CN104950027A - Synthesis of graphene/polyaniline/gold nanoparticle composite material and application thereof to dopamine detection - Google Patents
Synthesis of graphene/polyaniline/gold nanoparticle composite material and application thereof to dopamine detection Download PDFInfo
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Abstract
The invention relates to synthesis of a graphene/polyaniline/gold nanoparticle composite material and application thereof to high-sensitivity dopamine detection. The synthesis of the graphene/polyaniline/gold nanoparticle composite material and the application to dopamine detection comprise the following steps: preparing a graphene/polyaniline/gold nanoparticle composite material and preparing a graphene/polyaniline/gold nanoparticle composite material modified electrode. The synthesis of the graphene/polyaniline/gold nanoparticle composite material and the application to dopamine detection have the advantages that the composite material modified electrode has high sensitivity, low detection limit, simplicity and convenience in operation and quickness in detection of dopamine in a solution.
Description
Technical field
The present invention relates to the synthesis of a kind of graphene/polyaniline/golden nanometer particle compound substance and be applied to the highly sensitive detection of dopamine, belonging to biology sensor and materials synthesis field.
Technical background
Dopamine (DA) is a kind of Catecholamines Neurotransmitters in Blood be present in nerve fiber and body fluid, is the material base of brain function.Its content distribution of specific region in human brain affects the coordination of hypophysis endocrine dysfunction, and directly relevant with nervous activity.In brain, dopamine neuronal functional disturbance is the major reason of schizophrenia and Parkinson's disease.In addition, dopamine also has excited heart, increases the function of renal blood flow, is used for the treatment of ischemic, heart source property and infectious shock.Therefore, the research carrying out dopamine analyzing detecting method is important in inhibiting in the quality control etc. of nervous physiology function, medical diagnosis on disease and related drugs.At present, the method detecting dopamine is mainly: spectrophotometric method, chemoluminescence method, chemiluminescence, liquid phase chromatography and electrochemical process etc.Electrochemical process is for other detection method, and advantages such as having fast, energy consumption is low, small investment, simple to operate and detectability are low is a kind of economical and effective method.Therefore, electrochemical process is a kind of detection dopamine technology with development prospect.
Because chemically modified electrode has modified Functional Design to electrode surface by the method for chemistry or physics to electrode surface, therefore preparation method is the key of chemically modified electrode performance, the reliability of method directly has influence on repeatability and the stability of chemically modified electrode, and then has influence on theoretical research and the practical application of chemically modified electrode.In the work detecting dopamine, generally select electrocatalysis characteristic more excellent and the compound substance modified electrode that charge transport capability is stronger.In recent research, Graphene is extensively joined to improve the performance of material in various functional material, and Graphene is by individual layer sp
2hydbridized carbon atoms forms, and has good electric conductivity.Graphene, as a kind of carbon nanomaterial of two-dimensional structure, has peculiar electronics and physical characteristics, has special planar structure, high specific surface area (2600m
2/ g) and ultra-thin crystal thickness (0.34nm), there is important application prospect in fields such as molectronics, micro-nano device, high-efficiency battery, sensor, capacitors.In addition, the compound substance that conducting polymer and metal nanoparticle are formed can make full use of the advantage of both performance complements, therefore becomes the important channel of traditional material multifunction and new material exploitation.In numerous conducting polymer composites, polyaniline (PANI) raw material is cheap, synthesize easy, high temperature resistant and antioxygenic property is good, conductivity is variable, therefore demonstrates wide application prospect in a lot of fields.In recent years, increasing achievement in research shows, metal nanoparticle is introduced as Au Ag Pt Pd, copper etc. in polyaniline, the compound substance formed is compared with matrix polyaniline, its electrical property, electrochemical response performance and electrocatalysis characteristic etc. are obtained for further lifting, show more wide application prospect.The excellent electrocatalysis characteristic that the metal electrode that polyaniline and noble metal nano particles are modified jointly has derives from both synergy, and the existence of polyaniline makes metallic particles obtain higher dispersion degree and stability and have good electric conductivity.
Graphene/polyaniline/golden nanometer particle compound substance not only has nm of gold and the original specific performance of polyaniline simultaneously, and two also also exist mutual synergy between component, greatly improve the performance of polyaniline matrix, Graphene add the conductivity that more improve compound substance, make it show excellent electrocatalysis characteristic and special charge transfer.
Summary of the invention
The object of the invention is to be to provide a kind of new electrode modified material graphene/polyaniline/golden nanometer particle compound substance, and be applied to biology sensor detection dopamine.The dopamine in solution effectively can be detected after graphene/polyaniline/golden nanometer particle compound substance is made modified electrode.Present invention also offers a kind of synthetic method of new graphene/polyaniline/golden nanometer particle compound substance, Graphene and aniline are mixed in hydrochloric acid solution, under certain conditions obtained graphene/polyaniline/golden nanometer particle compound substance.
Synthesizing graphite alkene/polyaniline/golden nanometer particle compound substance of the present invention and be applied to biology sensor detect dopamine, comprise the following steps:
A, prepare graphene/polyaniline/golden nanometer particle compound substance: by a certain amount of Graphene and aniline ultrasonic disperse in hydrochloric acid solution, tap funnel drips oxygenant.Mixed liquor is kept reacting at a certain temperature.Reaction terminate after by product centrifuging, and with absolute ethyl alcohol and distilled water washing, drying, obtain graphene/polyaniline/golden nanometer particle compound substance;
B, prepare graphene/polyaniline/golden nanometer particle compound substance modified electrode: graphene/polyaniline/golden nanometer particle composite wood gob is applied on glass-carbon electrode by obtained for step a, pipetting Nafion (0.5%) solution is again added drop-wise on modified electrode, comes off from electrode surface to prevent graphene/polyaniline/golden nanometer particle compound substance.Drying at room temperature, obtains graphene/polyaniline/golden nanometer particle compound substance modified electrode;
C, electrochemical process detect the DA in solution: preparation DA solution, and polyaniline/Graphene/golden nanometer particle compound substance modified electrode obtained in step b is carried out cyclic voltammetry experiment.Cyclic voltammetry experiment adopts three-electrode system, and wherein working electrode is polyaniline/Graphene/golden nanometer particle compound substance modified electrode, is platinum electrode to electrode, and contrast electrode is mercurous chloride electrode.
Further, in step a, the content of Graphene is 0 ~ 20%, and temperature of reaction is 0 ~ 5 DEG C, and the reaction time is 4 ~ 6h.
Further, in step a, oxygenant is gold chloride, and concentration is 1 ~ 10mM.Concentration 1 ~ the 10M of hydrochloric acid solution.
Further, the temperature of compound substance drying in step a is 40 ~ 60 DEG C, drying time 6 ~ 24h.
Further, in step b, drip composite wood doses 1 ~ 10 μ L, drip Nafion solution 1 ~ 10 μ L.
Further, the Concentration Testing scope 0.01 ~ 0.54mM of DA solution in step c.
The invention has the beneficial effects as follows: the preparation method of graphene/polyaniline/golden nanometer particle compound substance is simple and easy to do, preparation process is environment friendly and pollution-free, detecting DA in solution with this compound substance modified electrode, to have lower detectability, higher sensitivity, detection time short, easy and simple to handle, and the performance that recycles of material there has also been and significantly promotes compared with material in the past.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is further described.
In Fig. 1, curve is respectively cyclic voltammetric (CV) figure of (a) graphene/polyaniline/golden nanometer particle, (b) graphene/polyaniline, (c) polyaniline/golden nanometer particle and (d) polyaniline.
In Fig. 2, curve is respectively (a) graphene/polyaniline/golden nanometer particle, (b) graphene/polyaniline, (c) polyaniline/golden nanometer particle and (d) polyaniline CV figure in the mixed solution containing 1mM DA and 0.1M PBS (pH=7.0).The CV figure of (e) graphene/polyaniline/golden nanometer particle in 0.1M PBS (pH=7.0) solution.
In Fig. 3, curve is respectively (a) polyaniline/golden nanometer particle, (b) graphene/polyaniline/golden nanometer particle (containing 10% Graphene), (c) graphene/polyaniline/golden nanometer particle (containing 15% Graphene) and (d) graphene/polyaniline/golden nanometer particle (containing 20% Graphene) cyclic voltammetric (CV) figure in the mixed solution containing 1mM DA and 0.1M PBS (pH=7.0).
In Fig. 4, curve is respectively the time current curve that (A) graphene/polyaniline/golden nanometer particle compound substance modified electrode detects DA; (B) the linear relationship curve of DA concentration and peak current.
Fig. 5 curve is the chrono-amperometric response curve adding 0.2mmol/L UA, 0.2mmol/L AA and 0.2mmol/L DA under 0.4V voltage in the PBS buffer solution (pH=7.0) of 0.1M successively.
Embodiment
Embodiment one:
Prepare graphene/polyaniline/golden nanometer particle compound substance modified electrode and comprise following step:
(1) by 0.5mg/mL graphene dispersing solution, 25mM aniline adds in 0.5M hydrochloric acid solution successively, stirs 10min, gets the gold chloride (5mM) of 10mL; With tap funnel, chlorauric acid solution is slowly added drop-wise in Graphene and aniline mixed solution under stirring.After dropwising, temperature is kept to be 0 ~ 5 DEG C, Keep agitation, reaction 6h; Stop stirring, hold over night.Centrifuging, and with absolute ethyl alcohol and distilled water washing, obtain graphene/polyaniline/golden nanometer particle compound substance.Dry 24h at 60 DEG C, grinds for subsequent use.
(2) by products therefrom in 1.0g step (1), the dispersion liquid of 10mg/mL is mixed with.Get above-mentioned dispersion liquid 10 μ L to drip and be coated on glass-carbon electrode, after drying at room temperature, drip 10 μ L Nafion (0.5%) solution on surface, drying at room temperature, namely obtain graphene/polyaniline/golden nanometer particle compound substance modified electrode.
In Fig. 2, curve e is cyclic voltammetric (CV) figure of graphene/polyaniline/golden nanometer particle compound substance modified electrode in the phosphate buffered solution (PBS) of 0.1M pH=7.0, not redox peak.Therefore, the redox peak in Fig. 2 on curve a, b, c and d belongs to the redox of DA, and the oxidation peak occurred is that DA produces when being oxidized to quinoid structure.And the redox peak current of graphene/polyaniline/golden nanometer particle compound substance is the highest.The synergy of Graphene, polyaniline and golden nanometer particle defines larger conjugated system, facilitate the transfer rate of electronics between electrode and DA, the oxidation reaction of catalysis DA on electrode interface, considerably improves the sensitivity detected DA, shows excellent electro catalytic activity.
Embodiment two:
The preparation process of graphene/polyaniline/golden nanometer particle compound substance modified electrode is identical with embodiment one.
Graphene/polyaniline/golden nanometer particle compound substance the modified electrode of preparation is under 0.4V current potential, and in the PBS (pH=7.0) constantly stirred, add the DA of variable concentrations continuously, minute-current curve, as Fig. 4 A.Fig. 4 B is the concentration of DA and the linear relationship curve of peak current.As can be seen from Fig. 4 B, when concentration is 0.01 ~ 0.54mM, current-responsive and DA concentration are that two-wire shape is relevant, are y=0.0186 × x+0.1332 at the linearity curve of low concentration (0.01 ~ 0.08mM), its coefficient R
2=0.9969, be y=0.0061 × x+1.0940 at the linearity curve of high concentration (0.08 ~ 0.54mM), its coefficient R
2=0.9998, the detection of this biology sensor is limited to 1.345 μMs (S/N=3).
Embodiment three:
The preparation process of graphene/polyaniline/golden nanometer particle compound substance modified electrode is identical with embodiment one.
Antijamming capability is one of important parameter of biology sensor.In this work, select uric acid (UA), ascorbic acid (AA) as chaff interference.Fig. 5 is the chrono-amperometric response curve that graphene/polyaniline/golden nanometer particle compound substance modified electrode adds 0.2mmol/L UA, 0.2mmol/L AA and 0.2mmol/L DA successively in the PBS buffer solution (pH=7.0) of 0.1M.Obviously can see, add UA, AA and do not cause current-responsive, and after adding DA, have obvious response current, illustrate that UA, AA detect DA for graphene/polyaniline/golden nanometer particle compound substance modified electrode and do not have interference effect.Also study for the stability of graphene/polyaniline/golden nanometer particle compound substance modified electrode detection DA herein.Use same modified electrode to the DA solution replicate determination 5 times of 1mM, relative standard deviation (RSD) is 2.33%, illustrates that this compound substance modified electrode has good stability.
Comparative example one:
Prepare grapheme/polyaniline composite material modified electrode, preparation process is as follows:
(1) by 0.5mg/mL graphene dispersing solution, 25mM aniline adds in 0.5M hydrochloric acid solution successively, stirs 10min, gets the Iron(III) chloride hexahydrate of 10mL 0.1M; With tap funnel, Iron(III) chloride hexahydrate solution is slowly added drop-wise in Graphene, aniline mixed solution under stirring.After dropwising, temperature is kept to be 0 ~ 5 DEG C, Keep agitation, reaction 6h; Stop stirring, hold over night.Centrifuging, and with absolute ethyl alcohol and distilled water washing, obtain grapheme/polyaniline composite material.Dry 24h at 60 DEG C, grinds for subsequent use.
(2) by products therefrom in 1.0g step (1), the dispersion liquid of 10mg/mL is mixed with.Get above-mentioned dispersion liquid 10 μ L, drip and be coated on glass-carbon electrode, after drying at room temperature, drip 10 μ L Nafion (0.5%) solution on surface, drying at room temperature, namely obtains grapheme/polyaniline composite material modified electrode.
The mixed solution that the grapheme/polyaniline composite material modified electrode prepared is used for 1mM DA and 0.1M PBS (pH=7.0) carries out cyclic voltammetry experiment, and sweep speed is 50mV/s.Can find out in Fig. 2 that the detection response of this compound substance modified electrode (curve b) to dopamine in solution is lower than graphene/polyaniline/(curve a) for golden nanometer particle compound substance modified electrode.
Comparative example two:
Prepare polyaniline/golden nanometer particle compound substance modified electrode, preparation process is as follows:
(1) 25mM aniline adds in 0.5M hydrochloric acid solution successively, stirs 10min, gets the gold chloride of 10mL 0.1M; With tap funnel, chlorauric acid solution is slowly added drop-wise in aniline solution under stirring.After dropwising, temperature is kept to be 0 ~ 5 DEG C, Keep agitation, reaction 6h; Stop stirring, hold over night.Centrifuging, and with absolute ethyl alcohol and distilled water washing, obtain polyaniline/golden nanometer particle compound substance.Dry 24h at 60 DEG C, grinds for subsequent use.
(2) by products therefrom in 1.0g step (1), the dispersion liquid of 10mg/mL is mixed with.Get above-mentioned dispersion liquid 10 μ L, drip and be coated on glass-carbon electrode, after drying at room temperature, drip 10 μ L Nafion (0.5%) solution on surface, drying at room temperature, namely obtain polyaniline/golden nanometer particle compound substance modified electrode.
The mixed solution that the polyaniline/golden nanometer particle compound substance modified electrode prepared is used for 1mM DA and 0.1M PBS (pH=7.0) carries out cyclic voltammetry experiment, and sweep speed is 50mV/s.Can find out in Fig. 2 that the detection response of this compound substance modified electrode (curve c) to DA in solution is lower than graphene/polyaniline/(curve a) for golden nanometer particle compound substance modified electrode.
Comparative example three:
Prepare polyaniline modified electrode, preparation process is as follows:
(1) 25mM aniline is added in 0.5M hydrochloric acid solution, stir 10min, get the Iron(III) chloride hexahydrate of 10mL 0.1M.After dropwising, temperature is kept to be 0 ~ 5 DEG C, Keep agitation, reaction 6h; Stop stirring, hold over night.Centrifuging, and with absolute ethyl alcohol and distilled water washing, obtain polyaniline material.Dry 24h at 60 DEG C, grinds for subsequent use.
(2) by gained modified electrode in 1.0g step (1), drip 10 μ L Nafion (0.5%) solution on its surface, drying at room temperature, namely obtains polyaniline modified electrode.
The mixed solution that the polyaniline modified electrode prepared is used for 1mM DA and 0.1M PBS (pH=7.0) carries out cyclic voltammetry experiment, sweep speed is can find out this modified electrode in 50mV/s, Fig. 2 to the detection response curve d of dopamine in solution lower than graphene/polyaniline/(curve a) for golden nanometer particle compound substance modified electrode.
The present invention with Graphene, aniline and gold chloride for raw material, obtained graphene/polyaniline/golden nanometer particle compound substance, this method preparation process is simple, reaction temperature and.Drip Nafion solution at material surface, make graphene/polyaniline/golden nanometer particle compound substance modified electrode, this modified electrode has excellent performance to the detection of dopamine in solution.
Claims (7)
1. synthesizing graphite alkene/polyaniline/golden nanometer particle compound substance and be applied to detect dopamine (DA), it is characterized in that: step is as follows:
A, prepare graphene/polyaniline/golden nanometer particle compound substance: add in hydrochloric acid solution by the graphene dispersing solution after ultrasonic and aniline, stir 5 ~ 30min, with separating funnel, chlorauric acid solution is slowly added drop-wise in Graphene, aniline mixed solution under stirring.After dropwising, temperature is kept to be 0 ~ 5 DEG C, Keep agitation, reaction 4 ~ 6h; Stop stirring, hold over night.Centrifuging, and with absolute ethyl alcohol and deionized water washing, obtain graphene/polyaniline/golden nanometer particle compound substance.At 60 DEG C, dry 6 ~ 24h, grinds for subsequent use;
B, prepare graphene/polyaniline/golden nanometer particle compound substance modified electrode: the graphene/polyaniline/golden nanometer particle compound substance in deionized water ultrasonic disperse obtained by step a, is mixed with dispersion liquid.Get above-mentioned dispersion liquid 5 ~ 20 μ L, dripping is coated on glass-carbon electrode, after drying at room temperature, the Nafion solution (0.5%) of 5 ~ 20 μ L is dripped on surface, come off from electrode surface to prevent graphene/polyaniline/golden nanometer particle compound substance, drying at room temperature, namely obtains graphene/polyaniline/golden nanometer particle compound substance modified electrode;
C, cyclic voltammetry detect dopamine: preparation dopamine solution, and graphene/polyaniline/golden nanometer particle compound substance modified electrode obtained in step b is carried out cyclic voltammetry experiment.Cyclic voltammetry detects dopamine experiment and adopts three-electrode system, and wherein working electrode is graphene/polyaniline/golden nanometer particle compound substance modified electrode, is platinum plate electrode to electrode, and contrast electrode is mercurous chloride electrode.
2. synthesizing graphite alkene/polyaniline/golden nanometer particle compound substance and be applied to detection dopamine according to claim 1, it is characterized in that: Graphene content (0 ~ 20%) in graphene/polyaniline/golden nanometer particle in described step a, temperature of reaction is 0 ~ 5 DEG C, and the reaction time is 4 ~ 6h.
3. synthesizing graphite alkene/polyaniline/golden nanometer particle compound substance and be applied to detection dopamine according to claim 1, it is characterized in that: in described step a, oxygenant is gold chloride, reductive agent is aniline, and oxidant concentration is 1 ~ 10mmol/L.Concentration of hydrochloric acid is 1 ~ 10M.
4. synthesizing graphite alkene/polyaniline/golden nanometer particle compound substance and be applied to detection dopamine according to claim 1, is characterized in that: the temperature of compound substance drying in step a be 40 ~ 60 DEG C drying time 6 ~ 24h.
5. synthesizing graphite alkene/polyaniline/golden nanometer particle compound substance and be applied to detection dopamine according to claim 1, is characterized in that: drip composite wood doses 1 ~ 10 μ L in step b, drips Nafion amount of solution 1 ~ 10 μ L.
6. synthesizing graphite alkene/polyaniline/golden nanometer particle compound substance and be applied to detection dopamine according to claim 1, is characterized in that: the detectable concentration scope 0.01 ~ 0.54mM of DA solution in step c.
7. synthesizing graphite alkene/polyaniline/golden nanometer particle compound substance and be applied to detection dopamine according to claim 1, is characterized in that: detecting dopamine in described step c is graphene/polyaniline/golden nanometer particle compound substance modified electrode.
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| CN113004541A (en) * | 2021-02-10 | 2021-06-22 | 陕西省石油化工研究设计院 | Method for preparing graphene oxide-polyaniline-gold nanoparticle solution |
| CN113406171A (en) * | 2021-05-27 | 2021-09-17 | 华南理工大学 | Composite electrode and preparation method and application thereof |
| CN114441494A (en) * | 2022-01-28 | 2022-05-06 | 常州大学 | Fluorescent detection method for sulfhydryl compound and uric acid by pH regulation |
| CN116879368A (en) * | 2023-09-06 | 2023-10-13 | 深圳市深水兆业工程顾问有限公司 | Electrochemical sensor and preparation method and application thereof |
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