.
5. the preparation method that a kind of electrochemical detection test strip as claimed in claim 1 is starched with carbon, it is characterised in that including with
Lower step：
Graphite, conductive black, polyester resin, surfactant and solvent are mixed, grinding obtains Electrochemical Detection test paper
Bar is starched with carbon.
6. preparation method according to claim 5, it is characterised in that mixed as follows：
Polyester resin is mixed with solvent, heated, polyester resin solution is obtained；
Surfactant is mixed with solvent, surfactant solution is obtained；
Polyester resin solution is mixed with surfactant solution, graphite and conductive black, stirring is added.
7. a kind of electrochemical detection test strip, it is characterised in that including：
Base material；
It is compound in the carbon slurry film layer of base material；
It is compound in the insulating lacquer layer that carbon starches film layer；
It is compound in the film layer containing enzyme of insulating lacquer layer；
The carbon slurry film layer is prepared by electrochemical detection test strip carbon as claimed in claim 1 slurry.
8. electrochemical detection test strip according to claim 7, it is characterised in that the film layer containing enzyme is to contain grape
The aqueous solution of carbohydrate oxidase or the aqueous solution of glucose dehydrogenase dry after into film.
9. a kind of preparation method of electrochemical detection test strip as claimed in claim 7, it is characterised in that including following step
Suddenly：
Carbon slurry and insulated paint are coated on successively by substrate surface by silk-screen printing, then one layer is coated on dry insulated paint surface
Enzyme liquid, makes siphon passage and slitting after drying, obtains electrochemical detection test strip successively.
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| CN105355530B (en) * | 2015-10-30 | 2017-08-11 | 三诺生物传感股份有限公司 | A kind of plasma treatment appts pre-processed for test strip electrode and method |
| CN108362753B (en) * | 2017-12-11 | 2023-09-12 | 南京晓庄学院 | Trace heavy metal detection system and detection method based on chronopotentiometric dissolution method |
| CN109884142A (en) * | 2019-03-08 | 2019-06-14 | 武汉璟泓万方堂医药科技股份有限公司 | A kind of test strip for blood-sugar containing decorating liquid |
| CN110763743A (en) * | 2019-11-06 | 2020-02-07 | 广州万孚生物技术股份有限公司 | Electrochemical detection test paper for triglyceride, preparation method and application thereof, and detection sensor comprising electrochemical detection test paper |
| CN111809447B (en) * | 2020-05-06 | 2023-04-18 | 安吉远耕科技有限公司 | Conductive paper and preparation method and application thereof |
| CN112164489B (en) * | 2020-09-04 | 2022-04-19 | 苏州烯时代材料科技有限公司 | Conductive carbon paste for blood glucose test paper, preparation method thereof and blood glucose test paper |
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| JPS58134163A (en) * | 1982-02-05 | 1983-08-10 | Mitsui Toatsu Chem Inc | Carbon paste and cured material thereof |
| CN101825603A (en) * | 2010-04-17 | 2010-09-08 | 上海交通大学 | Current enzyme electrode for detecting catalase-positive bacteria and preparation method thereof |
| CN202066830U (en) * | 2011-01-25 | 2011-12-07 | 北京师范大学 | Screen printing electrode enzyme sensor capable of quickly detecting organic phosphorous pesticides |
| CN103175872A (en) * | 2011-12-23 | 2013-06-26 | 长沙中生众捷生物技术有限公司 | Portable electrochemical detection test strip and preparation method thereof |
| CN102969076B (en) * | 2012-11-13 | 2015-04-15 | 苏州喜仁新材料科技有限公司 | High-performance superconductivity carbon paste and preparation method thereof |
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| CN104952510B (en) * | 2015-06-10 | 2017-03-29 | 浙江大学 | A kind of electrode slurry and the method detected in sample surfaces Direct Electrochemistry with which |
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