CN107941875A - The detection method and detecting electrode material of a kind of electrochemistry of uric acid in urine - Google Patents
The detection method and detecting electrode material of a kind of electrochemistry of uric acid in urine Download PDFInfo
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- CN107941875A CN107941875A CN201711197124.3A CN201711197124A CN107941875A CN 107941875 A CN107941875 A CN 107941875A CN 201711197124 A CN201711197124 A CN 201711197124A CN 107941875 A CN107941875 A CN 107941875A
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- LEHOTFFKMJEONL-UHFFFAOYSA-N Uric Acid Chemical compound N1C(=O)NC(=O)C2=C1NC(=O)N2 LEHOTFFKMJEONL-UHFFFAOYSA-N 0.000 title claims abstract description 46
- TVWHNULVHGKJHS-UHFFFAOYSA-N Uric acid Natural products N1C(=O)NC(=O)C2NC(=O)NC21 TVWHNULVHGKJHS-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229940116269 uric acid Drugs 0.000 title claims abstract description 46
- 239000007772 electrode material Substances 0.000 title claims abstract description 37
- 238000001514 detection method Methods 0.000 title claims abstract description 28
- 210000002700 urine Anatomy 0.000 title claims abstract description 15
- 230000005518 electrochemistry Effects 0.000 title abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 152
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 124
- 230000004048 modification Effects 0.000 claims abstract description 36
- 238000012986 modification Methods 0.000 claims abstract description 36
- 238000002360 preparation method Methods 0.000 claims abstract description 29
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000000835 electrochemical detection Methods 0.000 claims abstract description 16
- 230000003197 catalytic effect Effects 0.000 claims abstract description 14
- 125000004093 cyano group Chemical group *C#N 0.000 claims abstract description 7
- 238000004070 electrodeposition Methods 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 65
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 50
- 239000006185 dispersion Substances 0.000 claims description 41
- 239000007788 liquid Substances 0.000 claims description 26
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 23
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 21
- 239000007787 solid Substances 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 19
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000002253 acid Substances 0.000 claims description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 16
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 16
- 239000012498 ultrapure water Substances 0.000 claims description 16
- 238000000151 deposition Methods 0.000 claims description 15
- 230000008021 deposition Effects 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 15
- 235000019441 ethanol Nutrition 0.000 claims description 14
- 229910052799 carbon Inorganic materials 0.000 claims description 12
- 238000010992 reflux Methods 0.000 claims description 11
- 239000012086 standard solution Substances 0.000 claims description 10
- 238000002484 cyclic voltammetry Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims description 9
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 238000013329 compounding Methods 0.000 claims description 8
- 239000002659 electrodeposit Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 239000011780 sodium chloride Substances 0.000 claims description 8
- 229910006124 SOCl2 Inorganic materials 0.000 claims description 7
- 238000002848 electrochemical method Methods 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 239000008055 phosphate buffer solution Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 150000001721 carbon Chemical group 0.000 claims description 2
- -1 carboxy-modified graphite Alkene Chemical class 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 2
- HZBAVWLZSLOCFR-UHFFFAOYSA-N oxosilane Chemical compound [SiH2]=O HZBAVWLZSLOCFR-UHFFFAOYSA-N 0.000 claims description 2
- 238000002525 ultrasonication Methods 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 8
- 239000003054 catalyst Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 description 9
- 229960002163 hydrogen peroxide Drugs 0.000 description 8
- 238000011084 recovery Methods 0.000 description 7
- 229910002651 NO3 Inorganic materials 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 5
- 125000001731 2-cyanoethyl group Chemical group [H]C([H])(*)C([H])([H])C#N 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 4
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 3
- KDCGOANMDULRCW-UHFFFAOYSA-N 7H-purine Chemical compound N1=CNC2=NC=NC2=C1 KDCGOANMDULRCW-UHFFFAOYSA-N 0.000 description 2
- 241000283707 Capra Species 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 210000003734 kidney Anatomy 0.000 description 2
- 238000012417 linear regression Methods 0.000 description 2
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 1
- 201000005569 Gout Diseases 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002795 fluorescence method Methods 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N glycolonitrile Natural products N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 208000035474 group of disease Diseases 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 230000000640 hydroxylating effect Effects 0.000 description 1
- 230000033444 hydroxylation Effects 0.000 description 1
- 238000005805 hydroxylation reaction Methods 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000003902 lesion Effects 0.000 description 1
- 208000030159 metabolic disease Diseases 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000000451 tissue damage Effects 0.000 description 1
- 231100000827 tissue damage Toxicity 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
- 238000012795 verification Methods 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
- G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
-
- 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)
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- Electrodes For Compound Or Non-Metal Manufacture (AREA)
Abstract
The present invention relates to the detection method and detecting electrode material of a kind of electrochemistry of the uric acid in urine, belong to detection technique field.Electrochemical detection method provided by the present invention for uric acid in detection urine is mainly that make use of the surface of graphene passing through hydroxyl modification, it is set to be easier to be grafted cyano-containing group, again in its surface deposited catalyst by way of electro-deposition, the electrode material that there is preferable catalytic effect to uric acid is prepared, when the materials application detects in urine, have to uric acid and preferably detect stability, the relative standard deviation between the electrode detection result of multiple batches of preparation is smaller.
Description
Technical field
The present invention relates to the detection method and detecting electrode material of a kind of electrochemistry of the uric acid in urine, belong to detection skill
Art field.
Background technology
Uric acid height is likely to cause goat, therefore to prevent goat as the first to be appointed to an office.For universal, gout is due to purine
Metabolic disorder causes blood uric acid to increase and cause one group of disease of tissue damage, and cause is that prolonged uric acid is excessive caused,
The problems such as uric acid deposits at joint, kidney.Lesion often invades the tissue such as joint, kidney, and age of onset is more more than 40, illness rate
Increase with the age, the ratio between men and women is 50:1, most artificial post menopausal female woman of woman's venereal disease, Chang Chun, autumn morbidity.Therefore,
For the high patient of blood uric acid, should particularly pay attention to.
At present, the determination method of uric acid has fluorescence method, high performance liquid chromatography, enzyme method and electrochemical method etc..
These detection methods cut both ways, and chromatography is most basic detection method, and good separating effect, mobile phase is simple, easy to operate,
Quickly, but the sample handling processes of multistep are needed；Spectroscopic methodology is easily disturbed by other chromophories present in sample；Though enzyme method
So selectivity is good but expensive, limits its use scope；Electrochemical method have it is easy to operate, it is of low cost, it is sensitive
The features such as degree is high, and detection limit is low.
But a problem is existing for electrochemical method：The electrode of preparation is had a great influence be subject to preparation parameter, holds
Easily there is the detection performance of electrode in batch there are larger difference, influenced detection accuracy.
The content of the invention
The purpose of the present invention is：A kind of electrochemical detection method for being used to detect uric acid in urine is provided, this method is main
It is that make use of the surface of graphene passing through hydroxyl modification, allows it to be easier to be grafted cyano-containing group, then pass through electro-deposition
The electrode material for having preferable catalytic effect to uric acid is prepared in its surface deposited catalyst in mode, the materials application in
When being detected in urine, have to uric acid and preferably detect stability, the opposite mark between the electrode detection result of multiple batches of preparation
Quasi- deviation is smaller.
More specifically technical solution is：
A kind of preparation method of uric acid electrochemical detection electrode material, includes the following steps：
1st step, graphene oxide is prepared by Hummers methods；
2nd step, the reduction of graphene oxide：The graphene oxide that 1st step obtains is dispersed in water, obtains 4~8mg/mL's
Graphene oxide dispersion, takes 50~60mL graphene oxide dispersions, and 70~80wt% of 30~50 μ L is slowly added dropwise thereto
Hydrazine hydrate solution, then reacted at 85~90 DEG C, product is filtered out, is washed, it is dry after, obtain graphene；
3rd step, the acid of graphene are modified：By weight, 12~20 parts of graphene and sour 25~30 parts of mixed liquor are mixed
Close, then the heating reflux reaction under ultrasonication, the sour mixed liquor refers to by volume 3~4.5：The concentrated sulfuric acid of 1 compounding
With the mixed liquor of concentrated nitric acid, after reaction, product is filtered out, then is washed with deionized, is dry, sour carbon modified is obtained and receives
Mitron；
4th step, the acid of graphene are modified：By weight, by sour 20~25 parts of modified graphene with being modified mixed liquor 32~40
Part mixing, is warming up to 65~70 DEG C and is reacted, the modification mixed liquor is the hydrogen peroxide by the concentrated sulfuric acid and 20~30wt%
Solution mixes, and after reaction, product is filtered out, then is washed with deionized, is dry, obtains carboxy-modified graphite
Alkene；
5th step, the hydroxyl modification of graphene：By weight, by 4~8 parts carboxy-modified of graphene and 30~42 parts of SOCl2
Under the conditions of 60~65 DEG C carry out 8~12h of back flow reaction, after reaction, solids is filtered out, be redispersed in ethylene glycol 35~
In 40 parts, in 105~114 DEG C of 22~24h of back flow reaction, after reaction, solids is filtered out, is washed with deionized, does
It is dry, obtain the graphene of surface hydroxyl modification；
6th step, graphene surface it is cyanalation：By the graphene dispersion of surface hydroxyl modification in 130~140 parts of ethanol,
Add formula（I）10~15 parts shown of cyano group oxosilane modifying agent, stirring reaction, is centrifuged solids, then according to
After secondary use ethanol, water washing, the cyanalation graphene in surface is obtained；
（I）；
Wherein, R1, R2, R3 are separately selected from the straight chain containing 1~10 carbon atom or branched alkyl, more preferably
It is that R1, R2 and R3 are ethyl or isopropyl；
7th step, the preparation of modified electrode：Glass-carbon electrode is polished, is polished to minute surface, successively with ultra-pure water, absolute ethyl alcohol
After washing, dried up with nitrogen；The cyanalation graphene dispersion in surface is made into the dispersion liquid of 1~5mg/mL in ultra-pure water, will
Electrode is infiltrated in dispersion liquid, naturally dry after taking-up, is infiltrated-is dried step and be repeated 3 times, obtains modified electrode；
8th step, the deposition of surface catalytic layer：By the modified electrode of above-mentioned preparation be placed in the NaCl containing 1~3mol/L, 20~
The K of 35mmol3[Fe(CN)6], the Bi (NO of 20~25mmol3)3, 25~40mmol Ce (NO3)3Electrodeposit liquid in, with 2.0
The constant potential voltage of~3.0V is deposited, and is dried after taking-up, is obtained electrode material.
In 2nd step, the reaction time is 1~3h.
In 3rd step, the concentration of the concentrated sulfuric acid is 75~85wt%；The concentration of the concentrated sulfuric acid is 50~
60wt%；The time being heated to reflux is 2~4h.
In 4th step, the concentration of the concentrated sulfuric acid is 75~85wt%, and the reaction time is 1~4h.
In 8th step, the time of electro-deposition is 60~80s.
The electrochemical method of uric acid, includes the following steps in a kind of detection urine：
S1：Uric acid standard items are taken, are configured to the standard solution of various concentrations scope, it is molten using phosphate buffer solution adjustment criteria
The pH of liquid is in 5.0~5.5 scopes；
S2：The electrode material of above-mentioned preparation is taken, cyclic voltammetry scan is carried out by being placed in standard solution, it is big to obtain peak current
It is small；
S3：Standard curve is drawn according to peak current size and concentration of standard solution；
S4：Sample is detected, uric acid content is calculated by standard curve.
In the S2 steps, the concentration range of the standard solution of various concentrations scope is 2.0 × 10-9~6.0 × 10- 4mol/L。
In the S2 steps, the voltage range of cyclic voltammetry scan is -0.8~-0.05V.
Beneficial effect
Mainly it make use of provided by the present invention for the electrochemical detection method of uric acid in detection urine by the surface of graphene
By hydroxyl modification, its is set to be easier to be grafted cyano-containing group, then in its surface deposited catalyst by way of electro-deposition,
The electrode material that there is preferable catalytic effect to uric acid is prepared, when which detects in urine, has to uric acid
Preferable detection stability, the relative standard deviation between the electrode detection result of multiple batches of preparation are smaller.
Brief description of the drawings
Fig. 1 is the cyclic voltammetry curve when electrode material prepared in embodiment 3 carries out standard solution detection.
Fig. 2 is the standard curve of the electrode material prepared in embodiment 3.
Embodiment
In following embodiment, the step of Hummers methods prepare graphene oxide, is：1）By 1g native graphites, dense
H2SO4、H3PO4Three is placed in three-necked flask, and dense H2SO4With H3PO4Volume ratio be 9: 1, and by several times add 6g permanganic acid
Potassium, stirs 1h in ice-water bath.2）Temperature rises to 50 DEG C, insulation reaction 12h.3）Products therefrom is poured into frozen water, side stirring
Side adds appropriate hydrogen peroxide, until solution colour is changed into golden yellow, then filters, and use HCl（Volume fraction is 5%）And distillation
Product is washed till pH value close to 7 by water.Finally, gained graphite oxide is dispersed in water, ultrasonic 8h, is placed in vacuum drying chamber and does
It is dry spare.
Embodiment 1
Uric acid electrochemical detection electrode material step：
1st step, graphene oxide is prepared by Hummers methods；
2nd step, the reduction of graphene oxide：The graphene oxide that 1st step obtains is dispersed in water, obtains the oxidation of 4mg/mL
Graphene dispersing solution, takes 50mL graphene oxide dispersions, and the hydrazine hydrate solution of the 70wt% of 30 μ L is slowly added dropwise thereto, then
1h is reacted at 85 DEG C, product is filtered out, is washed, after drying, obtains graphene；
3rd step, the acid of graphene are modified：By weight, 12 parts of graphene is mixed with sour 25 parts of mixed liquor, then super
The lower heating reflux reaction 2h of sound effect, the sour mixed liquor refer to by volume 3：The 75wt% concentrated sulfuric acids and 50wt% of 1 compounding
The mixed liquor of concentrated nitric acid, after reaction, product is filtered out, then is washed with deionized, is dry, obtains sour modified carbon nano tube
Pipe；
4th step, the acid of graphene are modified：By weight, sour 20 parts of modified graphene is mixed with modified 32 parts of mixed liquor, risen
Temperature carries out reaction 1h to 65 DEG C, the modification mixed liquor be by the mixing of the hydrogenperoxide steam generator of the 75wt% concentrated sulfuric acids and 20wt% and
Into, after reaction, product is filtered out, then be washed with deionized, be dry, obtain carboxy-modified graphene；
5th step, the hydroxyl modification of graphene：By weight, by 4 parts carboxy-modified of graphene and 30 parts of SOCl2At 60 DEG C
Under the conditions of carry out back flow reaction 8h, after reaction, solids is filtered out, is redispersed in 35 parts of ethylene glycol, in 105 DEG C reflux
22h is reacted, after reaction, solids is filtered out, is washed with deionized, is dry, obtaining the graphene of surface hydroxyl modification；
6th step, graphene surface it is cyanalation：By the graphene dispersion of surface hydroxyl modification in 130 parts of ethanol, add
10 parts of (2- cyanoethyls) triethoxysilane, stirring reaction, is centrifuged solids, then successively with ethanol, water washing
Afterwards, the cyanalation graphene in surface is obtained；
7th step, the preparation of modified electrode：Glass-carbon electrode is polished, is polished to minute surface, successively with ultra-pure water, absolute ethyl alcohol
After washing, dried up with nitrogen；The cyanalation graphene dispersion in surface is made into the dispersion liquid of 1mg/mL in ultra-pure water, by electrode
It is infiltrated in dispersion liquid, naturally dry after taking-up, infiltrates-dry step and be repeated 3 times, obtain modified electrode；
8th step, the deposition of surface catalytic layer：The modified electrode of above-mentioned preparation is placed in NaCl, 20mmol containing 1mol/L
K3[Fe(CN)6], the Bi (NO of 20mmol3)3, 25mmol Ce (NO3)3Electrodeposit liquid in, with the constant potential voltage of 2.0V into
Row deposition 60s, dries after taking-up, obtains electrode material.
Embodiment 2
Uric acid electrochemical detection electrode material step：
1st step, graphene oxide is prepared by Hummers methods；
2nd step, the reduction of graphene oxide：The graphene oxide that 1st step obtains is dispersed in water, obtains the oxidation of 8mg/mL
Graphene dispersing solution, takes 60mL graphene oxide dispersions, and the hydrazine hydrate solution of the 80wt% of 50 μ L is slowly added dropwise thereto, then
3h is reacted at 90 DEG C, product is filtered out, is washed, after drying, obtains graphene；
3rd step, the acid of graphene are modified：By weight, 20 parts of graphene is mixed with sour 30 parts of mixed liquor, then super
The lower heating reflux reaction 4h of sound effect, the sour mixed liquor refer to by volume 4.5：1 compounding the 85wt% concentrated sulfuric acids and
The mixed liquor of 60wt% concentrated nitric acids, after reaction, product is filtered out, then is washed with deionized, is dry, obtains sour modification
Carbon nanotubes；
4th step, the acid of graphene are modified：By weight, sour 25 parts of modified graphene is mixed with modified 40 parts of mixed liquor, risen
Temperature carries out reaction 4h to 70 DEG C, the modification mixed liquor be by the mixing of the hydrogenperoxide steam generator of the 85wt% concentrated sulfuric acids and 30wt% and
Into, after reaction, product is filtered out, then be washed with deionized, be dry, obtain carboxy-modified graphene；
5th step, the hydroxyl modification of graphene：By weight, by 8 parts carboxy-modified of graphene and 42 parts of SOCl2At 65 DEG C
Under the conditions of carry out back flow reaction 12h, after reaction, solids is filtered out, is redispersed in 40 parts of ethylene glycol, in 114 DEG C return
Stream reaction 24h, after reaction, solids is filtered out, and is washed with deionized, is dry, obtaining the graphite of surface hydroxyl modification
Alkene；
6th step, graphene surface it is cyanalation：By the graphene dispersion of surface hydroxyl modification in 140 parts of ethanol, add
15 parts of (2- cyanoethyls) triethoxysilane, stirring reaction, is centrifuged solids, then successively with ethanol, water washing
Afterwards, the cyanalation graphene in surface is obtained；
7th step, the preparation of modified electrode：Glass-carbon electrode is polished, is polished to minute surface, successively with ultra-pure water, absolute ethyl alcohol
After washing, dried up with nitrogen；The cyanalation graphene dispersion in surface is made into the dispersion liquid of 5mg/mL in ultra-pure water, by electrode
It is infiltrated in dispersion liquid, naturally dry after taking-up, infiltrates-dry step and be repeated 3 times, obtain modified electrode；
8th step, the deposition of surface catalytic layer：The modified electrode of above-mentioned preparation is placed in NaCl, 35mmol containing 3mol/L
K3[Fe(CN)6], the Bi (NO of 25mmol3)3, 40mmol Ce (NO3)3Electrodeposit liquid in, with the constant potential voltage of 3.0V into
Row deposition 80s, dries after taking-up, obtains electrode material.
Embodiment 3
Uric acid electrochemical detection electrode material step：
1st step, graphene oxide is prepared by Hummers methods；
2nd step, the reduction of graphene oxide：The graphene oxide that 1st step obtains is dispersed in water, obtains the oxidation of 5mg/mL
Graphene dispersing solution, takes 55mL graphene oxide dispersions, and the hydrazine hydrate solution of the 75wt% of 40 μ L is slowly added dropwise thereto, then
2h is reacted at 88 DEG C, product is filtered out, is washed, after drying, obtains graphene；
3rd step, the acid of graphene are modified：By weight, 15 parts of graphene is mixed with sour 28 parts of mixed liquor, then super
The lower heating reflux reaction 3h of sound effect, the sour mixed liquor refer to by volume 4：The 80wt% concentrated sulfuric acids and 55wt% of 1 compounding
The mixed liquor of concentrated nitric acid, after reaction, product is filtered out, then is washed with deionized, is dry, obtains sour modified carbon nano tube
Pipe；
4th step, the acid of graphene are modified：By weight, sour 22 parts of modified graphene is mixed with modified 35 parts of mixed liquor, risen
Warm to 680 DEG C carry out reaction 2h, and the modification mixed liquor is mixed by the hydrogenperoxide steam generator of the 80wt% concentrated sulfuric acids and 25wt%
Form, after reaction, product is filtered out, then be washed with deionized, be dry, obtain carboxy-modified graphene；
5th step, the hydroxyl modification of graphene：By weight, by 5 parts carboxy-modified of graphene and 35 parts of SOCl2At 62 DEG C
Under the conditions of carry out back flow reaction 10h, after reaction, solids is filtered out, is redispersed in 38 parts of ethylene glycol, in 109 DEG C return
Stream reaction 23h, after reaction, solids is filtered out, and is washed with deionized, is dry, obtaining the graphite of surface hydroxyl modification
Alkene；
6th step, graphene surface it is cyanalation：By the graphene dispersion of surface hydroxyl modification in 135 parts of ethanol, add
12 parts of (2- cyanoethyls) triethoxysilane, stirring reaction, is centrifuged solids, then successively with ethanol, water washing
Afterwards, the cyanalation graphene in surface is obtained；
7th step, the preparation of modified electrode：Glass-carbon electrode is polished, is polished to minute surface, successively with ultra-pure water, absolute ethyl alcohol
After washing, dried up with nitrogen；The cyanalation graphene dispersion in surface is made into the dispersion liquid of 3mg/mL in ultra-pure water, by electrode
It is infiltrated in dispersion liquid, naturally dry after taking-up, infiltrates-dry step and be repeated 3 times, obtain modified electrode；
8th step, the deposition of surface catalytic layer：The modified electrode of above-mentioned preparation is placed in NaCl, 25mmol containing 2mol/L
K3[Fe(CN)6], the Bi (NO of 22mmol3)3, 35mmol Ce (NO3)3Electrodeposit liquid in, with the constant potential voltage of 2.5V into
Row deposition 70s, dries after taking-up, obtains electrode material.
Reference examples 1
Difference with embodiment 3 is：Cyano group modification is not carried out to the surface of graphene.
Uric acid electrochemical detection electrode material step：
1st step, graphene oxide is prepared by Hummers methods；
2nd step, the reduction of graphene oxide：The graphene oxide that 1st step obtains is dispersed in water, obtains the oxidation of 5mg/mL
Graphene dispersing solution, takes 55mL graphene oxide dispersions, and the hydrazine hydrate solution of the 75wt% of 40 μ L is slowly added dropwise thereto, then
2h is reacted at 88 DEG C, product is filtered out, is washed, after drying, obtains graphene；
3rd step, the acid of graphene are modified：By weight, 15 parts of graphene is mixed with sour 28 parts of mixed liquor, then super
The lower heating reflux reaction 3h of sound effect, the sour mixed liquor refer to by volume 4：The 80wt% concentrated sulfuric acids and 55wt% of 1 compounding
The mixed liquor of concentrated nitric acid, after reaction, product is filtered out, then is washed with deionized, is dry, obtains sour modified carbon nano tube
Pipe；
4th step, the acid of graphene are modified：By weight, sour 22 parts of modified graphene is mixed with modified 35 parts of mixed liquor, risen
Warm to 680 DEG C carry out reaction 2h, and the modification mixed liquor is mixed by the hydrogenperoxide steam generator of the 80wt% concentrated sulfuric acids and 25wt%
Form, after reaction, product is filtered out, then be washed with deionized, be dry, obtain carboxy-modified graphene；
5th step, the hydroxyl modification of graphene：By weight, by 5 parts carboxy-modified of graphene and 35 parts of SOCl2At 62 DEG C
Under the conditions of carry out back flow reaction 10h, after reaction, solids is filtered out, is redispersed in 38 parts of ethylene glycol, in 109 DEG C return
Stream reaction 23h, after reaction, solids is filtered out, and is washed with deionized, is dry, obtaining the graphite of surface hydroxyl modification
Alkene；
6th step, the preparation of modified electrode：Glass-carbon electrode is polished, is polished to minute surface, successively with ultra-pure water, absolute ethyl alcohol
After washing, dried up with nitrogen；The graphene dispersion of surface hydroxyl modification is made into the dispersion liquid of 3mg/mL in ultra-pure water, by electricity
Pole is infiltrated in dispersion liquid, naturally dry after taking-up, is infiltrated-is dried step and be repeated 3 times, obtains modified electrode；
7th step, the deposition of surface catalytic layer：The modified electrode of above-mentioned preparation is placed in NaCl, 25mmol containing 2mol/L
K3[Fe(CN)6], the Bi (NO of 22mmol3)3, 35mmol Ce (NO3)3Electrodeposit liquid in, with the constant potential voltage of 2.5V into
Row deposition 70s, dries after taking-up, obtains electrode material.
Reference examples 2
Difference with embodiment 3 is：Before cyano group modification is carried out, hydroxylating processing is not carried out to its surface.
Uric acid electrochemical detection electrode material step：
1st step, graphene oxide is prepared by Hummers methods；
2nd step, the reduction of graphene oxide：The graphene oxide that 1st step obtains is dispersed in water, obtains the oxidation of 5mg/mL
Graphene dispersing solution, takes 55mL graphene oxide dispersions, and the hydrazine hydrate solution of the 75wt% of 40 μ L is slowly added dropwise thereto, then
2h is reacted at 88 DEG C, product is filtered out, is washed, after drying, obtains graphene；
3rd step, the acid of graphene are modified：By weight, 15 parts of graphene is mixed with sour 28 parts of mixed liquor, then super
The lower heating reflux reaction 3h of sound effect, the sour mixed liquor refer to by volume 4：The 80wt% concentrated sulfuric acids and 55wt% of 1 compounding
The mixed liquor of concentrated nitric acid, after reaction, product is filtered out, then is washed with deionized, is dry, obtains sour modified carbon nano tube
Pipe；
4th step, the acid of graphene are modified：By weight, sour 22 parts of modified graphene is mixed with modified 35 parts of mixed liquor, risen
Warm to 680 DEG C carry out reaction 2h, and the modification mixed liquor is mixed by the hydrogenperoxide steam generator of the 80wt% concentrated sulfuric acids and 25wt%
Form, after reaction, product is filtered out, then be washed with deionized, be dry, obtain carboxy-modified graphene；
5th step, graphene surface it is cyanalation：By carboxy-modified graphene dispersion in 135 parts of ethanol, (2- cyanogen is added
Ethyl) 12 parts of triethoxysilane, stirring reaction, is centrifuged solids, then successively with ethanol, after water washing,
Obtain the cyanalation graphene in surface；
6th step, the preparation of modified electrode：Glass-carbon electrode is polished, is polished to minute surface, successively with ultra-pure water, absolute ethyl alcohol
After washing, dried up with nitrogen；The cyanalation graphene dispersion in surface is made into the dispersion liquid of 3mg/mL in ultra-pure water, by electrode
It is infiltrated in dispersion liquid, naturally dry after taking-up, infiltrates-dry step and be repeated 3 times, obtain modified electrode；
7th step, the deposition of surface catalytic layer：The modified electrode of above-mentioned preparation is placed in NaCl, 25mmol containing 2mol/L
K3[Fe(CN)6], the Bi (NO of 22mmol3)3, 35mmol Ce (NO3)3Electrodeposit liquid in, with the constant potential voltage of 2.5V into
Row deposition 70s, dries after taking-up, obtains electrode material.
Reference examples 3
Difference with embodiment 3 is：Bismuth nitrate is not added in the deposition of surface catalytic layer.
Uric acid electrochemical detection electrode material step：
1st step, graphene oxide is prepared by Hummers methods；
2nd step, the reduction of graphene oxide：The graphene oxide that 1st step obtains is dispersed in water, obtains the oxidation of 5mg/mL
Graphene dispersing solution, takes 55mL graphene oxide dispersions, and the hydrazine hydrate solution of the 75wt% of 40 μ L is slowly added dropwise thereto, then
2h is reacted at 88 DEG C, product is filtered out, is washed, after drying, obtains graphene；
3rd step, the acid of graphene are modified：By weight, 15 parts of graphene is mixed with sour 28 parts of mixed liquor, then super
The lower heating reflux reaction 3h of sound effect, the sour mixed liquor refer to by volume 4：The 80wt% concentrated sulfuric acids and 55wt% of 1 compounding
The mixed liquor of concentrated nitric acid, after reaction, product is filtered out, then is washed with deionized, is dry, obtains sour modified carbon nano tube
Pipe；
4th step, the acid of graphene are modified：By weight, sour 22 parts of modified graphene is mixed with modified 35 parts of mixed liquor, risen
Warm to 680 DEG C carry out reaction 2h, and the modification mixed liquor is mixed by the hydrogenperoxide steam generator of the 80wt% concentrated sulfuric acids and 25wt%
Form, after reaction, product is filtered out, then be washed with deionized, be dry, obtain carboxy-modified graphene；
5th step, the hydroxyl modification of graphene：By weight, by 5 parts carboxy-modified of graphene and 35 parts of SOCl2At 62 DEG C
Under the conditions of carry out back flow reaction 10h, after reaction, solids is filtered out, is redispersed in 38 parts of ethylene glycol, in 109 DEG C return
Stream reaction 23h, after reaction, solids is filtered out, and is washed with deionized, is dry, obtaining the graphite of surface hydroxyl modification
Alkene；
6th step, graphene surface it is cyanalation：By the graphene dispersion of surface hydroxyl modification in 135 parts of ethanol, add
12 parts of (2- cyanoethyls) triethoxysilane, stirring reaction, is centrifuged solids, then successively with ethanol, water washing
Afterwards, the cyanalation graphene in surface is obtained；
7th step, the preparation of modified electrode：Glass-carbon electrode is polished, is polished to minute surface, successively with ultra-pure water, absolute ethyl alcohol
After washing, dried up with nitrogen；The cyanalation graphene dispersion in surface is made into the dispersion liquid of 3mg/mL in ultra-pure water, by electrode
It is infiltrated in dispersion liquid, naturally dry after taking-up, infiltrates-dry step and be repeated 3 times, obtain modified electrode；
8th step, the deposition of surface catalytic layer：The modified electrode of above-mentioned preparation is placed in NaCl, 25mmol containing 2mol/L
K3[Fe(CN)6], the Ce (NO of 35mmol3)3Electrodeposit liquid in, deposition 70s is carried out with the constant potential voltage of 2.5V, after taking-up
Dry, obtain electrode material.
To the methodology validation of uric acid detection
1st, it is repeated
Prepare 1.0 × 10-6The uric acid aqueous solution of mol/L, while pH to 5.2 is adjusted with phosphate buffer solution, according to above-mentioned side
Method prepares electrode, and each embodiment and reference examples respectively prepare 6, swept with cyclic voltammetry in the range of -0.8~-0.05V
Retouch, record maximum current value, the average value and relative standard deviation of the electric current of each group are as shown in the table：
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Reference examples 1 | Reference examples 2 | Reference examples 3 | |
| Current average × 10-5A | 0.021 | 0.025 | 0.024 | 0.015 | 0.018 | 0.012 |
| Electric current relative standard deviation RSD % | 2.5 | 2.9 | 1.4 | 12.5 | 10.6 | 3.2 |
As can be seen from the above table, electrode of the invention has the repetition of preferable electrode material when carrying out Electrochemical Detection
Property, when be repeated several times experiment, the deviation of current average is small.
2nd, it is linear
The concentration range for preparing the standard solution of various concentrations scope is 1.0 × 10-8、5.0×10-6、1.0×10-5、2.0×
10-5、4.0×10-5The uric acid solution of mol/L, is respectively adopted above-mentioned electrode material and carries out cyclic voltammetry scanning, investigate dense
Degree and the linear relationship of size of current.Embodiment 3 prepare electrode it is linear as shown in Figure 2.
R squares of the regression equation and regression coefficient of each group are as follows（The unit of Y is × 10-5A）：
| Regression equation | R2 | |
| Embodiment 1 | Y=1952.1X+0.1152 | 0.9947 |
| Embodiment 2 | Y=2142.8X-0.0865 | 0.9925 |
| Embodiment 3 | Y=2536.8X+0.1069 | 0.9969 |
| Reference examples 1 | Y=3252.1X+0.1125 | 0.9234 |
| Reference examples 2 | Y=1622.3X+0.2427 | 0.9527 |
| Reference examples 3 | Y=3051.2X-0.3215 | 0.9912 |
As can be seen from the above table, electrode material provided by the invention is 1.0 × 10-8~6.0 × 10-4It is linear in the range of mol/L
Well, the material in reference examples 1 does not carry out material due to cyanomodified so that there is surface catalysis when electrode is detected
The problem of material load is uneven, linear regression coeffficient is bad；Due to not carrying out hydroxyl modification to graphene in reference examples 2, make
Cyanomodified dose bad in its surface grafting, it is bad to also result in the load of material surface catalysis material, imitates linear regression
Fruit is bad.
3rd, detection limit
Prepare 2.0 × 10-9The uric acid aqueous solution of mol/L, while pH to 5.2 is adjusted with phosphate buffer solution, according to above-mentioned side
Method prepares electrode, and each embodiment and reference examples respectively prepare 6, swept with cyclic voltammetry in the range of -0.8~-0.05V
Retouch, record maximum current value, the average value and relative standard deviation of the electric current of each group are as shown in the table：
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Reference examples 1 | Reference examples 2 | Reference examples 3 | |
| Current average × 10-8A | 0.045 | 0.049 | 0.045 | Do not detect | 0.018 | Do not detect |
| Electric current relative standard deviation RSD % | 7.5 | 8.2 | 7.2 | Do not detect | 20.4 | Do not detect |
As can be seen from the table, electrode of the invention can be detected under extremely low uric acid concentration, low with detection limit
Advantage.Due to not using cyanomodified electrode material in reference examples 1, cause its surface catalysis electrical conduction effect bad, fail to examine
Go out phase induced current；Due to not adding bismuth nitrate in reference examples 3, cause catalytic effect bad, can also make detection limit excessive.
4th, sample recovery rate
True urine specimen is taken, is separately added into 1.0 × 10-6mol/L、5.0×10-6mol/L、1.0×10-5The uric acid of mol/L,
And pH to 5.2 is adjusted with phosphate buffer solution at the same time, electrode is prepared according to the above method, each embodiment and reference examples are respectively prepared
6, be scanned with cyclic voltammetry in the range of -0.8~-0.05V, according to standard curve calculate sample recovery rate, every group
Sample recovery rate it is as follows：
1.0×10-6Sample recovery rate under mol/L concentration
| 1.0×10-6mol/L | 5.0×10-6mol/L | 1.0×10-5mol/L | |
| Embodiment 1 | 101.2% | 101.5% | 99.8% |
| Embodiment 2 | 99.2% | 98.5% | 102.1% |
| Embodiment 3 | 98.5% | 101.3 | 100.5% |
| Reference examples 1 | 47.8% | 62.2% | 67.2% |
| Reference examples 2 | 65.2% | 75.4% | 79.9% |
| Reference examples 3 | 85.6% | 81.5% | 86.2% |
As can be seen from the table, when carrying out sample recovery rate verification, the scope of the rate of recovery exists electrode material provided by the invention
In the range of 95%~105%, there is preferable detection result.Since electrode material is without cyanomodified, electronics biography in reference examples 1
Defeated and surface catalysis material load effect is bad, and it is bad to result in detection result；Due to not carrying out graphene in reference examples 2
Surface hydroxylation is modified, and can not be grafted enough cyanomodified dose, the problem of detection result is bad also occurs；Reference examples 3 by
In not adding bismuth nitrate, cause catalytic effect bad, can not detect enough uric acid in sample, it is inclined to result in sample recovery rate
It is low.
Claims (8)
1. a kind of preparation method of uric acid electrochemical detection electrode material, it is characterised in that include the following steps：
1st step, graphene oxide is prepared by Hummers methods；
2nd step, the reduction of graphene oxide：The graphene oxide that 1st step obtains is dispersed in water, obtains 4~8mg/mL's
Graphene oxide dispersion, takes 50~60mL graphene oxide dispersions, and 70~80wt% of 30~50 μ L is slowly added dropwise thereto
Hydrazine hydrate solution, then reacted at 85~90 DEG C, product is filtered out, is washed, it is dry after, obtain graphene；
3rd step, the acid of graphene are modified：By weight, 12~20 parts of graphene and sour 25~30 parts of mixed liquor are mixed
Close, then the heating reflux reaction under ultrasonication, the sour mixed liquor refers to by volume 3~4.5：The concentrated sulfuric acid of 1 compounding
With the mixed liquor of concentrated nitric acid, after reaction, product is filtered out, then is washed with deionized, is dry, sour carbon modified is obtained and receives
Mitron；
4th step, the acid of graphene are modified：By weight, by sour 20~25 parts of modified graphene with being modified mixed liquor 32~40
Part mixing, is warming up to 65~70 DEG C and is reacted, the modification mixed liquor is the hydrogen peroxide by the concentrated sulfuric acid and 20~30wt%
Solution mixes, and after reaction, product is filtered out, then is washed with deionized, is dry, obtains carboxy-modified graphite
Alkene；
5th step, the hydroxyl modification of graphene：By weight, by 4~8 parts carboxy-modified of graphene and 30~42 parts of SOCl2
Under the conditions of 60~65 DEG C carry out 8~12h of back flow reaction, after reaction, solids is filtered out, be redispersed in ethylene glycol 35~
In 40 parts, in 105~114 DEG C of 22~24h of back flow reaction, after reaction, solids is filtered out, is washed with deionized, does
It is dry, obtain the graphene of surface hydroxyl modification；
6th step, graphene surface it is cyanalation：By the graphene dispersion of surface hydroxyl modification in 130~140 parts of ethanol,
Add formula（I）10~15 parts shown of cyano group oxosilane modifying agent, stirring reaction, is centrifuged solids, then according to
After secondary use ethanol, water washing, the cyanalation graphene in surface is obtained；
（I）；
Wherein, R1, R2, R3 are separately selected from the straight chain containing 1~10 carbon atom or branched alkyl, more preferably
It is that R1, R2 and R3 are ethyl or isopropyl；
7th step, the preparation of modified electrode：Glass-carbon electrode is polished, is polished to minute surface, successively with ultra-pure water, absolute ethyl alcohol
After washing, dried up with nitrogen；The cyanalation graphene dispersion in surface is made into the dispersion liquid of 1~5mg/mL in ultra-pure water, will
Electrode is infiltrated in dispersion liquid, naturally dry after taking-up, is infiltrated-is dried step and be repeated 3 times, obtains modified electrode；
8th step, the deposition of surface catalytic layer：By the modified electrode of above-mentioned preparation be placed in the NaCl containing 1~3mol/L, 20~
The K of 35mmol3[Fe(CN)6], the Bi (NO of 20~25mmol3)3, 25~40mmol Ce (NO3)3Electrodeposit liquid in, with 2.0
The constant potential voltage of~3.0V is deposited, and is dried after taking-up, is obtained electrode material.
2. the preparation method of uric acid electrochemical detection electrode material according to claim 1, it is characterised in that described
In 2 steps, the reaction time is 1~3h.
3. the preparation method of uric acid electrochemical detection electrode material according to claim 1, it is characterised in that described
In 3 steps, the concentration of the concentrated sulfuric acid is 75~85wt%；The concentration of the concentrated sulfuric acid is 50~60wt%；It is heated to reflux
Time is 2~4h.
4. the preparation method of uric acid electrochemical detection electrode material according to claim 1, it is characterised in that described
In 4 steps, the concentration of the concentrated sulfuric acid is 75~85wt%, and the reaction time is 1~4h.
5. the preparation method of uric acid electrochemical detection electrode material according to claim 1, it is characterised in that described
In 8 steps, the time of electro-deposition is 60~80s.
6. a kind of electrochemical method for detecting uric acid in urine, it is characterised in that include the following steps：
S1：Uric acid standard items are taken, are configured to the standard solution of various concentrations scope, it is molten using phosphate buffer solution adjustment criteria
The pH of liquid is in 5.0~5.5 scopes；
S2：The electrode material of above-mentioned preparation is taken, cyclic voltammetry scan is carried out by being placed in standard solution, it is big to obtain peak current
It is small；
S3：Standard curve is drawn according to peak current size and concentration of standard solution；
S4：Sample is detected, uric acid content is calculated by standard curve.
7. the electrochemical method of uric acid in detection urine according to claim 6, it is characterised in that the S2 steps
In, the concentration range of the standard solution of various concentrations scope is 2.0 × 10-9~6.0 × 10-4mol/L。
8. the electrochemical method of uric acid in detection urine according to claim 6, it is characterised in that the S2 steps
In, the voltage range of cyclic voltammetry scan is -0.8~-0.05V.
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