CN109164093A - A kind of preparation method for the Au nano particle detecting dopamine - Google Patents

A kind of preparation method for the Au nano particle detecting dopamine Download PDF

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Publication number
CN109164093A
CN109164093A CN201810851312.1A CN201810851312A CN109164093A CN 109164093 A CN109164093 A CN 109164093A CN 201810851312 A CN201810851312 A CN 201810851312A CN 109164093 A CN109164093 A CN 109164093A
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nano particle
dopamine
detecting dopamine
solution
added
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王毅
张学铭
张新娟
陈进剑
张庆文
赵若鹏
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WENZHOU BIOMEDICAL MATERIALS AND ENGINEERING RESEARCH INSTITUTE
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WENZHOU BIOMEDICAL MATERIALS AND ENGINEERING RESEARCH INSTITUTE
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65Raman scattering
    • G01N21/658Raman scattering enhancement Raman, e.g. surface plasmons

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
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Abstract

The invention discloses a kind of preparation methods of Au nano particle for detecting dopamine, and include the following steps to obtain: step 1: taking chlorauric acid solution, is put into round-bottomed flask, is heated, until liquid boiling;Step 2: taking sodium citrate to be added in the boiling solution in step 1, continues heating stirring, is cooled to room temperature is cooled to room temperature to temperature later, obtains Au nanoparticles solution;Step 3: Au nanoparticles solution addition sulfhydryl compound and two thiobis succinimidyl propionates is taken to be sufficiently stirred;Step 4: being added solvent and boronic acid compounds sustained response obtains the Au nano particle of surface modification.The Au nano particle obtained after being surface modified to Au nano particle can be special combination dopamine, formed aggregation, generate color change, dopamine can be measured by colorimetric method and Raman spectrum.

Description

A kind of preparation method for the Au nano particle detecting dopamine
Technical field
Field of nanometer material technology, the preparation method of the Au nano particle of specifically a kind of detection dopamine.
Background technique
Dopamine belongs to Catecholamines Neurotransmitters in Blood, has different degrees of distribution in nervous centralis and periphery, is people One of most important neurotransmitter of body.Its content distribution of specific region in human brain affects the association of hypophysis endocrine dysfunction It adjusts, and directly related with nervous activity.Numerous zooperies and human research have proven to dopamine and its receptor and human body A variety of diseases, such as schizophrenia, pharmacological dependence and habituation, Parkinson's disease, hypertension, hepatic encephalopathy and dopa reaction flesh Power obstacle has close relationship, and in a variety of digestion such as gastrointestinal motility, gastric acid secretion, the oxygen supply of Gastric Mucosa Blood Flow, tumours Important regulative is played in tract disease.Furthermore dopamine also has the function of excited heart, increases renal blood flow, for treating Ischemic, cardiogenic and infectious shock.Therefore, the research for carrying out dopamine analysis method is examined in nervous physiology function, disease Disconnected and related drugs quality controls etc. important in inhibiting.In recent years, the detection method of dopamine mainly has electrochemistry Method, chemiluminescence, chemoluminescence method, spectrophotometry and liquid chromatography etc..But due to brain mechanism and substance group At complex, these methods can not carry out precisely single measurement to the dopamine in brain system.
Summary of the invention
It, can specificity in view of the deficiencies of the prior art, the present invention intends to provide a kind of Au nano particle Combination dopamine in ground forms aggregation, generates corresponding color change, can be detected by colorimetric method to dopamine.
To achieve the above object, the present invention provides the following technical scheme that
A kind of preparation method for the Au nano particle detecting dopamine,
Include the following steps to obtain:
Step 1: taking chlorauric acid solution, is put into round-bottomed flask, is heated, until liquid boiling;
Step 2: taking sodium citrate to be added in the boiling solution in step 1, continues heating stirring, is cooled to room temperature later It is cooled to room temperature to temperature, obtains Au nanoparticles solution;
Step 3: Au nanoparticles solution addition sulfhydryl compound and two thiobis succinimidyl propionates is taken sufficiently to stir It mixes;
Step 4: being added solvent and boronic acid compounds sustained response obtains the Au nano particle of surface modification.
As a further improvement of the present invention:
The sulfhydryl compound is 4- mercaptophenyl boric acid or Mercamine Cysteamine or mercaptopropionic acid.
As a further improvement of the present invention:
The boronic acid compounds are 4- nitrobenzene boronic acid or 4- brombutyl boric acid.
As a further improvement of the present invention:
The molar ratio of gold chloride and step 2 sodium citrate is 1~200: 1~500 in the step 1.
As a further improvement of the present invention:
Sulfhydryl compound and two thiobis succinimidyl propionate molar ratios are 1~25: 1~200. in the step 3
As a further improvement of the present invention:
The molar ratio of the boronic acid compounds in sulfhydryl compound and step 4 in the step 3 is 1~25: 20~50.
As a further improvement of the present invention:
After sodium citrate is added in the step 2, solution becomes claret, continues 1~60min of heating stirring.
As a further improvement of the present invention:
Mixing time is 0.1~5 hour in the step 3.
As a further improvement of the present invention:
20 DEG C are heated to after boronic acid compounds are added in the step 4, the reaction was continued 2~48 hours.
It can be in micromolar level to the dopamine molecule colorimetric visual analyzing of intracerebral using Au nano particle.It should The characteristics of method has directly, high specific and high sensitivity, and it is theoretical more simple, and technical operation requirement is low, implementable Property it is high.It is generated during plasmon coupling or Au aggregates of nanoparticles redisperse between particle during Au nanoparticle aggregate The colorimetric method of color change have been used for detecting various targets, including nucleic acid, protein, small molecule and metal ion.
In addition, Raman spectrum analysis technology is the molecular structure characterization technology set up based on Ramam effect, it Identical as infrared spectroscopy, signal derives from the vibration and rotation of molecule, is that molecular polarizability variation induction generates, its spectrum Line intensity depends on the size of polarizability variation during corresponding normal mode vibration, and provided structural information is about intramolecular The case where various normal mode vibration frequencies in portion and related vibration level, so as to be used to identify functional group present in molecule.Table Face enhancing Raman scattering refers to that in the metal good conductor surface of some special preparations or colloidal sol, Raman scattering signal is drawn than common The phenomenon that graceful scattered signal intensity increases, it is a kind of enhancing effectiveness with surface selectivity.
The Au nano particle obtained after being surface modified to Au nano particle can be special combination dopamine, formed poly- Collective generates color change, can be measured to dopamine by colorimetric method.Meanwhile gap or the connection of Au nano particle Place will appear the enhancing of field strength, and the Raman signal of group is significantly enhanced, to realize that surface-enhanced Raman detects DOPA Amine content.
Detailed description of the invention
Fig. 1 is the UV-Vis absorption spectrum after Au nano particle is reacted with the dopamine of various concentration;
Fig. 2 is the raman scattering spectrum that Au nano particle reacts front and back with 9 μM of dopamine.
Specific embodiment
The present invention is described in further detail below in conjunction with embodiment given by attached drawing.
Case study on implementation 1
Firstly, measuring the chlorauric acid solution of 50ml 1mM, it is put into round-bottomed flask, is heated in oil bath pan, until liquid Body boiling.
It measures 5ml 38.8mM sodium citrate to be added in the solution of boiling, solution becomes claret at once, continues heating and stirs Mix 20min.It is cooled to room temperature to temperature, obtains Au nanoparticles solution.
Measure 10mlAu nanoparticles solution, 20 μ l 1mM 4- mercaptophenyl boric acid, 40 μ l 0.49mM, bis- thiobis amber Amber propionates are added to the container, and are stirred 2h, are mixed well liquid.The Au that acquisition can specifically bind dopamine receives Rice material.
Case study on implementation 2
Firstly, measure 4ml 25mM chlorauric acid solution and 96ml ultrapure water, be put into round-bottomed flask, in oil bath pan into Row heating, until liquid boiling.
It measures 10ml 38.8mM sodium citrate to be added in the solution of boiling, solution becomes claret at once, continues heating and stirs Mix 25min.It is cooled to room temperature to temperature, obtains Au nanoparticles solution.
Measure 20mlAu nanoparticles solution, 40 μ l 1mM Mercamine Cysteamines, 160 μ l 0.49mM, bis- thiobis succinyl Imines propionic ester is added to the container, and is stirred 2h, is mixed well liquid.
20ml ultrapure water and 388 μ l 1mM 4- brombutyl boric acid are measured, for 24 hours, acquisition can be specifically bound for 80 DEG C of reactions The Au nano material of dopamine.
Case study on implementation 3
Firstly, measuring the chlorauric acid solution of 40ml 1mM, it is put into round-bottomed flask, is heated in oil bath pan, until liquid Body boiling.
It measures 4ml 38.8mM sodium citrate to be added in the solution of boiling, solution becomes claret at once, continues heating and stirs Mix 30min.It is cooled to room temperature to temperature, obtains Au nanoparticles solution.
Measure 20mlAu nanoparticles solution, 40 μ l 1mM mercaptopropionic acids, the thio double amber imide of 80 μ l 0.49mM bis- Propionic ester is added to the container, and is stirred 2h, is mixed well liquid.
Measuring 20ml ultrapure water and 388 μ l 1mM 4- nitrobenzene boronic acids, 80 DEG C of reaction 20h, acquisition can specifically bind The Au nano material of dopamine.
Test 1:
Measure the Au nano particle in 2ml embodiment, respectively be 12 μM with concentration, 9 μM, 6 μM, 3 μM of dopamine it is molten Liquid carries out reaction observation color.
0 3μM 6μM 9μM 12μM
Embodiment 1 Claret Peony Aubergine Hyacinthine Atropurpureus
Embodiment 2 Claret Peony Aubergine Hyacinthine Atropurpureus
Embodiment 3 Claret Peony Aubergine Hyacinthine Atropurpureus
After dopamine is added in prepared Au nano particle, color becomes hyacinthine from red, and with DOPA The increase of amine content, color are successively deepened.Illustrate, Au nano material can be chemically reacted with dopamine.
Test 2: using UV, visible light-near infrared spectrometer, in the wave-length coverage of 400-900nm after measurement reaction UV-Vis absorption spectrum.
Referring to Fig.1, Au nano particle can produce with the dopamine that concentration is 6 μM and react, and can produce at the wavelength of 650nm Raw absorption peak.With the enhancing of dopamine concentration, absorption peak strength enhancing.Illustrate, enhance with dopamine concentration, Au nano particle with The reaction of dopamine also enhances, which has good sensitivity.
Test 3: with the Au nano particle in embodiment 1, using laser Raman spectrometer under continuous scanning mode, measurement 600-2800cm-1Raman spectrum after Au nano particle is reacted with 0 μM, 9 μM of dopamine in range.
Referring to Fig. 2, Au nano particle has the Raman spectrum of 3 characteristic peaks, and and concentration after reacting with dopamine The intensity value for reacting postpeak for 9 μM of dopamines is larger.
It can be in micromolar level to the dopamine molecule colorimetric visual analyzing of intracerebral using Au nano particle.It should The characteristics of method has directly, high specific and high sensitivity, and it is theoretical more simple, and technical operation requirement is low, implementable Property it is high.It is generated during plasmon coupling or Au aggregates of nanoparticles redisperse between particle during Au nanoparticle aggregate The colorimetric method of color change have been used for detecting various targets, including nucleic acid, protein, small molecule and metal ion.
In addition, Raman spectrum analysis technology is the molecular structure characterization technology set up based on Ramam effect, it Similar with infrared spectroscopy, signal derives from the vibration and rotation of molecule, is that molecular polarizability variation induction generates, its spectrum Line intensity depends on the size of polarizability variation during corresponding normal mode vibration, and provided structural information is about intramolecular The case where various normal mode vibration frequencies in portion and related vibration level, so as to be used to identify functional group present in molecule.Table Face enhancing Raman scattering refers to that in the metal good conductor surface of some special preparations or colloidal sol, Raman scattering signal is drawn than common The phenomenon that graceful scattered signal intensity increases, it is a kind of enhancing effectiveness with surface selectivity.
The Au nano particle obtained after being surface modified to Au nano particle can be special combination dopamine, formed poly- Collective generates color change, can be measured to dopamine by colorimetric method.Meanwhile gap or the connection of Au nano particle Place will appear the enhancing of field strength, and the Raman signal of group is significantly enhanced, to realize that surface-enhanced Raman detects DOPA Amine content.
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation Example, all technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for the art Those of ordinary skill for, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications It should be regarded as protection scope of the present invention.

Claims (9)

1. a kind of preparation method for the Au nano particle for detecting dopamine, it is characterised in that:
Include the following steps to obtain:
Step 1: taking chlorauric acid solution, is put into round-bottomed flask, is heated, until liquid boiling;
Step 2: taking sodium citrate to be added in the boiling solution in step 1, continues heating stirring, is cooled to room temperature later to temperature Degree is cooled to room temperature, and obtains Au nanoparticles solution;
Step 3: Au nanoparticles solution addition sulfhydryl compound and two thiobis succinimidyl propionates is taken to be sufficiently stirred;
Step 4: being added solvent and boronic acid compounds sustained response obtains the Au nano particle of surface modification.
2. a kind of Au nano particle for detecting dopamine according to claim 1, it is characterised in that:
The sulfhydryl compound is the one or more of 4- mercaptophenyl boric acid or Mercamine Cysteamine or mercaptopropionic acid.
3. a kind of Au nano particle for detecting dopamine according to claim 1, it is characterised in that:
The boronic acid compounds are the one or more of 4- nitrobenzene boronic acid or 4- brombutyl boric acid.
4. a kind of Au nano particle for detecting dopamine according to claim 1, it is characterised in that:
The molar ratio of gold chloride and step 2 sodium citrate is 1~200:1~500 in the step 1.
5. a kind of Au nano particle for detecting dopamine according to claim 1, it is characterised in that:
Sulfhydryl compound and two thiobis succinimidyl propionate molar ratios are 1~25:1~200 in the step 3.
6. a kind of Au nano particle for detecting dopamine according to claim 1 or 5, it is characterised in that:
The molar ratio of the boronic acid compounds in sulfhydryl compound and step 4 in the step 3 is 1~25:20~50.
7. a kind of Au nano particle for detecting dopamine according to claim 1, it is characterised in that:
After sodium citrate is added in the step 2, solution becomes claret, continues 1~60min of heating stirring.
8. a kind of Au nano particle for detecting dopamine according to claim 1, it is characterised in that:
Mixing time is 0.1~5 hour in the step 3.
9. a kind of Au nano particle for detecting dopamine according to claim 1, it is characterised in that:
20 DEG C are heated to after boronic acid compounds are added in the step 4, the reaction was continued 2~48 hours.
CN201810851312.1A 2018-07-27 2018-07-27 A kind of preparation method for the Au nano particle detecting dopamine Pending CN109164093A (en)

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CN112569974A (en) * 2019-09-27 2021-03-30 北华大学 Gold-polyacid catalyst for chromogenic detection of dopamine and preparation method thereof
CN113340867A (en) * 2021-04-28 2021-09-03 华南师范大学 Method for detecting tyrosinase by using colorimetric-SERS double-readout sensor

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CN112569974B (en) * 2019-09-27 2023-05-23 北华大学 Gold-polyacid catalyst for color development detection of dopamine and preparation method thereof
CN113340867A (en) * 2021-04-28 2021-09-03 华南师范大学 Method for detecting tyrosinase by using colorimetric-SERS double-readout sensor
CN113340867B (en) * 2021-04-28 2022-03-29 华南师范大学 Method for detecting tyrosinase by using colorimetric-SERS double-readout sensor

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Application publication date: 20190108