CN108344785A - A kind of preparation method for the composite material modified electrode can be used for detecting ascorbic acid, dopamine and uric acid simultaneously - Google Patents
A kind of preparation method for the composite material modified electrode can be used for detecting ascorbic acid, dopamine and uric acid simultaneously Download PDFInfo
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- CN108344785A CN108344785A CN201810063091.1A CN201810063091A CN108344785A CN 108344785 A CN108344785 A CN 108344785A CN 201810063091 A CN201810063091 A CN 201810063091A CN 108344785 A CN108344785 A CN 108344785A
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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
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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
- G01N27/416—Systems
Abstract
The present invention relates to a kind of preparation methods for the composite material modified electrode can be used for detecting ascorbic acid, dopamine and uric acid simultaneously.Include the following steps：It is detected while the preparation of porous carbon ball, the preparation of zinc oxide copper/porous carbon ball composite material, the preparation of zinc oxide copper/porous carbon ball composite material modified electrode, composite material modified electrode Ascorbic Acid, dopamine and uric acid.The beneficial effects of the invention are as follows this zinc oxide copper/porous carbon ball composite materials to have excellent electric conductivity and preferable catalytic activity, ascorbic acid, dopamine and the uric acid in solution can be realized while be measured have wider linear detection range.
Description
Technical field
The present invention relates to a kind of composite material modified electrodes can be used for detecting ascorbic acid, dopamine and uric acid simultaneously
Preparation method belongs to materials synthesis and medicine detection research field.
Technical background
Ascorbic acid, dopamine and uric acid usually exist in the matrix of organism, and these biomolecule are for biology
Many physiology courses of body are all extremely important.Dopamine is a kind of neurotransmitter of key in mammalian central nervous system,
Nervous centralis, kidney and systema cariovasculare functional can be adjusted, it can lead to various types in the exception of machine in-vivo content level
The nervous system disease such as schizophrenia, Alzheimer disease and Parkinson's disease, and be easy aids infection poison.Uric acid is
The clinical manifestation of the primary product of purine metabolism, many diseases is exactly the exception of uric acid.Therefore, in health care, bioanalysis
Wish to develop with fields such as pathological researches and the important bioanalysis side such as gets well and detect simultaneously with high sensitivity, selectivity
Method.
Traditional electrode is detected simultaneously using three kinds of voltammetry Ascorbic Acid, dopamine and uric acid substances, since they are non-
Often similar oxidizing potential will appear the phenomenon that oxidation overlap of peaks, is difficult to realize while detecting, limits Ascorbic Acid, DOPA
It is detected while amine and uric acid.In recent years, electrochemical sensor is designed and manufactured using various modified electrodes, is aoxidized
Zinc/oxidation carbon/carbon-copper composite material is due to its change with high catalytic activity, optics sensitivity, the biocompatibility of safety and height
Learn the highest attention that the characteristics such as stability cause scientific research personnel.Carbon ball is applied in terms of electro-catalysis and is seldom aroused attention, but because
The hydro-thermal method used in preparation process to have the advantages that process control, step are simple, method is environmentally protective etc. a series of and by
Using.
By in the zinc oxide-copper oxide prepared/porous carbon ball composite material modification to electrode, it is successfully applied to fight
It is measured while bad hematic acid, dopamine and uric acid, and the oxidation peak of three kinds of substances can be very good to separate, it was demonstrated that zinc oxide-
Copper oxide/porous carbon ball composite material measures at the same time has certain application prospect in ascorbic acid, dopamine and uric acid.
Invention content
The purpose of the present invention is to provide a kind of composite materials can be used for detecting ascorbic acid, dopamine and uric acid simultaneously
The preparation method of modified electrode, zinc oxide-copper oxide/porous carbon ball composite material modification can be to Vitamin C after glass-carbon electrode
Acid, dopamine and uric acid are realized while being measured.
A kind of composite material modified electrode can be used for detecting ascorbic acid, dopamine and uric acid simultaneously of the present invention
Preparation method includes the following steps：
A, the preparation of porous carbon ball：Glucose is added in the beaker containing 60mL ultra-pure waters, by ultrasonic disperse shape
At glucose solution, then glucose solution is placed in the stainless steel autoclave containing teflon liner, in program-controlled case
10h is reacted in formula electric furnace under the conditions of 160 DEG C, being formed by dehydrating polycondensation reaction in glucose water thermal process reactor has nanometer ruler
Very little spherical precursor, there are many oxygen-containing functional groups on surface, and reaction product is taken out after reaction kettle natural cooling with anhydrous
Ethyl alcohol and ultra-pure water centrifuge washing carry out freeze-drying process to centrifugation product and are transferred in crucible, crucible is put in tube furnace
High-temperature calcination is inside carried out under an argon, is cooled to room temperature and is obtained porous carbon ball；
B, the preparation of zinc oxide-copper oxide/porous carbon ball composite material：Weigh gained porous carbon ball, five water sulphur in step a
Sour copper and zinc nitrate are scattered in ultra-pure water, and dispersion liquid is transferred in 100mL hydrothermal reaction kettles, 180 DEG C of reaction 10h, reaction
After, product absolute ethyl alcohol and ultra-pure water centrifuge washing are taken out, freeze-drying process is carried out to get to oxygen to centrifugation product
Change zinc-copper oxide/porous carbon ball composite material；
C, the preparation of zinc oxide-copper oxide/porous carbon ball composite material modified electrode：By gained zinc oxide-oxygen in step b
Change copper/porous carbon ball compound material ultrasound to be scattered in ultra-pure water, dispersant liquid drop is coated onto on electrode, is dried at room temperature, is obtained
Zinc oxide-copper oxide/porous carbon ball composite material modified electrode；
D, it is detected while ascorbic acid, dopamine and uric acid：Prepare ascorbic acid, dopamine and the uric acid of various concentration
Solution, with gained zinc oxide-copper oxide/porous carbon ball composite material modified electrode Ascorbic Acid, dopamine and urine in step c
Acid is carried out while being detected, and then fits linear relationship chart according to the differential pulse figure of various concentration.
Further, the dosage of glucose is 10~30g in step a；
Further, the calcination temperature of tube furnace is 500~900 DEG C in step a；
Further, calcination time is 4~8h in tube furnace in step a；
Further, porous carbon ball dosage is 0.04~0.1g in step b；
Further, Salzburg vitriol dosage is 0.05~0.3g in step b；
Further, zinc nitrate dosage is 0.1~0.5g in step b；
Further, it is 30~80mL for the ultrapure water consumption of dispersion in step b；
Further, in step c zinc oxide-copper oxide/porous carbon ball composite material dispersion liquid a concentration of 1~4mg/
mL；
Further, the dispersion liquid volume in step c in drop coating to electrode is 3~10 μ L；
Further, in step d the range of linearity of ascorbic acid, dopamine and uric acid solution be respectively 100~3000 μM/
L, 13~400 μM/L and 54~1600 μM/L.
The beneficial effects of the invention are as follows this zinc oxide-copper oxide/porous carbon ball composite materials to have excellent electric conductivity
With preferable catalytic activity, ascorbic acid, dopamine and the uric acid in solution can be realized and be measured simultaneously, with wider linear
Detection range.
Description of the drawings
This experiment is further illustrated below in conjunction with the accompanying drawings.
Fig. 1 is the X-ray diffractogram of zinc oxide-copper oxide/porous carbon ball composite material and porous carbon ball in embodiment one；
Fig. 2 be embodiment two in zinc oxide-copper oxide/porous carbon ball composite material be applied to and meanwhile detect ascorbic acid,
The differential pulse figure of dopamine and uric acid；
Fig. 3 is that zinc oxide-copper oxide/porous carbon ball composite material is applied to while detecting various concentration in embodiment two
The differential pulse figure and working curve of ascorbic acid, dopamine and uric acid.Wherein a is differential pulse figure, and b-d is followed successively by Vitamin C
The linear relationship chart of acid, dopamine and uric acid content detection.
Specific implementation mode
Presently in connection with specific embodiment, the present invention will be further described, following embodiment be intended to illustrate invention rather than
Limitation of the invention further.
Embodiment one：
16.2g glucose is added in the beaker of the ultra-pure water containing 60mL, it is molten to form glucose by ultrasonic disperse
Glucose solution is then placed in the stainless steel autoclave containing teflon liner, 160 in program-controlled cabinet-type electric furnace by liquid
10h is reacted under the conditions of DEG C, glucose forms the spherical shape with nano-scale in hydrothermal reaction process by dehydrating polycondensation reaction
Presoma, there are many oxygen-containing functional groups on surface, and reaction product priority absolute ethyl alcohol is taken out after reaction kettle natural cooling
With ultra-pure water centrifuge washing, freeze-drying process is carried out to centrifugation product and is transferred in crucible, crucible is put in argon in tube furnace
High-temperature calcination is carried out under atmosphere, constant temperature 8h carries out carbonization treatment under the conditions of 750 DEG C, to be cooled to obtain porous carbon to room temperature
Ball.It weighs 60mg porous carbon balls, 120mg cupric sulfate pentahydrates and 238mg zinc nitrates and is scattered in ultrasonic disperse in the ultra-pure water of 60mL,
Dispersion liquid is transferred in 100mL hydrothermal reaction kettles, 180 DEG C reaction 10h, after reaction, take out product absolute ethyl alcohol and
Ultra-pure water centrifuge washing carries out freeze-drying process to get to zinc oxide-copper oxide/porous carbon ball composite wood to centrifugation product
Material.
X-ray powder diffraction figure such as attached drawing 1, shows that composite material is successfully prepared, and copper oxide and zinc oxide and porous carbon
The crystal form of copper oxide and zinc oxide will not be changed after ball is compound.
Embodiment two：
It is carried out together with zinc oxide-copper oxide/porous carbon ball composite material modified electrode Ascorbic Acid, dopamine and uric acid
When detect.Include the following steps：
(1) zinc oxide-copper oxide/porous carbon ball compound material ultrasound is scattered in ultra-pure water, then that 5 μ L are a concentration of
In the dispersion liquid modification to electrode of 4mg/mL, dries at room temperature, obtain the zinc oxide-copper oxide/porous carbon ball composite material and repair
The electrode of decorations.
(2) use zinc oxide-copper oxide/porous carbon ball composite material modified electrode Ascorbic Acid, dopamine and uric acid into
It goes while detecting, this experiment uses three-electrode system, and zinc oxide-copper oxide in step (1)/porous carbon ball composite material is modified
Electrode is working electrode, and platinized platinum is to electrode, and saturated calomel electrode is reference electrode, and electrolyte is to contain 2.0mM/L Vitamin Cs
The phosphate buffer of acid, 0.5mM/L dopamines and 2mM/L uric acid.Differential pulse test is carried out, and by differential pulse
The analysis of spike potential and peak current in (attached drawing 2), show composite material modified electrode can realize Ascorbic Acid, dopamine and
It is detected while uric acid.
Embodiment three：
Zinc oxide-copper oxide made from embodiment one/porous carbon ball compound material ultrasound is scattered in ultra-pure water, then
By in the dispersion liquid modification to electrode of 5 a concentration of 4mg/mL of μ L, dries at room temperature, it is multiple to obtain zinc oxide-copper oxide/porous carbon ball
Condensation material modified electrode.Difference is carried out in the phosphate buffer of the ascorbic acid containing various concentration, dopamine and uric acid
Pulse test and peak current fitting operations curve (attached drawing 3) according to differential pulse calculate zinc oxide-copper oxide/porous carbon ball
Composite material modified electrode Ascorbic Acid, dopamine and uric acid detection the range of linearity be respectively 100~3000 μM/L, 13~
400 μM/L and 54~1600 μM/L.
Claims (5)
1. a kind of preparation method for the composite material modified electrode can be used for detecting ascorbic acid, dopamine and uric acid simultaneously, step
It is rapid as follows：
A, the preparation of porous carbon ball：Glucose is added in the beaker containing 60mL ultra-pure waters, Portugal is formed by ultrasonic disperse
Glucose solution is then placed in the stainless steel autoclave containing teflon liner by grape sugar juice, in program-controlled box electricity
10h is reacted in stove under the conditions of 160 DEG C, is formed with nano-scale by dehydrating polycondensation reaction in glucose water thermal process reactor
Spherical precursor, there are many oxygen-containing functional groups on surface, and reaction product absolute ethyl alcohol is taken out after reaction kettle natural cooling
With ultra-pure water centrifuge washing, freeze-drying process is carried out to centrifugation product and is transferred in crucible, crucible is put in tube furnace
High-temperature calcination is carried out under argon atmospher, is cooled to room temperature and is obtained porous carbon ball；
B, the preparation of zinc oxide-copper oxide/porous carbon ball composite material：Weigh gained porous carbon ball, cupric sulfate pentahydrate in step a
It is scattered in ultra-pure water with zinc nitrate, dispersion liquid is transferred in 100mL hydrothermal reaction kettles, 180 DEG C of reaction 10h, reaction terminates
Afterwards, product absolute ethyl alcohol and ultra-pure water centrifuge washing are taken out, freeze-drying process is carried out to get to oxidation to centrifugation product
Zinc-copper oxide/porous carbon ball composite material；
C, the preparation of zinc oxide-copper oxide/porous carbon ball composite material modified electrode：By gained zinc oxide-oxidation in step b
Copper/porous carbon ball compound material ultrasound is scattered in ultra-pure water, and dispersant liquid drop is coated onto on electrode, is dried at room temperature, oxygen is obtained
Change zinc-copper oxide/porous carbon ball composite material modified electrode；
D, it is detected while composite material modified electrode Ascorbic Acid, dopamine and uric acid：Prepare the Vitamin C of various concentration
Acid, dopamine and uric acid solution are fought with zinc oxide-copper oxide/porous carbon ball composite material modified electrode of gained in step c
Bad hematic acid, dopamine and uric acid are carried out while being detected, and then fit linear relationship chart according to the differential pulse figure of various concentration.
2. a kind of composite material modification can be used for detecting ascorbic acid, dopamine and uric acid simultaneously according to claim 1
The preparation method of electrode, it is characterized in that：The dosage of glucose is 10~30g in the step a, and the calcination temperature of tube furnace is
500~900 DEG C, calcination time is 4~8h in tube furnace.
3. a kind of composite material modification can be used for detecting ascorbic acid, dopamine and uric acid simultaneously according to claim 1
The preparation method of electrode, it is characterized in that：The dosage of porous carbon ball is 0.04~0.1g in the step b, Salzburg vitriol
Dosage is 0.05~0.3g, and the dosage of zinc nitrate is 0.1~0.5g, and the dosage of the ultra-pure water for dispersion is 30~80mL.
4. a kind of composite material modification can be used for detecting ascorbic acid, dopamine and uric acid simultaneously according to claim 1
The preparation method of electrode, it is characterized in that：The concentration of zinc oxide-copper oxide/porous carbon ball composite material dispersion liquid in the step c
For 1~4mg/mL, the dispersion liquid volume in drop coating to electrode is 3~10 μ L.
5. a kind of composite material modification can be used for detecting ascorbic acid, dopamine and uric acid simultaneously according to claim 1
The preparation method of electrode, it is characterized in that：The range of linearity of ascorbic acid, dopamine and uric acid solution is respectively in the step d
100~3000 μM/L, 13~400 μM/L and 54~1600 μM/L.
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Cited By (8)
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| CN109387552A (en) * | 2018-10-12 | 2019-02-26 | 温州大学 | A kind of copper-based porous carbon microsphere composite material and preparation method and purposes |
| CN110018214A (en) * | 2019-05-20 | 2019-07-16 | 中南大学 | A kind of method of modified coal Quito pore electrod measurement ascorbic acid content |
| CN111257387A (en) * | 2020-02-19 | 2020-06-09 | 常州大学 | Preparation method of chiral copper oxide-glycine compound modified electrode applicable to electrochemical chiral recognition |
| CN113017995A (en) * | 2021-03-03 | 2021-06-25 | 杭州可靠护理用品股份有限公司 | Adult diaper with uric acid prompting function |
| CN113466299A (en) * | 2020-09-22 | 2021-10-01 | 镇江宏祥自动化科技有限公司 | Electrochemical sensor for detecting ascorbic acid, uric acid and dopamine and preparation method thereof |
| CN114088787A (en) * | 2021-11-17 | 2022-02-25 | 上海第二工业大学 | Two-dimensional ferromagnetic nano composite sensing electrode and preparation method and application thereof |
| CN114436316A (en) * | 2020-11-03 | 2022-05-06 | 中国石油天然气集团有限公司 | Monodisperse flower-shaped copper oxide/carbon nano composite material and preparation method thereof |
| CN114989641A (en) * | 2022-06-23 | 2022-09-02 | 四川轻化工大学 | Modified carbon microsphere/zinc oxide hybrid and preparation method and application thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109387552A (en) * | 2018-10-12 | 2019-02-26 | 温州大学 | A kind of copper-based porous carbon microsphere composite material and preparation method and purposes |
| CN109387552B (en) * | 2018-10-12 | 2021-04-16 | 温州大学 | Copper-based porous carbon microsphere composite material and preparation method and application thereof |
| CN110018214A (en) * | 2019-05-20 | 2019-07-16 | 中南大学 | A kind of method of modified coal Quito pore electrod measurement ascorbic acid content |
| CN110018214B (en) * | 2019-05-20 | 2021-07-23 | 中南大学 | Method for determining content of ascorbic acid by using modified coal-based porous electrode |
| CN111257387A (en) * | 2020-02-19 | 2020-06-09 | 常州大学 | Preparation method of chiral copper oxide-glycine compound modified electrode applicable to electrochemical chiral recognition |
| CN111257387B (en) * | 2020-02-19 | 2021-11-09 | 常州大学 | Preparation method of chiral copper oxide-glycine compound modified electrode applicable to electrochemical chiral recognition |
| CN113466299A (en) * | 2020-09-22 | 2021-10-01 | 镇江宏祥自动化科技有限公司 | Electrochemical sensor for detecting ascorbic acid, uric acid and dopamine and preparation method thereof |
| CN114436316A (en) * | 2020-11-03 | 2022-05-06 | 中国石油天然气集团有限公司 | Monodisperse flower-shaped copper oxide/carbon nano composite material and preparation method thereof |
| CN113017995A (en) * | 2021-03-03 | 2021-06-25 | 杭州可靠护理用品股份有限公司 | Adult diaper with uric acid prompting function |
| CN114088787A (en) * | 2021-11-17 | 2022-02-25 | 上海第二工业大学 | Two-dimensional ferromagnetic nano composite sensing electrode and preparation method and application thereof |
| CN114989641A (en) * | 2022-06-23 | 2022-09-02 | 四川轻化工大学 | Modified carbon microsphere/zinc oxide hybrid and preparation method and application thereof |
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