CN108426933A - Preparation method of electrochemical working electrode and detection method of blood sugar - Google Patents
Preparation method of electrochemical working electrode and detection method of blood sugar Download PDFInfo
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- 239000008280 blood Substances 0.000 title claims abstract description 27
- 210000004369 blood Anatomy 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000001514 detection method Methods 0.000 title claims description 16
- 239000000243 solution Substances 0.000 claims abstract description 70
- 239000011521 glass Substances 0.000 claims abstract description 49
- 239000000463 material Substances 0.000 claims abstract description 25
- 229910052751 metal Inorganic materials 0.000 claims abstract description 15
- 239000002184 metal Substances 0.000 claims abstract description 15
- 239000012266 salt solution Substances 0.000 claims abstract description 14
- 239000004065 semiconductor Substances 0.000 claims abstract description 12
- 150000001412 amines Chemical class 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- 239000002086 nanomaterial Substances 0.000 claims abstract description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 84
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 46
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 24
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 20
- 239000008103 glucose Substances 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 15
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 15
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 229910021592 Copper(II) chloride Inorganic materials 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 101710134784 Agnoprotein Proteins 0.000 claims description 7
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- -1 polyethylene pyrrole Polymers 0.000 claims description 5
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 claims description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 4
- 229910000366 copper(II) sulfate Inorganic materials 0.000 claims description 4
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 3
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 229910021590 Copper(II) bromide Inorganic materials 0.000 claims description 2
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 claims description 2
- 239000000920 calcium hydroxide Substances 0.000 claims description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 150000001879 copper Chemical class 0.000 claims description 2
- QTMDXZNDVAMKGV-UHFFFAOYSA-L copper(II) bromide Substances [Cu+2].[Br-].[Br-] QTMDXZNDVAMKGV-UHFFFAOYSA-L 0.000 claims description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 2
- 125000004122 cyclic group Chemical group 0.000 claims description 2
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical compound CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 claims description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 2
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 2
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 2
- 239000011686 zinc sulphate Substances 0.000 claims description 2
- BHHGXPLMPWCGHP-UHFFFAOYSA-N Phenethylamine Chemical compound NCCC1=CC=CC=C1 BHHGXPLMPWCGHP-UHFFFAOYSA-N 0.000 claims 1
- 230000001476 alcoholic effect Effects 0.000 claims 1
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims 1
- 238000000354 decomposition reaction Methods 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 9
- 206010012601 diabetes mellitus Diseases 0.000 abstract description 5
- 201000010099 disease Diseases 0.000 abstract description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 abstract description 2
- 238000013399 early diagnosis Methods 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 239000003513 alkali Substances 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 44
- 229960002163 hydrogen peroxide Drugs 0.000 description 22
- 239000011787 zinc oxide Substances 0.000 description 22
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 20
- 239000002073 nanorod Substances 0.000 description 14
- 239000011701 zinc Substances 0.000 description 14
- 238000012360 testing method Methods 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 239000008363 phosphate buffer Substances 0.000 description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- 238000002484 cyclic voltammetry Methods 0.000 description 9
- 229910021607 Silver chloride Inorganic materials 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 238000002604 ultrasonography Methods 0.000 description 6
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Inorganic materials [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 6
- 229910052697 platinum Inorganic materials 0.000 description 5
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 3
- 239000004020 conductor Substances 0.000 description 3
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004448 titration Methods 0.000 description 3
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000000835 electrochemical detection Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 241000270722 Crocodylidae Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 206010067130 Spastic diplegia Diseases 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- VEUACKUBDLVUAC-UHFFFAOYSA-N [Na].[Ca] Chemical compound [Na].[Ca] VEUACKUBDLVUAC-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 206010008129 cerebral palsy Diseases 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- LNNWVNGFPYWNQE-GMIGKAJZSA-N desomorphine Chemical compound C1C2=CC=C(O)C3=C2[C@]24CCN(C)[C@H]1[C@@H]2CCC[C@@H]4O3 LNNWVNGFPYWNQE-GMIGKAJZSA-N 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910000397 disodium phosphate Inorganic materials 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 150000004040 pyrrolidinones Chemical class 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
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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
- G01N27/36—Glass electrodes
-
- 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
- G01N27/416—Systems
- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Conductive Materials (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The invention discloses a preparation method of an electrochemical working electrode, which comprises the following steps: cleaning ITO conductive glass, performing hydrophilic treatment, immersing the ITO conductive glass into a mixed solution of a metal salt solution and an alkali solution, taking out the ITO conductive glass, and drying the ITO conductive glass; soaking the ITO conductive glass dried in the step S1 in a mixed solution of a metal salt solution and an organic amine solution, and growing for 5-25h at 60-200 ℃, wherein a layer of semiconductor material is attached to the ITO conductive glass; and dropwise adding the conductive nano material on one surface of the ITO conductive glass on which the semiconductor nano material grows to obtain the electrochemical working electrode. The working electrode can amplify an electrochemical signal generated by lower-concentration blood sugar in the process of detecting the blood sugar, and has guiding significance for early diagnosis of diseases such as diabetes and the like in the fields of biomedicine and the like.
Description
Technical field
The present invention relates to the technical field of blood glucose Electrochemical Detection, more particularly to a kind of preparation side of electrochemical working electrode
The detection method of method and blood glucose.
Background technology
Inorganic nano material has great significance in human health and environmentally, with special physicochemical property, in addition
Big specific surface area, it is more and more extensive that high active site makes it apply, and is now chiefly used in chemical industry, biology, medicine and other fields.Peroxide
It is a kind of important molecule to change hydrogen, is the basis of clinical industry and environmental area.Many reports all give this molecule at certain
Effect in a little diseases, generated hydrogen peroxide carries out Concentration Testing and can be made into blood glucose sensing when being catalytically decomposed according to blood glucose
Device understands blood glucose normal value and is monitored in real time, according to detected value and normal value by this Technology application in blood sugar test
Comparison carry out initial stage judgement, the actual blood glucose level of body can be directly acquainted with, this for find diabetes potential danger,
The detection of diagnosis diabetes, treating diabetes effect suffers from important meaning.It is highly sensitive with the development of detection technique,
There is better foreground, the present invention to be catalyzed to hydrogen peroxide using silver wire for high accuracy, blood sugar monitoring instrument easy to operate
It decomposing, prepared blood glucose is easy to operate without enzyme sensor, and cost of manufacture is cheap, and the sensitivity and accuracy of sensor are higher,
It is with good stability.Working electrode used in electrochemical detection method for blood glucose be also it is varied, such as
ITO/Ag working electrodes, but there is these methods limitation, nano-silver thread cannot be stably adhered to ito glass on piece, it should
Method is just not suitable for.
Invention content
The purpose of the present invention is to provide a kind of preparation method of electrochemical working electrode and the detection methods of blood glucose, solve
One or more in above-mentioned prior art problem.
The present invention provides a kind of preparation method of electrochemical working electrode, includes the following steps：
α 1, ITO electro-conductive glass is cleaned up and carries out hydrophilic treated, it is molten that ITO electro-conductive glass is immersed metal salt later
In the mixed solution of liquid and aqueous slkali, dried after taking-up；
α 2, the mixed solution that the ITO electro-conductive glass dried in step S1 is immersed in metal salt solution and Amine Solutions
In, 5-25h is grown at 60-200 DEG C, is adhered on ITO electro-conductive glass and has been gone up layer of semiconductor material；
α 3, electrical-conductive nanometer droplets of material is added in the growth of ITO electro-conductive glass there is the one side of semiconductor nano material to get to institute
State electrochemical working electrode.
Wherein, ITO electro-conductive glass be on the basis of sodium calcium base or silicon boryl substrate glass, using sputtering, evaporation etc. it is more
Kind method plates indium oxide layer tin (i.e. ITO) film and manufactures.
Clear water processing refers to being put into ITO electro-conductive glass in the mixed solution of the concentrated sulfuric acid and hydrogen peroxide, its surface is made to have
Hydrophilic characteristic.
Wherein, the mixing that the ITO electro-conductive glass dried in step S1 is immersed in metal salt solution and Amine Solutions is molten
In liquid, growth temperature is preferably 80 DEG C~150 DEG C, and growth time is preferably 10h~15h.
In some embodiments, metal salt solution is Zn (NO3)2、Zn(CH3COO)2、ZnCl2、ZnSO4、Cu(NO3)2、
CuCl2、CuSO4At least one of.
In some embodiments, aqueous slkali KOH, NaOH, Ba (OH)2、Ca(OH)2At least one of.
In some embodiments, Amine Solutions are hexa, methylamine, ethamine, isopropylamine, n-butylamine, benzene
At least one of ethamine, pyridine.
In some embodiments, a concentration of 0.01M~0.1M of metal salt solution, the aqueous slkali it is a concentration of
0.01M~0.05M, a concentration of 0.01M~0.1M of the Amine Solutions, the volume ratio of the metal salt solution and aqueous slkali
It is 1:2~2:1, the volume ratio of the metal salt solution and Amine Solutions is 1:2~2:1, the drop of the electrical-conductive nanometer material
The amount added is 1 μ of μ L~10 L.Wherein, the amount of the dropwise addition of electrical-conductive nanometer material is preferably 1 μ of μ L~5 L.
In some embodiments, electrical-conductive nanometer material is nano silver wire, a diameter of 20- of the electrical-conductive nanometer material
200nm, length are 10-30 μm.Wherein, the diameter of electrical-conductive nanometer material is preferably 20-30nm, and length is preferably 20-30 μm.
In some embodiments, the preparation method of electrical-conductive nanometer material includes the following steps：
β 1, ethylene glycol solution is added in glass container, is heated to 160-170 DEG C, by the ethylene glycol solution of mantoquita and
AgNO3Ethylene glycol solution pour into glass container, wherein the ethylene glycol solution a concentration of 0.001-0.01M, AgNO of mantoquita3's
A concentration of 0.1-1M of ethylene glycol solution, the ethylene glycol solution solution and AgNO of mantoquita3Ethylene glycol solution volume ratio be 1:1-1:
10, the ethylene glycol solution of polyvinylpyrrolidone is added dropwise in subsequent constant speed；
Stop heating after β 2, completion of dropwise addition, be cooled to room temperature, solution is settled and is cleaned multiple times using acetone, centrifugation is heavy
Redisperse in ethanol, obtains the electrical-conductive nanometer material behind shallow lake.
In some embodiments, copper salt solution is Cu (NO3)2、CuSO4、CuCl2、CuI2、CuBr2At least one of.
In some embodiments, the molecular weight ranges of polyvinylpyrrolidone are 10000~1300000, polyethylene pyrrole
It is molten that polyvinylpyrrolidone is added dropwise in a concentration of 0.1-1M (in terms of polyvinylpyrrolidone monomer) of the ethylene glycol solution of pyrrolidone
Drop speed ranging from 40mL/min~60mL/min of liquid.
Wherein, the molecular weight ranges of polyvinylpyrrolidone are preferably 40000~55000.Polyvinylpyrrolidone is added dropwise
The drop speed of solution ranges preferably from 48mL/min~58mL/min.
A kind of detection method of blood glucose, includes the following steps：A kind of preparation method of above-mentioned electrochemical working electrode makes
Electrode as working electrode, the concentration of hydrogen peroxide generated decomposes blood glucose by electrochemical workstation and carries out cyclic voltammetric inspection
It surveys.
Advantageous effect：The semiconductor nano material point of the preparation method synthesis of the electrochemical working electrode of the embodiment of the present invention
Cloth is uniform, and size is uniform, there is larger specific surface area, has good biocompatibility.The conductive material nano-silver thread of synthesis
A diameter of 20-30nm, length are 70-80 μm, and elongate is presented, therefore have more active site, are a kind of biology close friend materials
Material, so the two can combine well, and the receiving that can stablize of semiconductor nano material and fixed nano-silver thread, to blood glucose
Decomposing the hydrogen peroxide generated has preferable electrochemical response signal.
The detection method of a kind of blood glucose of the embodiment of the present invention, using the electro-conductive glass ITO with semi-conducting material, at it
Working electrode of the nano-silver thread as three-electrode system is added dropwise in surface, and the concentration of hydrogen peroxide generated is decomposed to blood glucose and carries out electrification
The method for learning detection, makes semi-conducting material and nano-silver thread reach synergistic effect, can detect lower concentration of hydrogen peroxide, make
In biomaterial blood glucose detection it is more convenient, can be used as a kind of good blood glucose without enzyme sensor.
Description of the drawings
Fig. 1 is the structural schematic diagram of the electrochemical working electrode of embodiment 1；
Fig. 2 is the SEM figures of the semi-conducting material ZnO nanorod of embodiment 1；
Fig. 3 is the partial enlarged view of Fig. 2；
Fig. 4 is the SEM figures of the electrical-conductive nanometer material nano silver wire of embodiment 1；
Fig. 5 is the partial enlarged view of Fig. 4；
Fig. 6 is the cyclic voltammogram in the electro-chemical test for test 1-4
Specific implementation mode
With reference to embodiment, the invention will be further described.Following embodiment is only intended to clearly illustrate this
The performance of invention, and the following examples cannot be limited only to.
Embodiment 1：
Prepare electrical-conductive nanometer material：
It measures 50mL ethylene glycol solutions to be added in three-necked bottle, heats 1.2h at 165 DEG C, weigh 1.4mg CuCl2,
1.2740g AgNO3, it is dissolved in respectively in the ethylene glycol solution of 2.6mL and 15mL, wherein CuCl2A concentration of 0.004M, AgNO3
A concentration of 0.05M, then weigh 3.7296g molecular weight be 29000 polyvinylpyrrolidone be dissolved in 48mL ethylene glycol, wherein
A concentration of 0.7M (in terms of polyvinylpyrrolidone monomer) of the ethylene glycol solution of polyvinylpyrrolidone, by the CuCl of 2.6mL2
The AgNO of solution and 15mL3Solution pours into three-necked bottle, finally by the polyvinylpyrrolidonesolution solution of 48mL with the drop of 48mL/h
Speed is added dropwise in reaction solution, is stopped heating after titration, is cooled to room temperature, is settled using acetone, then cleaned with acetone,
Product, is finally scattered in ethyl alcohol by centrifugation.Obtained product nano silver wire passes through Figure 4 and 5 scanning electron microscope (SEM)
It can be seen that.
Weigh 21.95mg Zn (CH3COO)2·2H2O, 16.83mg KOH, are dissolved in the deionized water of 10mL respectively,
Middle Zn (CH3COO)2·2H2A concentration of 0.03M of a concentration of 0.01M of O, KOH, weigh 35.05mg hexas,
74.37mg Zn(NO3)2·6H2O is dissolved in the deionized water of 5mL respectively, wherein a concentration of 0.05M of hexa,
Zn(NO3)2·6H2A concentration of 0.05M of O.
ITO electro-conductive glass is soaked in the Zn (CH of 5mL3COO)2·2H2In O, the KOH that 5mL is slowly added dropwise in ultrasound is molten
Then liquid, ultrasound 15min again after being added dropwise place 15min in 65 DEG C of baking ovens, ITO electro-conductive glass is taken out, in 50 DEG C of baking ovens
Middle placement 5min further takes out ITO electro-conductive glass and repeats the above steps.After being repeated once, by 5mL Zn (NO3)2·6H2O solution and
5mL hexa solutions are uniformly mixed and pour into reaction kettle, then ITO electro-conductive glass is immersed in solution, make have ITO conductive
Glass one side diagonally downward, reaction kettle is placed in 120 DEG C of baking ovens and reacts 20h.ITO electro-conductive glass deionizations are taken out after 20h
2h drying is placed after water rinsed clean in 65 DEG C of baking ovens.Obtained product ZnO nanorod passes through the scanning electricity of Fig. 2 and 3
Sub- microscope (SEM) is visible.
10 μ L nano-silver threads are added dropwise on the ITO electro-conductive glass for having grown ZnO nanorod, work is prepared in hair-dryer drying
Make electrode ITO/ZnO/Ag, as shown in Figure 1, the working electrode include ITO electro-conductive glass 1, ZnO nanorod constitute semiconductor material
The conductive material layer that the bed of material 2 and nano-silver thread are constituted.
Embodiment 2：
Prepare electrical-conductive nanometer material：
It measures 50mL ethylene glycol solutions to be added in three-necked bottle, heats 1.2h at 165 DEG C, weigh 0.672mg CuCl2,
0.085g AgNO3, it is dissolved in respectively in the ethylene glycol solution of 5mL and 5mL, wherein CuCl2A concentration of 0.001M, AgNO3It is dense
Degree is 0.1M, then weighs the polyvinylpyrrolidone that 0.444g molecular weight is 10000 and be dissolved in 40mL ethylene glycol, wherein polyethylene
A concentration of 0.1M (in terms of polyvinylpyrrolidone monomer) of the ethylene glycol solution of pyrrolidones, by the CuCl of 5mL2Solution and
The AgNO of 5mL3Solution pours into three-necked bottle, finally adds the polyvinylpyrrolidonesolution solution of 40mL dropwise with the drop speed of 40mL/h
Enter into reaction solution, stop heating after titration, be cooled to room temperature, settled using acetone, then cleaned with acetone, centrifuges, most
Product is scattered in ethyl alcohol afterwards, obtained product nano silver wire.
Weigh 43.9mg Zn (CH3COO)2·2H2O, 5.611mg KOH, are dissolved in the deionized water of 10mL respectively, wherein
Zn(CH3COO)2·2H2A concentration of 0.01M of a concentration of 0.02M of O, KOH, weigh 14.02mg hexas,
29.76mg Zn(NO3)2·6H2O is dissolved in the deionized water of 10mL respectively, wherein a concentration of 0.01M of hexa,
Zn(NO3)2·6H2A concentration of 0.01M of O.
ITO electro-conductive glass is soaked in the Zn (CH of 5mL3COO)2·2H2In O, the KOH of 10mL is slowly added dropwise in ultrasound
Then solution, ultrasound 15min again after being added dropwise place 15min in 65 DEG C of baking ovens, take out ITO electro-conductive glass, are dried at 50 DEG C
5min is placed in case, is further taken out ITO electro-conductive glass and is repeated the above steps.After being repeated once, by 5mL Zn (NO3)2·6H2O solution
It is uniformly mixed and is poured into reaction kettle with 10mL hexa solutions, then ITO electro-conductive glass is immersed in solution, make have ITO
Electro-conductive glass one side diagonally downward, reaction kettle is placed in 120 DEG C of baking ovens and reacts 20h.ITO electro-conductive glass is taken out after 20h to spend
2h drying, obtained product ZnO nanorod are placed after ionized water rinsed clean in 65 DEG C of baking ovens.
1 μ L nano-silver threads are added dropwise on the ITO electro-conductive glass for having grown ZnO nanorod, work is prepared in hair-dryer drying
Electrode ITO/ZnO/Ag.
Embodiment 3：
Prepare electrical-conductive nanometer material：
It measures 50mL ethylene glycol solutions to be added in three-necked bottle, heats 4h at 170 DEG C, weigh 1.34mg CuCl2,
1.7g AgNO3, it is dissolved in respectively in the ethylene glycol solution of 1mL and 10mL, wherein CuCl2A concentration of 0.01M, AgNO3Concentration
It for 1M, then weighs the polyvinylpyrrolidone that 6.66g molecular weight is 1300000 and is dissolved in 60mL ethylene glycol, wherein polyethylene pyrrole
A concentration of 1M (in terms of polyvinylpyrrolidone monomer) of the ethylene glycol solution of pyrrolidone, by the CuCl of 1mL2Solution and 10mL's
AgNO3Solution pours into three-necked bottle, is finally added dropwise to the polyvinylpyrrolidonesolution solution of 60mL with the drop speed of 60mL/h
In reaction solution, stop heating after titration, be cooled to room temperature, settled using acetone, then cleaned with acetone, centrifuge, finally will
Product is scattered in ethyl alcohol, obtained product nano silver wire.
Weigh 219.5mg Zn (CH3COO)2·2H2O, 28.06mg KOH, are dissolved in the deionized water of 10mL respectively,
Middle Zn (CH3COO)2·2H2A concentration of 0.05M of a concentration of 0.1M of O, KOH, weigh 140.18mg hexas,
297.5mg Zn(NO3)2·6H2O is dissolved in the deionized water of 10mL respectively, wherein a concentration of 0.1M of hexa,
Zn(NO3)2·6H2A concentration of 0.1M of O.
ITO electro-conductive glass is soaked in the Zn (CH of 10mL3COO)2·2H2In O, the KOH of 5mL is slowly added dropwise in ultrasound
Then solution, ultrasound 15min again after being added dropwise place 15min in 65 DEG C of baking ovens, take out ITO electro-conductive glass, are dried at 50 DEG C
5min is placed in case, is further taken out ITO electro-conductive glass and is repeated the above steps.After being repeated once, by 10mL Zn (NO3)2·6H2O is molten
Liquid and 5mL hexa solutions, which are uniformly mixed, to be poured into reaction kettle, then ITO electro-conductive glass is immersed in solution, makes have ITO
Electro-conductive glass one side diagonally downward, reaction kettle is placed in 120 DEG C of baking ovens and reacts 20h.ITO electro-conductive glass is taken out after 20h to spend
2h drying, obtained product ZnO nanorod are placed after ionized water rinsed clean in 65 DEG C of baking ovens.
5 μ L nano-silver threads are added dropwise on the ITO electro-conductive glass for having grown ZnO nanorod, work is prepared in hair-dryer drying
Electrode ITO/ZnO/Ag.
The method for simulating blood sugar test：
Electrochemical workstation switch is opened, opening operation software pours into 20ML phosphate buffers as electrolyte, is added dropwise suitable
Hydrogenperoxide steam generator is measured, is inserted into working electrode, reference electrode respectively：Silver/silver chloride electrode, to electrode：Platinum plate electrode, by crocodile
Folder and each electrode connect, and select test pattern for cyclic voltammetry, set parameters, click starts, you can start
Test.
Prepare the phosphate buffer of 0.02M：
First prepare 0.2M, the Na of 100mL2HPO4Solution and NaH2PO4Solution：Weigh the Na of 7.1628g2HPO4·12H2O,
3.1202g NaH2PO4·2H2O is separately added into 100mL deionized waters, then measures 62mL's in above-mentioned solution respectively
Na2HPO4The NaH of solution and 38mL2PO4Solution pours into beaker, is uniformly mixed, then measure above-mentioned mixed solution 10mL and add water
It is diluted to 100mL, then weighs 0.7455gKCl and is dissolved in the phosphoric acid that can be configured to 0.02M chloride ion-containings in 100mL mixed solutions
Buffer solution.
The preparation of the hydrogenperoxide steam generator of 55mM：
After 30% hydrogenperoxide steam generator of measurement 1.42mL is diluted to 25mL, wherein 1mL solution is taken to be diluted to 10mL i.e.
It can.
Experiment 1：Naked ITO electrode detects the phosphate buffer containing 0.1mM hydrogen peroxide：
Using the naked ITO without ZnO nanorod as working electrode, the hydrogenperoxide steam generator for measuring the 55mM of 36.4 μ L is put into
In the phosphate buffer of 20mL, voltage range is -0.8V~0V, and using Ag/AgCl electrodes as reference electrode, platinum plate electrode is to electricity
Pole carries out cyclic voltammetry.Gained test result is visible by Fig. 6 cyclic voltammograms.
Experiment 2：ITO/ZnO/Ag electrode detections contain the phosphate buffer of 1mM hydrogen peroxide：
10 μ L nano-silver threads, hair-dryer drying, in this, as working electrode, amount are added dropwise on the ITO for grown ZnO nanorod
The hydrogenperoxide steam generator of the 55mM of 364 μ L is taken to be put into the phosphate buffer of 20mL, voltage range is -0.8V~0V, with Ag/
AgCl electrodes are reference electrode, and platinum plate electrode is to carry out cyclic voltammetry to electrode.Gained test result is recycled by Fig. 6 and is lied prostrate
Antu is visible.
Experiment 3：ITO/ZnO/Ag electrode detections contain the phosphate buffer of 0.5mM hydrogen peroxide：
10 μ L nano-silver threads, hair-dryer drying, in this, as working electrode, amount are added dropwise on the ITO for grown ZnO nanorod
The hydrogenperoxide steam generator of the 55mM of 182 μ L is taken to be put into the phosphate buffer of 20mL, voltage range is -0.8V~0V, with Ag/
AgCl electrodes are reference electrode, and platinum plate electrode is to carry out cyclic voltammetry to electrode.Gained test result is recycled by Fig. 6 and is lied prostrate
Antu is visible.
Experiment 4：ITO/ZnO/Ag electrode detections contain the phosphate buffer of 0.1mM hydrogen peroxide：
10 μ L nano-silver threads, hair-dryer drying, in this, as working electrode, amount are added dropwise on the ITO for grown ZnO nanorod
The hydrogenperoxide steam generator of the 55mM of 36.4 μ L is taken to be put into the phosphate buffer of 20mL, voltage range is -0.8V~0V, with Ag/
AgCl electrodes are reference electrode, and platinum plate electrode is to carry out cyclic voltammetry to electrode.Gained test result is recycled by Fig. 6 and is lied prostrate
Antu is visible.
As can be seen from Figure 6, naked ITO does not have reduction peak on cyclic voltammogram, illustrates naked ITO to peroxidating as working electrode
Hydrogen does not respond to；After hydrogen peroxide is added, ITO/ZnO/Ag electrodes are restored on cyclic voltammogram as working electrode
Peak, and as the increase of concentration of hydrogen peroxide, reduction peak are more and more obvious, illustrate ITO/ZnO/Ag electrodes as working electrode
It is very high to the sensitivity of hydrogen peroxide, it is suitble to monitor the hydrogen peroxide ingredient in blood glucose.
ZnO nanorod in embodiment provided by the invention is evenly distributed, and size is uniform, large specific surface area, in nanometer
More transmission channels are provided for nano-silver thread on scale, improve electron transfer rate, are furthermore possible to accommodate and fix well
Nano-silver thread provides larger specific surface area for it, enhances the stability of its test.Used conductive material nano-silver thread is in
Elongated threadiness has more active site, to zinc oxide nano rod and nano-silver thread can advantage combined, in detection process
In, electrochemical signals caused by the blood glucose of low concentration can be amplified, this is for the fields such as biomedicine diabetes etc.
The early diagnosis of disease has directive significance.
Presented above is only the preferred embodiment of the present invention, it is noted that those skilled in the art, not
Under the premise of being detached from the invention design, various modifications and improvements can be made, these also should be regarded as the protection of the present invention
Within the scope of.
Claims (10)
1. a kind of preparation method of electrochemical working electrode, which is characterized in that include the following steps：
α 1, ITO electro-conductive glass is cleaned up and carries out hydrophilic treated, later by ITO electro-conductive glass immerse metal salt solution and
In the mixed solution of aqueous slkali, dried after taking-up；
α 2, the ITO electro-conductive glass dried in step S1 is immersed in the mixed solution of metal salt solution and Amine Solutions,
5-25h is grown at 60-200 DEG C, is adhered on ITO electro-conductive glass and has been gone up layer of semiconductor material；
α 3, electrical-conductive nanometer droplets of material is added in the growth of ITO electro-conductive glass there is the one side of semiconductor nano material to get to the electricity
Chemical work electrode.
2. a kind of preparation method of electrochemical working electrode according to claim 1, which is characterized in that the metal salt is molten
Liquid is Zn (NO3)2、Zn(CH3COO)2、ZnCl2、ZnSO4、Cu(NO3)2、CuCl2、CuSO4At least one of.
3. a kind of preparation method of electrochemical working electrode according to claim 1, which is characterized in that the aqueous slkali is
KOH、NaOH、Ba(OH)2、Ca(OH)2At least one of.
4. a kind of preparation method of electrochemical working electrode according to claim 1, which is characterized in that the organic amine is molten
Liquid is at least one of hexa, methylamine, ethamine, isopropylamine, n-butylamine, phenyl ethylamine, pyridine.
5. a kind of preparation method of electrochemical working electrode according to claim 1, which is characterized in that the metal salt is molten
A concentration of 0.01M~0.1M of liquid, a concentration of 0.01M~0.05M of the aqueous slkali, the Amine Solutions it is a concentration of
The volume ratio of 0.01M~0.1M, the metal salt solution and aqueous slkali is 1:2~2:1, the metal salt solution and organic amine are molten
The volume ratio of liquid is 1:2~2:1, the amount of the dropwise addition of the electrical-conductive nanometer material is 1 μ of μ L~10 L.
6. a kind of preparation method of electrochemical working electrode according to claim 1, which is characterized in that the electrical-conductive nanometer
Material is nano silver wire, a diameter of 20-200nm of the electrical-conductive nanometer material, and length is 10-30 μm.
7. a kind of preparation method of electrochemical working electrode according to claim 6, which is characterized in that the electrical-conductive nanometer
The preparation method of material includes the following steps：
β 1, ethylene glycol solution is added in glass container, is heated to 160-170 DEG C, by the ethylene glycol solution and AgNO of mantoquita3
Ethylene glycol solution pour into glass container, wherein the ethylene glycol solution a concentration of 0.001-0.01M, AgNO of mantoquita3Second two
A concentration of 0.1-1M of alcoholic solution, the ethylene glycol solution solution and AgNO of mantoquita3Ethylene glycol solution volume ratio be 1:1-1:10, with
The ethylene glycol solution of polyvinylpyrrolidone is added dropwise in constant speed afterwards；
Stop heating after β 2, completion of dropwise addition, is cooled to room temperature, solution is settled and is cleaned multiple times using acetone, after centrifugation
Redisperse in ethanol, obtains the electrical-conductive nanometer material.
8. a kind of preparation method of electrochemical working electrode according to claim 7, which is characterized in that the copper salt solution
For Cu (NO3)2、CuSO4、CuCl2、CuI2、CuBr2At least one of.
9. a kind of preparation method of electrochemical working electrode according to claim 7, which is characterized in that the polyethylene pyrrole
The molecular weight ranges of pyrrolidone are 10000~1300000, a concentration of 0.1- of the ethylene glycol solution of the polyvinylpyrrolidone
Drop speed ranging from 40mL/min~60mL/min of polyvinylpyrrolidonesolution solution is added dropwise in 1M.
10. a kind of detection method of blood glucose, which is characterized in that include the following steps：By any claim in claim 1-9
The electrode that a kind of preparation method of electrochemical working electrode makes is as working electrode, by electrochemical workstation to blood
The concentration of hydrogen peroxide that sugar decomposition generates carries out cyclic voltammetric detection.
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