CN110031526A - One kind being based on K2Fe4O7The dopamine of electrode is without enzyme sensor, preparation method and applications - Google Patents
One kind being based on K2Fe4O7The dopamine of electrode is without enzyme sensor, preparation method and applications Download PDFInfo
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- CN110031526A CN110031526A CN201910326090.6A CN201910326090A CN110031526A CN 110031526 A CN110031526 A CN 110031526A CN 201910326090 A CN201910326090 A CN 201910326090A CN 110031526 A CN110031526 A CN 110031526A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
- G01N27/3275—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction
- G01N27/3277—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction being a redox reaction, e.g. detection by cyclic voltammetry
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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
- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
Abstract
One kind being based on K2Fe4O7The dopamine of electrode belongs to electrochemical sensor technology field without enzyme sensor, preparation method and its application in terms of detecting dopamine.Sensor is made of electrochemical workstation, electrolytic cell and electrode, and electrode is three-electrode system of the platinized platinum to electrode, Ag/AgCl reference electrode and working electrode, working electrode K2Fe4O7The glass-carbon electrode of modification, the electrolyte in electrolytic cell are the phosphate buffer solution containing dopamine to be measured.Sensor of the invention has good selectivity, reproducibility and stability, and electrode catalyst performance is good, can accurately be detected to dopamine, strong antijamming capability；There is wider detection range, lower detection limit simultaneously.
Description
Technical field
The invention belongs to electrochemical sensor technology fields, and in particular to one kind is based on K2Fe4O7The dopamine of electrode is without enzyme
Sensor, preparation method and its application in terms of detecting dopamine.
Background technique
Dopamine (dopamine DA) is present in diplomacy as very important a kind of catecholamine in a kind of organism
All sympathetic nerve, neuromere and central nervous system are a kind of most important neurotransmitters, have and adjust renal function, hormone
The important function such as secretion.The exception of DOPAMINE CONTENT IN RABBIT can cause neurological disease very serious, such as epilepsy, Parkinson's disease, spirit
Split disease, HIV, hyperuricemia and rheumatoid arthritis etc..0.2~0.4ug/ of concentration range of dopamine in normal human
ML, if DOPAMINE CONTENT IN RABBIT increases always or is in a high level, human body can keep excited state, easily be addicting.Cause
And the research detection of dopamine has great importance to the research of neuro-physiology, clinical application, pharmaceutics etc..Inspection at present
The method for surveying dopamine is more, has respectively: high performance liquid chromatography, fluorescent spectrometry, capillary electrophoresis, uv-spectrophotometric
Method and Electrochemical Detection etc..
Electrochemical detection method has and has higher recognition capability to object, and amount of samples is few, response is fast, at low cost,
It is small in size, convenient for universal advantage.In the detection method of dopamine, mostly dependent on the enzyme of dopamine specific recognition or antibody etc.
Bioactive substance prepares biosensor, not only expensive, temperature, the pH value etc. of environment in storage and use process
Aspect all seriously affects its bioactivity.Existing non-enzyme sensor is mostly with carbon material and decorative material and some nano junctions
Structure material is as sensitive material.But these material synthesis method complexity are cumbersome, and synthesis condition is harsh, are not easy to realize, and required original
Material price is expensive, is not suitable for mass production application.A kind of K of patent (201510245772.6) research and development2Fe4O7Inorganic metal
Oxide is a kind of super potassium ion conductor, and is synthesized using conventional hydrothermal synthetic method, and synthesis condition is mild, required original
Material storage is abundant, cheap.
Summary of the invention
In order to solve the disadvantage that the above prior art and shortcoming, the primary purpose of the present invention is that providing one kind has
Good selectivity, high sensitivity and stability it is strong based on K2Fe4O7The Dopamine Sensor of electrode, preparation method and its
Detect the application in dopamine.
The sensor is made of electrochemical workstation, electrolytic cell and electrode, and electrode is platinized platinum to electrode, Ag/AgCl reference
The three-electrode system of electrode and working electrode, working electrode K2Fe4O7The glass-carbon electrode of modification, the electrolyte in electrolytic cell are
Phosphate buffer solution (PBS) containing dopamine to be measured.
The electrochemistry Dopamine Sensor can realize the detection of micro DOPAMINE CONTENT IN RABBIT, and the detection range of linearity is 2 μM~140
μM, lowest detection is limited to 0.082 μM.
K2Fe4O7Decorative material is prepared by one step of hydrothermal synthesis method, and the method is simple, mildly.Required synthesis
Material is Fe (NO3)3·9H2O and KOH, these material storages are abundant, cheap, can be with mass production.
Specifically, the present invention is achieved through the following technical solutions:
K is synthesized according to the method for patent (201510245772.6)2Fe4O7Crystal.
It is of the present invention to be based on K2Fe4O7The preparation method of the Dopamine Sensor of electrode, its step are as follows:
(1) K is prepared2Fe4O7The glass-carbon electrode of modification
Firstly, by K2Fe4O7Crystal is ground into partial size by ball grinding method in dehydrated alcohol and is less than or equal to 3 μm
K2Fe4O7Powder is dried after sieving；
Secondly, by 5mgK2Fe4O7Powder is distributed in n,N-Dimethylformamide (DMF), and ultrasonic disperse 20~40 minutes,
Then 1~3 μ L naphthols is added, K is configured to2Fe4O7Concentration is the electrode modification liquid of 0.5~2.0mg/mL；
Then, glassy carbon electrode surface is processed by shot blasting using the alumina slurry of 0.05 μm of specification, then uses deionization
Water and dehydrated alcohol are cleaned by ultrasonic the glass-carbon electrode after polishing treatment, finally dry to obtain pretreatment glass carbon at room temperature
Electrode；
Finally, weighing electrode A with liquid-transfering gun modifies drop-coated to pretreatment glassy carbon electrode surface, dries, obtain at room temperature
K as working electrode2Fe4O7The glass-carbon electrode of modification；
(2) with the phosphate buffer solution (PBS) containing dopamine to be measured for electrolyte, the concentration of PBS is 0.1M (in solution
The concentration of all phosphate anions)；By working electrode, reference electrode, electrochemical workstation is connected to one end of electrode, by work
Make electrode, reference electrode, above-mentioned electrolyte is inserted into the other end of electrode, electrolyte is placed in electrolytic cell；In electrochemical operation
Differentiated pulse volt-ampere technology (DPV) is used on standing, voltage range is -0.4V~0.8V, record current-voltage curve, i.e. DOPA
The DPV curve of amine response, to be prepared based on K2Fe4O7The Dopamine Sensor of electrode.
The beneficial effect of the present invention compared with the existing technology is:
Materials synthesis is at low cost, and the detection range of linearity is wide, and the advantage that detection limit is low and selectivity is good, furthermore this sensor can
To be applied in the qualitative and quantitative analysis of dopamine, main reason is that the modified electrode material of sensor has high potassium ion to lead
Electric energy power, good electro-catalysis ability.
Detailed description of the invention
Fig. 1 is K produced by the present invention2Fe4O7The peak current and phosphoric acid for the DPV curve that electrode measures in 100 μM of DA are slow
Rush the relation curve of the pH of solution；
Fig. 2 is K produced by the present invention2Fe4O7DPV of the electrode in the phosphate buffer solution containing various concentration dopamine
Curve；
Fig. 3 is K produced by the present invention2Fe4O7The concentration of the linear fit dopamine of electrode and the relationship of its peak current are bent
Line；
Fig. 4 is K produced by the present invention2Fe4O7The selective figure of electrode；
Fig. 5 is K produced by the present invention2Fe4O7Reproducibility, repeatability and the stability diagram of electrode.
Specific embodiment
Required raw material is K in each embodiment2Fe4O7, it is DMF (traditional Chinese medicines production), naphthols, secondary deionized water (self-control), anhydrous
Ethyl alcohol (Beijing chemical industry).
The preparation of 1 working electrode of embodiment
By K2Fe4O7Crystal is ground into the powder less than or equal to 3 μm by ball grinding method in dehydrated alcohol, is sieved, and dries
It is dry；By 5mg K2Fe4O7Powder is distributed in the n,N-Dimethylformamide (DMF) of 5mL, and ultrasonic disperse 30 minutes, 2 μ L are added
Naphthols, being configured to concentration is 1mg/mL electrode modification liquid；
Glass-carbon electrode is processed by shot blasting using the alumina slurry of 0.05 μm of specification, with deionized water and dehydrated alcohol
Glass-carbon electrode is cleaned by ultrasonic, last room temperature dries to obtain pretreatment glass-carbon electrode；0.5 μ L preparation gained is taken with liquid-transfering gun
Electrode modification drop be coated onto the glassy carbon electrode surface of polishing, room temperature is dried, and K is obtained2Fe4O7The glass-carbon electrode of modification.
Embodiment 2
The pH of phosphate buffer solution is selected
Embodiment 1 is repeated, by K obtained2Fe4O7The glass-carbon electrode of modification immerses electrode, reference electrode and contains 100 μM
In the phosphate buffer solution of the pH=7.0 of dopamine, 7.2,7.4,7.6,7.8, DPV technology is selected on electrochemical workstation,
Scanning range is -0.4V~0.8V, obtains the DPV curve of dopamine.From figure 1 it appears that the oxidation peak current of dopamine
With the increase of pH, first increase reduces afterwards, and in pH=7.6, peak current reaches maximum.
Embodiment 3
The linear quantitative detection performance of sensor
The phosphate buffer solution for the pH=7.6 that one group of dopamine concentration is 2 μM to 140 μM is configured, embodiment 1 is repeated, is surveyed
The DPV curve of sensor is tried, scanning range is -0.4V~0.8V.From Fig. 2 it is known that the oxidation peak current of dopamine with
The increase of dopamine concentration and increase.Two can be divided by the concentration of linear fit acquisition dopamine and the relationship of its peak current
Section linear relationship, such as Fig. 3, first is that when the concentration of dopamine is at 2~30 μM, peak current Ip (mA) and dopamine concentration CDA(μ
M) linear equation of relationship is Ip (mA)=1.12+0.023CDA(μM), (R2=0.992).Second is that when the concentration of dopamine is 40
At~140 μM, the linear relationship equation of peak current and concentration is Ip (mA)=1.55+0.01CDA(μM), (R2=0.990).
The detection limit that dopamine is estimated by three times noise method (S/N=3) is 0.082 μM.
Embodiment 4
The selective enumeration method of sensor
The phosphate buffer solution containing 1mM ascorbic acid and 100 μM of uric acid is respectively configured and contains 1mM ascorbic acid, 100
The phosphate buffer solution of μM uric acid and 100 μM of dopamines repeats the K that embodiment 1 will obtain2Fe4O7It is the glass-carbon electrode of modification, right
Electrode, reference electrode immerse in two kinds of solution, with the selectivity of differentiated pulse volt-ampere technology detection sensor.As can be seen from Figure 4, when
In the presence of dopamine, the oxidation peak of uric acid disappears, and the testing result of ascorbic acid is the same, illustrates that the material has dopamine detection
Selectivity well.
Embodiment 5
The reproducibility of sensor, repeatability, Detection of Stability
Reproducibility: embodiment 1, the K that will be obtained are repeated2Fe4O7The glass-carbon electrode of modification immerses electrode, reference electrode and inserts
Enter in the phosphate buffer solution containing 100 μM of dopamines, retest 8 times, obtains current -voltage curve.As shown in Figure 5 a, 8
Secondary peak current difference is very small, and calculating gained relative standard deviation is 1.07%.
Repeatability: embodiment 1 is repeated, 5 K are obtained2Fe4O7The glass-carbon electrode of modification, and electrode, reference electrode are distinguished
It immerses in the phosphate buffer solution containing 100 μM of dopamines, tests the DPV curve of sensor.As shown in Figure 5 b, 5 electrodes
Peak current difference is very small, and calculating gained relative standard deviation is 0.16%.
Storage stability: embodiment 1 is repeated, modified electrode is stored in PBS 3 days at 4 DEG C, tests the sensor
Current -voltage curve.Such as Fig. 5 c, in 3 days, the peak point current in the very small third day of peak current variation is the 93.5% of first day.
From the above as it can be seen that it is of the present invention it is a kind of detect dopamine electrochemical sensor and preparation method thereof,
At low cost with materials synthesis, it is good that the detection range of linearity is wide, detection limits low and selectivity, reproducibility, repeatability, stability
Advantage.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, exist
Under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to of the invention
Protection scope.
Claims (5)
1. one kind is based on K2Fe4O7The dopamine of electrode is without the enzyme sensor sensor, by electrochemical workstation, electrolytic cell and electricity
Pole composition, electrode are three-electrode system of the platinized platinum to electrode, Ag/AgCl reference electrode and working electrode, it is characterised in that: work
Electrode is K2Fe4O7The glass-carbon electrode of modification, the electrolyte in electrolytic cell are the phosphate buffer solution containing dopamine to be measured.
2. as described in claim 1 a kind of based on K2Fe4O7The dopamine of electrode exists without the enzyme sensor sensor, feature
In: the sensor can realize the detection of micro DOPAMINE CONTENT IN RABBIT, and the detection range of linearity is 2 μM~140 μM.
3. as claimed in claim 2 a kind of based on K2Fe4O7The dopamine of electrode exists without the enzyme sensor sensor, feature
In: the sensor is limited to 0.082 μM to the lowest detection of dopamine.
4. one kind described in claims 1 to 3 any one is based on K2Fe4O7The dopamine of electrode is without the enzyme sensor sensor
Preparation method, its step are as follows:
(1) K is prepared2Fe4O7The glass-carbon electrode of modification
Firstly, by K2Fe4O7Crystal is ground into the K that partial size is less than or equal to 3 μm by ball grinding method in dehydrated alcohol2Fe4O7Powder
End is dried after sieving；
Secondly, by 5mgK2Fe4O7Powder is distributed in n,N-Dimethylformamide, ultrasonic disperse 20~40 minutes, is then added again
Enter 1~3 μ L naphthols, is configured to K2Fe4O7Concentration is the electrode modification liquid of 0.5~2.0mg/mL；
Then, glassy carbon electrode surface is processed by shot blasting using the alumina slurry of 0.05 μm of specification, then with deionized water and
Dehydrated alcohol is cleaned by ultrasonic the glass-carbon electrode after polishing treatment, finally dries to obtain pretreatment glass carbon electricity at room temperature
Pole；
Finally, weighing electrode modification drop with liquid-transfering gun is coated onto pretreatment glassy carbon electrode surface, dries, obtained as work at room temperature
Make the K of electrode2Fe4O7The glass-carbon electrode of modification；
(2) using the phosphate buffer solution containing dopamine to be measured as electrolyte, by working electrode, reference electrode, to the one of electrode
End is connected to electrochemical workstation, by working electrode, reference electrode, is inserted into above-mentioned electrolyte, electrolyte to the other end of electrode
It is placed in electrolytic cell；Differentiated pulse volt-ampere technology is used on electrochemical workstation, voltage range is -0.4V~0.8V, record
Current -voltage curve, to be prepared based on K2Fe4O7The Dopamine Sensor of electrode.
5. one kind described in claims 1 to 3 any one is based on K2Fe4O7The dopamine of electrode is more in detection without enzyme sensor
Application in bar amine.
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| CN111157601A (en) * | 2020-01-15 | 2020-05-15 | 吉林大学 | Based on K2Fe4O7Room-temperature high-humidity hydrogen sulfide gas sensor of electrolyte, preparation method and application thereof |
| CN113702472A (en) * | 2021-09-01 | 2021-11-26 | 吉林大学 | (Ni1-xFex) Mixed potential type room temperature NO sensor with-MOF as sensitive electrode and preparation method thereof |
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| CN113702472A (en) * | 2021-09-01 | 2021-11-26 | 吉林大学 | (Ni1-xFex) Mixed potential type room temperature NO sensor with-MOF as sensitive electrode and preparation method thereof |
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