CN108254421B - Flower shape Au micro nano structure, modified electrode and preparation method and application - Google Patents
Flower shape Au micro nano structure, modified electrode and preparation method and application Download PDFInfo
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Abstract
The present invention relates to a kind of flower shape Au micro nano structure, modified electrode and preparation sides and application, during synthesis, by the experiment parameter in regulation synthesis process, to regulate and control the pattern of flower nanostructure, and finally it has been made and has been self-assembled by Au nanometer sheet into Au micro nano structure；Develop Dopamine Sensor as working electrode using this flower shape Au applied field electrode；Electrochemical data shows that flower shape Au nanostructure can speed up electronics and transmit in dopamine and electrode surface, reduce the overpotential in electrochemical oxidation process, 1.25 μM of concentration in dopamine are arrived 1.07mM range, there are linear relationship (R=0.997), detection is limited to 0.61 μM for oxidation peak current and concentration.In addition, synthesized electrochemical sensor is with good stability and repeated；A kind of new method is provided for the actual analysis detection of dopamine.
Description
Technical field
The present invention relates to electrochemica biological sensor technical field, especially a kind of flower shape Au micro nano structure, modification
Electrode and preparation method and application.
Background technique
Metal nano material causes the sizable interest of scientists in recent years, due to its novel optics, electronics, urges
Change, is magnetic and potentially apply in the fields such as physics, chemistry, biology, medicine and material and interdisciplinary fields, it is especially golden
Belonging to base nano electrochemical, the interdisciplinary fields emerging as one have become interesting one of field, this is because
The modified electrochemical interface of metal nano material is capable of providing very high electrochemical surface area to sensitive to improve detection
Degree, and metal nano material has good transmission electronic capability, is conducive to accelerate electronics in electrode surface and probe molecule
Between transfer, to accelerate current-responsive, while reducing the overpotential of electrochemical reaction.Compared to humble nanostructure, three
Tieing up multi-layer nano structure has multilayered structure abundant and bigger surface area, shows more excellent characteristic.Due to nanometer
The many advantages of multilayered structure, design synthesize more nanostructures and receive more and more attention.For example, Torati et al. benefit
It is prepared for multilayer gold nano structure with an one-step electrochemistry sedimentation, and develops electrochemical immunosensor as conducting medium
Detect CA125 antibody, the range of linearity (10-100U mL that the electrochemica biological sensor prepared has been shown-1), low spot inspection
Survey limit (3U mL-1) and good repeatability and stability.How people devises a simple two steps hot steam reaction process
Prepare the p-Te/SnO of toothbrush pattern2Multi-layer nano structure, this nano-multilayered structures assembling sensor are used to detect NH3, show
Excellent catalytic performance.
Dopamine, also known as catechol aminopherase, a kind of important mind as nervous system and endocrine system
Through mediator, the various physiological processes of brain and body are participated in.It is synthesized by 3,4-dihydroxy benzenes ethylene alanine, and can be used as
Synthesize the presoma of neurotransmitter adrenaline and noradrenaline.Dopamine regulates and controls mediator as cerebral nerve, can also be right
Mood, behavior, memory, attention and behavior are regulated and controled.Disease in terms of dopamine will appear spirit extremely in vivo, for example, pa
The gloomy disease of gold, schizophrenia, epilepsy, senile dementia and attention deficit-hyperactivity disorder.In addition, dopamine exceeds permission in vivo
Value may cause myocardial infarction, hypertension, bronchial asthma and polarity heart disease.Therefore, develop it is a kind of it is simple and quick, have
The dopamine that highly selective and sensitivity method measures is of great significance.Currently, the method for dopamine detection has
High performance liquid chromatography, ultraviolet spectrophotometry, Capillary Electrophoresis, liquid chromatogram-mass spectrometry, Flow Injection Spectrophotometry,
Coulomb equation and electrochemical determination method etc..Electrochemical method is considered as most promising one of method, because he
Highly sensitive and low cost the advantages that.However, it is irreversible that dopamine aoxidizes directly on bare electrode, and need high
Overpotential leads to electrode fouling, and reproducibility is poor, the low and poor sensitivity of selectivity.Currently, various nano materials are selected
Selectivity, sensitivity are improved as sensor interface decorative material.
As a kind of nano material of classics, there are excellent transmission electronic capability, high catalytic activity for gold nano-material
And good biocompatibility.This is because the specific surface rate of the Jin Yougao of Nano grade, has more active atomics exposed
In outer surface.In terms of dopamine catalysis oxidation, gold nano-material can increase electron-transport speed as good sensor information
Rate, the activation energy for reducing reaction and increase detection signal.The catalytic performance of nano material and its pattern, size have very high point
System.Therefore, new pattern is prepared, the gold nano structure of excellent function is very important.
Summary of the invention
The purpose of the present invention is to provide a kind of flower shape Au micro nano structures, and with this flower shape Au micro nano structure pair
Bare electrode is modified to realize the detection to dopamine.
The purpose of the present invention can be achieved through the following technical solutions:
The present invention provides a kind of flower shape Au micro nano structure, the flower shape Au micro nano structure by thickness 5-60nm,
1-20 μm of length of nanometer sheet is self-assembled into, and the particle size range of flower shape Au micro nano structure is 2-40 μm.
The present invention also provides a kind of preparation methods of flower shape Au micro nano structure, including following reaction step:
Step 1: preparing certain density ammonium chloride solution and certain density chlorauric acid solution respectively；
Step 2: a certain amount of ammonium chloride solution and a certain amount of chlorauric acid solution are taken respectively, it under stirring conditions, will
The ammonium chloride solution taken is added in acquired chlorauric acid solution, and a certain amount of polyvinyl pyrrole is then added into solution again
Alkanone continues to stir certain time, obtains mixed solution；
Step 3: electro-conductive glass being cleaned up with acetone, ethyl alcohol and deionized water respectively, then uses N2Air-blowing is dry, is put into
In the mixed solution of step 2；
Step 4: step 3 gained mixed solution being transferred in the reaction kettle of teflon lined, Muffle furnace is put into, one
Hydro-thermal reaction is carried out at fixed temperature and certain time；
Step 5: after completion of the reaction, by reaction kettle cooled to room temperature, centrifuge separation gained hydro-thermal reaction product will be from
Product after heart separation dries certain time at a certain temperature, obtains flower shape Au micro nano structure.
Further, the concentration of ammonium chloride solution is 0.5-5mM in step 1, and the concentration of chlorauric acid solution is 0.5-5mM.
Further, the dosage of ammonium chloride solution is 2-10mL in step 2, and the dosage of chlorauric acid solution is 5-30mL, is gathered
Second
The dosage of alkene pyrrolidone is 0.2-2g, mixing time 10-30min.
Further, the reaction temperature in step 4 is 150-300 DEG C, and the reaction time is 2-6 hours.
Further, the drying temperature in step 5 is 50-80 DEG C, and drying time is 3-6 hours.
The present invention also provides a kind of preparation methods of flower shape Au micro nano structure modified electrode, comprising the following steps: will
Flower shape Au micro nano structure, which is scattered in a certain amount of distilled water, obtains flower shape Au micro nano structure aqueous solution, to gained
A certain amount of naphthols is added in aqueous solution, obtains mixed solution after mixing evenly, takes a certain amount of mixed solution drop coating to processing
Good electrode surface, is dried with infrared lamp, obtains flower shape Au micro nano structure modified electrode；
The dosage of the distilled water is 10-30mL, and the amount of naphthols used is 0.4-2mL, and the concentration of naphthols is 2-10wt%,
The dosage of the mixed solution is 1-5 μ L.
The present invention also provides a kind of application of flower shape Au micro nano structure modified electrode in measurement dopamine.Flower shape
Au applied field electrode and Ag/AgCl (3.5M KCl) electrode, Pt plate electrode be assembled into three-electrode system measurement DOPA
Amine；The electrochemical methods such as cyclic voltammetric, chrono-amperometric are used to measure the catalysis oxidation behavior of dopamine.
Wherein, electro-chemical test uses electrochemical workstation CHI 660D, characterizes Scanning Electron microscope (SEM) used and is
Hitachi S-5200 model (Japan), x-ray diffractometer (XRD) are D/tex Ultra/UItimaIV-ray
Diffractometer model.
The present invention its advantage compared with prior art are as follows:
(1) present invention synthesizes flower shape Au micro nano structure in conductive glass surface using a step hydrothermal synthesis technology；?
During synthesis, by the experiment parameter (temperature and time) in regulation synthesis process, to regulate and control flower micro nano structure
Pattern, and be finally made and be self-assembled by Au nanometer sheet into Au micro nano structure；
(2) spirit to dopamine is realized using the electro-conductive glass assembling three-electrode system of flower shape Au micro nano structure modification
Quick detection；Electrochemical data shows that this sensor has a good catalytic performance, the wide range of linearity, good selectivity and long-term
Stability；
(3) it is irreversible that the present invention, which solves dopamine and aoxidizes directly on bare electrode, and needs high overpotential,
Lead to electrode fouling, reproducibility is poor, selectivity low and poor sensitivity the problem of.
Detailed description of the invention
Figure 1A-D is the Au micro nano structure that the present invention characterizes prepared flower shape using SEM.
Fig. 2 is that hydrothermal synthesis temperature setting is 180 DEG C, and the reaction time is set as 4h；Nanowire structure obtained.
Fig. 3 is the XRD diagram of the Au micro nano structure of flower shape.
Fig. 4 curve A is that cyclic voltammetry curve of the Au micro nano structure to dopamine catalysis oxidation, the curve B of flower shape are
Cyclic voltammetry curve of the electro-conductive glass for dopamine catalysis oxidation.
Fig. 5 is electro catalytic activity of the Au micro nano structure for dopamine when the concentration of dopamine is from 1mM to 9mM
Relationship of the Fig. 6 between scanning speed and redox peak current to dopamine flower shape Au micro nano structure
The kinetics relation of electrode surface reaction.
Fig. 7 is chrono-amperometric response curve of the dopamine in the Au micro-and nano-structural surface of flower shape.
Fig. 8 is that dopamine concentration does linear relationship in step oxidation current and corresponding solution.
Fig. 9 is glucose, urea, L-cysteine, H2O2, interference of the ascorbic acid to dopamine determination.
Specific embodiment
The present invention provides a kind of flower shape Au micro nano structure, the flower shape Au micro nano structure by thickness 5-60nm,
1-30 μm of length of Au nanometer sheet is self-assembled into.
The present invention also provides a kind of preparation methods of flower shape Au micro nano structure, including following reaction step:
Step 1: 5mL 2mM NH4Cl and 1g PVP being added separately in 20mL 2mM HAuCl4 solution, are stirred
Uniformly, mixed solution is prepared；
Step 2: electro-conductive glass acetone, ethyl alcohol and deionized water being cleaned up, N is then used2Air-blowing is dry, is put into step
In 1 mixed solution；
Step 3: mixed solution in step 2 being transferred in the reaction kettle of teflon lined, Muffle furnace is put into and is added
Heat, reaction temperature are 220 DEG C, and the reaction time is 4 hours；
Step 4: after completion of the reaction, by reaction kettle cooled to room temperature, centrifuge separation gained hydro-thermal reaction product will be from
Product after heart separation is 7-14 hours dry in 60-80 DEG C of vacuum oven, obtains flower shape Au micro nano structure.
Such as Figure 1A-D, when temperature setting is 220 DEG C, the reaction time is set as 4h, the Au micro nano structure of flower shape by
Function synthesis, can clearly find that the Au nanostructure of flower shape is made of Au nanometer sheet；The Au of this flower shape is micro-nano
Structure can provide more active site and big electrochemical surface area, and substrate is accelerated to spread in the mass transfer of electrode surface；For
Further probe into the formation mechenism of nanometer sheet；
As a comparison, other conditions are constant, and when being 180 DEG C hydrothermal synthesis temperature setting, the reaction time is similarly 4h；Most
The nanowire structure (such as Fig. 2) obtained afterwards.It is possible thereby to infer, other conditions are constant, and temperature is higher, it is intended to synthesize nanometer sheet
Structure.
It is characterized using Au micro nano structure of the XRD to flower shape；As seen from Figure 3,38.2,44,6,64.7,
Occurs Au characteristic peak at 77.6 and 81.7 respectively；Illustrate in hydrothermal reaction process, gold ion is successfully reduced into flower shape
Au micro nano structure.
The present invention also provides a kind of preparation methods of flower shape Au micro nano structure modified electrode, comprising the following steps:
Flower shape Au micro nano structure is dissolved in the secondary distilled water of 20mL to obtain flower shape Au micro nano structure water-soluble
1mL 5wt% naphthols is added into obtained aqueous solution, obtains mixed solution after mixing evenly, takes 1-5 μ L mixed solution drop coating for liquid
It to the glassy carbon electrode surface handled well, is dried with infrared lamp, obtains flower shape Au micro nano structure modified electrode.
The present invention also provides a kind of application of flower shape Au micro nano structure modified electrode in measurement dopamine.Flower shape
Au applied field electrode and Ag/AgCl (3.5M KCl) electrode, Pt plate electrode be assembled into three-electrode system measurement DOPA
Amine；The electrochemical methods such as cyclic voltammetric, chrono-amperometric are used to measure the catalysis oxidation behavior of dopamine.
Electrochemical behavior of the dopamine in flower shape Au micro-and nano-structural surface:
Fig. 4 curve A shows cyclic voltammetry curve of the Au micro nano structure to dopamine catalysis oxidation of flower shape；As right
Than Fig. 4 curve B is cyclic voltammetry curve of the electro-conductive glass for dopamine catalysis oxidation；As shown, the current potential on A curve
Showing a pair of apparent redox peaks at 0.214 V and 0.103V, peak current is respectively 631.5 μ A and -475.5 μ A, and
Redox peak current is unobvious on Fig. 4 curve B curve；We further study Au nanostructure and the electricity of dopamine are urged
Change activity, when the concentration of dopamine is gradually increased from 1mM to 9mM, oxidation peak current also gradually increases (Fig. 5).
The influence of scanning speed:
It is micro-nano in the Au of flower shape to dopamine by the relationship between research scanning speed and redox peak current
The dynamic behavior of structure electrode surface reaction is studied (Fig. 6), and as seen from the figure, with the increase of scanning speed, oxidation is also
Parent peak electric current gradually increases, and redox peak current and the square root of surface sweeping speed is taken to do calibration curve；By insertion figure it is found that oxygen
Change the square root of reduction peak current and surface sweeping speed there are linear relationship, related coefficient is respectively 0.999 and -0.999；As a result it shows
Show, dopamine the Au nanostructured surface of flower shape be diffusion velocity quickly, electrode process is controlled by diffusion.
The catalysis behavior of sensor
Fig. 7 is chrono-amperometric response curve of the dopamine in the Au nanostructured surface of flower shape, and 0.214V is arranged in current potential,
With the addition of dopamine, oxidation current step is gradually risen, and transition is completed in 5s；Take step oxidation current with it is corresponding molten
Dopamine concentration does linear relationship chart (Fig. 8) in liquid；As shown in Figure 8,1.017mM concentration range is arrived at 1.25 μM of dopamine concentration
Interior, with corresponding dopamine concentration there are good linear relationship, related coefficient 0.997 detects and is limited to 0.61 μM step-flow,
Sensitivity is 166.5 μ AmMcm-2。
Table 1 is that the Dopamine Sensor and document report Dopamine Sensor prepared by us are limited in the range of linearity, detection
It is compared in terms of sensitivity；Data show that the Dopamine Sensor that we prepare has the wide range of linearity, and high is sensitive
Degree.
Table 1
Chaff interferent measurement
In actual sample analysis, some biomolecule coexisted tend to the measurement of interference dopamine, we study
Some coexisting substances (glucose, urea, L-cysteine, H2O2, ascorbic acid) interference (Fig. 9) to dopamine determination；?
Under 0.214V current potential, 50 μ L 2mM dopamines (A), 50 μ L20mM glucose (B), 50 μ L20mM uric acid (C), 50 μ are gradually added dropwise
L20mM H2O2(D), 50 μ L20mM L-cysteines (E), 50 μ L20mM ascorbic acid (F) and 500 μ L 2mM dopamines；By
Figure is it is found that when solution, glucose, H is added in chaff interferent2O2, uric acid, L-cysteine without significantly oxidation step occur, it is anti-bad
Hematic acid generates a small oxidation current step after being added, but interferes smaller.
Stability and repeatability
As the important indicator of evaluation sensor, we grind the repeatability and stability of Dopamine Sensor
Study carefully, the Au micro nano structure of flower shape continuous scanning 50 in the buffer solution of 5mM dopamine is enclosed, and catalysis oxidation electric current becomes former
94.12% come, illustrating sensor, there are good repeatability；The Au nanostructure of flower shape is stored in 4 DEG C of refrigerator
In, catalysis oxidation electric current becomes original 95.2% after 15 days, and there are good stability for display sensor.
Claims (3)
1. a kind of flower shape Au micro nano structure, it is characterised in that: the flower shape Au micro nano structure is long by thickness 5-60nm
The Au nanometer sheet self assembly of 1-20 μm of degree forms, and the particle size range of flower shape Au micro nano structure is 2-40 μm；
The preparation method of the flower shape Au micro nano structure includes following reaction step:
Step 1: by 5mL 2mM NH4Cl and 1g PVP is added separately to 20mL 2mM HAuCl4In solution, it is stirred
It is even, prepare mixed solution；
Step 2: electro-conductive glass acetone, ethyl alcohol and deionized water being cleaned up, N is then used2Air-blowing is dry, is put into the mixed of step 1
It closes in solution；
Step 3: mixed solution in step 2 being transferred in the reaction kettle of teflon lined, Muffle furnace is put into and is heated, instead
Answering temperature is 220 DEG C, and the reaction time is 4 hours；
Step 4: after completion of the reaction, by reaction kettle cooled to room temperature, centrifuge separation gained hydro-thermal reaction product, by centrifugation point
Product from after is 7-14 hours dry in 60-80 DEG C of vacuum oven, obtains flower shape Au micro nano structure.
2. a kind of preparation method of flower shape Au micro nano structure modified electrode, the flower shape Au micro nano structure uses right
It is required that flower shape Au micro nano structure described in 1, which comprises the following steps: by flower shape Au micro nano structure
It is dissolved in the secondary distilled water of 20mL and obtains flower shape Au micro nano structure aqueous solution, 1mL 5wt% is added into obtained aqueous solution
Nafion obtains mixed solution after mixing evenly, takes 1-5 μ L mixed solution drop coating to the glassy carbon electrode surface handled well, and use is red
Outer lamp drying, obtains flower shape Au micro nano structure modified electrode.
3. a kind of flower shape Au micro nano structure modified electrode prepared by the preparation method using claim 2 is in measurement dopamine
In application.
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|---|---|---|---|---|
| CN102828176A (en) * | 2012-07-31 | 2012-12-19 | 东南大学 | Preparation method for uniform gold nanoparticle film |
| CN103273079A (en) * | 2013-05-10 | 2013-09-04 | 安徽医科大学 | Gold nanoflower preparing method and application of gold nanoflowers |
| CN105903948A (en) * | 2016-04-21 | 2016-08-31 | 玉林师范学院 | Gold nanoflower nano-particle and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102828176A (en) * | 2012-07-31 | 2012-12-19 | 东南大学 | Preparation method for uniform gold nanoparticle film |
| CN103273079A (en) * | 2013-05-10 | 2013-09-04 | 安徽医科大学 | Gold nanoflower preparing method and application of gold nanoflowers |
| CN105903948A (en) * | 2016-04-21 | 2016-08-31 | 玉林师范学院 | Gold nanoflower nano-particle and preparation method thereof |
Non-Patent Citations (2)
| Title |
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| A gold electrode with a flower-like gold nanostructure for simultaneous determination of dopamine and ascorbic acid;Yanjie Zheng 等;《Microchim Acta》;20130215;第537-534页 * |
| Flower-like gold nanostructures electrodeposited on indium tin oxide (ITO) glass as a SERS-active substrate for sensing dopamine;Yanru Bu 等;《Microchim Acta》;20150206;第1313-1321页 * |
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