CN110538325A - Precious metal nanoparticle/g-C3N 4 composite material, preparation method and application - Google Patents
Precious metal nanoparticle/g-C3N 4 composite material, preparation method and application Download PDFInfo
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- CN110538325A CN110538325A CN201910592367.XA CN201910592367A CN110538325A CN 110538325 A CN110538325 A CN 110538325A CN 201910592367 A CN201910592367 A CN 201910592367A CN 110538325 A CN110538325 A CN 110538325A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K41/00—Medicinal preparations obtained by treating materials with wave energy or particle radiation ; Therapies using these preparations
- A61K41/0057—Photodynamic therapy with a photosensitizer, i.e. agent able to produce reactive oxygen species upon exposure to light or radiation, e.g. UV or visible light; photocleavage of nucleic acids with an agent
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- A—HUMAN NECESSITIES
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- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P25/00—Drugs for disorders of the nervous system
- A61P25/14—Drugs for disorders of the nervous system for treating abnormal movements, e.g. chorea, dyskinesia
- A61P25/16—Anti-Parkinson drugs
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P25/00—Drugs for disorders of the nervous system
- A61P25/28—Drugs for disorders of the nervous system for treating neurodegenerative disorders of the central nervous system, e.g. nootropic agents, cognition enhancers, drugs for treating Alzheimer's disease or other forms of dementia
Abstract
The invention provides a noble metal nanoparticle/g-C3N 4 composite material, a preparation method and application, noble metal is loaded on the surface of g-C3N4, and the noble metal nanoparticle has stronger plasma resonance characteristic and can capture and store generated free electrons, so that the service life of plasmas locally generated is prolonged, and the photocatalytic capacity of graphitic carbonitride (g-C3N4) is improved. Can be used for degrading amyloid aggregates and further treating diseases caused by the amyloid aggregates; the preparation of the medicine for treating diseases caused by amyloid aggregates can also be used for degrading rhodamine.
Description
Technical Field
The invention relates to the technical field of biomedical materials, in particular to a noble metal nanoparticle/g-C3N 4 composite material, a preparation method and application.
Background
The high incidence of amyloidosis-associated diseases, represented by alzheimer's disease, and the inability to completely treat them have received much attention. Based on the existing studies, many amyloidosis such as type II diabetes, Alzheimer's Disease (AD), Parkinson's Disease, etc. are caused by amyloid (polypeptide) misfolding and abnormal self-assembly aggregation. The amyloid protein (polypeptide) aggregation fiber tangle in a patient is one of the characteristics of diseases, the self-assembly aggregation and protein fiber formation process of the amyloid protein (polypeptide) is the process of abnormally aggregating the amyloid protein (polypeptide) from soluble and unstructured protein monomers into insoluble amyloid protein fibers rich in beta-sheet structures, the amyloid protein fibers (such as the amyloid protein in a type II diabetic patient) in the patient cannot be cleared timely, and the fiber tangle formed by mass deposition causes the damage of tissue functions.
Therefore, the inhibitor and the method which can reduce, inhibit and even reverse amyloid aggregation fibers rich in beta-sheet structures have wide application prospects in the aspects of pathogenesis research and potential treatment.
Many inhibitors have been used to regulate the formation of amyloid (polypeptide) fibrosis, such as carbon nanotubes and Graphene Oxide (GO). These inhibitors are believed to inhibit the aggregation process of amyloid (polypeptide) monomers, but most inhibitors do not break down aggregated protein fibrillar aggregates. In addition, although various enzymes including neprilysin, insulin-degrading enzyme and endothelin-converting enzyme have the ability to degrade amyloid a β (33-42) monomer, the above enzymes are not sensitive to more cytotoxic oligomers of amyloid (polypeptide), and are difficult to be applied to large-scale disease treatment due to the influence of various factors. Therefore, the development of a novel amyloid aggregation inhibitor for inhibiting and even eliminating aggregates degrading amyloid has great scientific research significance and social and economic values.
Disclosure of Invention
aiming at the defects in the prior art, the invention provides a noble metal nanoparticle/g-C3N 4 composite material, a preparation method and application thereof, wherein the noble metal nanoparticle/g-C3N 4 composite material can degrade amyloid aggregates under the condition of illumination, and provides a new treatment method for diseases caused by amyloid fibers.
The present invention achieves the above-described object by the following technical means.
A preparation method of a noble metal nanoparticle/g-C3N 4 composite material is characterized by comprising the following steps:
(1) Preparation of ultrathin g-C3N4 nanosheets: preparing a block g-C3N4 by treating melamine at high temperature, and peeling g-C3N4 in liquid to obtain a g-C3N4 nanosheet;
(2) preparing a noble metal nano particle/g-C3N 4 composite material:
Firstly, preparing a noble metal reduction reaction solution, adding the prepared g-C3N4 nanosheet into the solution, stirring, fixing the reduced Au on the g-C3N4 nanosheet to prepare a noble metal nanoparticle/g-C3N 4 composite material, filtering, washing and drying under K393 overnight.
Further, the noble metal reduction reaction solution was a gold reduction reaction solution, HAuCl4 was dissolved in a polyvinyl alcohol solution, a newly prepared NaBH4 solution was added to the HAuCl4 solution, and incubated at room temperature for 30 minutes.
Further, the specific steps for preparing the block g-C3N4 are as follows: the melamine was heated to 600 ℃ at a ramp rate of 3 ℃/min and held for 2 hours to give a yellow product as g-C3N 4.
Further, the specific steps of peeling g-C3N4 in the liquid to obtain g-C3N4 nanosheets are as follows: dispersing g-C3N4 powder in water and then sonicating for about 16 hours; the resulting suspension was then centrifuged at about 5000rpm to remove the residual unexfoliated g-C3N4 bulk to obtain g-C3N4 nanoplates.
the noble metal nano particle/g-C3N 4 composite material is prepared by the preparation method of the noble metal nano particle/g-C3N 4 composite material.
Further, the noble metal nanoparticles in the noble metal nanoparticle/g-C3N 4 composite material are gold nanoparticles.
the noble metal nanoparticle/g-C3N 4 composite material is used for degrading amyloid aggregates, and is characterized in that Au/g-C3N4 degrades the amyloid aggregates under the condition of light.
Further, the light source is ultraviolet light.
The noble metal nano particle/g-C3N 4 composite material is used for preparing a medicine for treating diseases caused by amyloid aggregate.
The noble metal nano particle/g-C3N 4 composite material is used for degrading rhodamine.
According to the invention, precious metal is loaded on the surface of g-C3N4, such as Au and Pt, precious metal nanoparticles have stronger plasma resonance characteristics, can capture and store generated free electrons, thus prolonging the service life of plasmas generated locally, and the photocatalysis capability of graphitic carbonitride (g-C3N4) is improved by modifying carbon nitride nanomaterial (g-C3N4) through precious metal nanoparticles. In the current medical science and technology, photo-thermal treatment and Photodynamic Therapy (PDT) research have precedent; in fact, medical personnel can perform treatment related to tumors by irradiating light through human tissues in a directional manner, and scientific research is largely and widely used at present. The noble metal nano particle/g-C3N 4 composite material is used for degrading amyloid aggregates, and the specific application mode can adopt PDT therapy.
The noble metal nano particle/g-C3N 4 composite material can effectively degrade amyloid aggregates so as to eradicate existing amyloid aggregates in a patient body; thereby treating diseases caused by amyloid aggregates.
Drawings
FIG. 1 is an XRD pattern of Au/g-C3N4 prepared according to the present invention.
FIG. 2 is a TEM image of Au/g-C3N4 prepared according to the present invention.
In FIG. 3, (a) and (b) are respectively the infrared spectrum and ultraviolet spectrum of Au/g-C3N4 prepared by the present invention.
In FIG. 4, (a) and (b) are absorption peaks of rhodamine in the degradation process of the C3N4 and Au/g-C3N4 materials for rhodamine, respectively.
FIG. 5 is an AFM height map of the morphology of the positive control and degraded product of Amylin (20-29), wherein (a) is the positive control of Amylin (20-29) and (d) is the morphology of the aggregate of degraded Amylin (20-29).
FIG. 6: amylin (20-29) was detected by Circular Dichroism (CD) degradation under different conditions.
FIG. 7: the degradation of the Amylin (20-29) aggregates by irradiation with Au/g-C3N4 was detected using a Quartz Crystal Microbalance (QCM).
Detailed Description
The invention will be further described with reference to the following figures and specific examples, without limiting the scope of the invention.
The preparation method of the noble metal nano particle/g-C3N 4 composite material comprises the following steps:
(1) Preparation of ultrathin g-C3N4 nanosheets: preparing a block g-C3N4 by treating melamine at high temperature, and peeling g-C3N4 in liquid to obtain a g-C3N4 nanosheet;
(2) Preparing a noble metal nano particle/g-C3N 4 composite material:
firstly, preparing a noble metal reduction reaction solution, adding the prepared g-C3N4 nanosheet into the solution, stirring, fixing the reduced Au on the g-C3N4 nanosheet to prepare a noble metal nanoparticle/g-C3N 4 composite material, filtering, washing and drying under K393 overnight.
Taking gold nanoparticles/g-C3N 4 composite material as an example, the preparation method is as follows:
Heating melamine to 600 ℃ for 2 hours at a heating rate of 3 ℃/min; the yellow product obtained was g-C3N 4. Dispersing 100mg or a large amount of g-C3N4 powder in 100mL of water, followed by sonication for about 16 hours; the resulting suspension was then centrifuged at about 5000rpm to remove the residual unsplit g-C3N4 bulk to obtain g-C3N4 nanoplatelets. HAuCl4 was dissolved in 7mL of a polyvinyl alcohol (1%) solution at a concentration of 1.5 mmol/L. Next, 7mL of freshly prepared, 0.1mol/L NaBH4 solution was added to the HAuCl4 solution at a final molar ratio of 1:3 and incubated at room temperature for 30 minutes. 5g of g-C3N4 nanosheets prepared above were added to the above mixed solution of HAuCl4 and NaBH4 and stirred for 2 hours. The prepared Au/g-C3N4 was then filtered, washed and prepared to dry overnight at 393K.
Au/g-C3N4 nanocomposites were characterized by XRD, TEM, FTIR and UV-Vis diffuse reflectance spectroscopy (UV-Vis DRS).
The XRD pattern of the prepared Au/g-C3N4 is shown in figure 1, and the diffraction peaks in figure 1 prove the structural identity and phase composition of the prepared Au/g-C3N 4. The XRD patterns of Au/g-C3N4 nanocomposite and pure g-C3N4 showed three typical peaks at 38, 44 and 64 ° 2 θ, expressed as face-centered cubic (111), (200) and (220) planes. Except for two different g-C3N4 peaks at 12 and 27 deg.. FTIR spectra of Au/g-C3N4 and g-C3N4 observed a broad band of about 3200-3500cm-1 and several strong bands in the range of 1200-1650cm-1 due to the NH stretching and typical stretching modes of the CN heterocycles.
FIG. 2 is a TEM image of the prepared Au/g-C3N4, the TEM showing a lamellar structure with gray areas corresponding to g-C3N4 and dark spots for Au nanoparticles. According to TEM images, the diameter of Au particles on the surface of g-C3N4 is in the range of 12-20 nm. The Au/g-C3N4 prepared by the invention has a single-layer or multi-layer super-Bo structure.
In FIG. 3, (a) and (b) are respectively the infrared spectrum characterization and the ultraviolet spectrum characterization of Au/g-C3N4 prepared by the invention, and the characteristic signals in the graph prove that the gold nanoparticles deposited on the g-C3N4 sample show enhanced absorption of visible light.
Example 1: degrading organic molecule rhodamine
We measured the ability of 1mg/mL Au/g-C3N4 to degrade 0.1g/L rhodamine B (RhB) under UV irradiation, and used C3N4 as a control. The degradation effect is shown in FIG. 4, as the illumination duration is increased, the rhodamine absorption peak gradually disappears, and the g-C3N4 material loaded with the Au nanoparticles completely degrades rhodamine B (RhB) within 1 hour.
FIG. 4 is a comparison of experiments for degrading rhodamine by C3N4 and Au/g-C3N4 materials, (a) analyzing the degradation process by ultraviolet absorption spectrum; (b) the absorption spectrum is at 555 nm. And (3) characterizing the effect difference of degrading rhodamine by Au/g-C3N4 and g-C3N4 by using an ultraviolet absorption spectrum. After 60 minutes of degradation, the rate of Au/g-C3N4 of the former is improved by 10 percent compared with the rate of g-C3N 4.
Example 2: degradation of amyloid (polypeptide) and its aggregates
Au/g-C3N4 is used for degrading self-assembled aggregated products of amyloid Amylin (20-29) for example. Amyloid aggregation products were prepared by incubating a monomer solution of Amylin (20-29) purchased from Shanghai peptide Biotech, Inc. for 10 hours at 37 ℃. The incubation product and Au/g-C3N4 mixture were then irradiated under UV light to degrade the prepared amyloid aggregation product. Aggregates of Amylin (20-29) were used as positive controls and the morphology of the degradation products was characterized by Atomic Force Microscopy (AFM) after the amyloid aggregates were degraded under UV irradiation.
The AFM results in FIG. 5 show that the aggregate without degradation appears as a large number of fibers, and the height of the fibers is distributed mostly between 1-3nm, as shown in FIG. 5 (a). After the Au/g-C3N4 material is subjected to photodegradation, the Amylin (20-29) aggregates are obviously dotted and highly distributed in the interval of 5-30nm, and the disaggregation of the protein aggregates into a loose structure is proved, as shown in FIG. 5 (d). After irradiation treatment, the photocatalytic degradation of Au/g-C3N4 is proved to have strong degradation and clearance effects on amyloid aggregates.
FIG. 6 shows the detection of degradation of Amylin (20-29) by Circular Dichroism (CD) under different conditions. The graph shows that after the Au/g-C3N4 material is subjected to light degradation, the circular dichroism spectrum of the Amylin (20-29) aggregate is reduced, and the beta-sheet structure of the protein aggregate is disaggregated.
FIG. 7 shows the detection of degradation of Amylin (20-29) aggregates by irradiation with Au/g-C3N4 using a Quartz Crystal Microbalance (QCM). The rising resonant frequency curve in the figure demonstrates that the aggregates are gradually degraded and the mass becomes smaller on the surface of the quartz crystal microbalance chip.
the present invention is not limited to the above-described embodiments, and any obvious improvements, substitutions or modifications can be made by those skilled in the art without departing from the spirit of the present invention.
Claims (10)
1. the preparation method of the noble metal nano particle/g-C3N 4 composite material is characterized by comprising the following steps:
(1) Preparation of ultrathin g-C3N4 nanosheets: preparing a block g-C3N4 by treating melamine at high temperature, and stripping g-C3N4 in liquid to obtain a g-C3N4 nanosheet;
(2) Preparing a noble metal nano particle/g-C3N 4 composite material:
Firstly, preparing a noble metal reduction reaction solution, adding the prepared g-C3N4 nanosheet into the solution, stirring, fixing the reduced Au on the g-C3N4 nanosheet to prepare a noble metal nanoparticle/g-C3N 4 composite material, filtering, washing and drying at 393K overnight.
2. the method of preparing a noble metal nanoparticle/g-C3N 4 composite material according to claim 1, wherein the noble metal reduction reaction solution is a gold reduction reaction solution, HAuCl4 is dissolved in a polyvinyl alcohol solution, a newly prepared NaBH4 solution is added to the HAuCl4 solution, and incubated at room temperature for 30 minutes.
3. The method for preparing the noble metal nanoparticle/g-C3N 4 composite material according to claim 1, wherein the specific steps for preparing the bulk g-C3N4 are as follows: the melamine was heated to 600 ℃ at a ramp rate of 3 ℃/min and held for 2 hours to give a yellow product as g-C3N 4.
4. The preparation method of the noble metal nanoparticle/g-C3N 4 composite material according to claim 1, wherein the specific steps of peeling g-C3N4 in a liquid to obtain g-C3N4 nanosheets are as follows: dispersing g-C3N4 powder in water and then sonicating for about 16 hours; the resulting suspension was then centrifuged at about 5000rpm to remove the residual unsplit g-C3N4 bulk to obtain g-C3N4 nanoplatelets.
5. The noble metal nanoparticles/g-C3N 4 composite made from the preparation of the noble metal nanoparticles/g-C3N 4 composite of claim 1.
6. The noble metal nanoparticle/g-C3N 4 composite material according to claim 1, wherein the noble metal nanoparticles are gold nanoparticles.
7. Use of noble metal nanoparticles/g-C3N 4 composite material according to claim 1 for degrading amyloid aggregates, wherein Au/g-C3N4 degrades amyloid aggregates under light conditions.
8. Use of noble metal nanoparticles/g-C3N 4 composite according to claim 1, wherein the light source is ultraviolet light.
9. Use of noble metal nanoparticles/g-C3N 4 composite material according to claim 1 for the preparation of a medicament for the treatment of diseases caused by amyloid aggregates.
10. use of noble metal nanoparticles/g-C3N 4 composite according to claim 1 for degrading rhodamine.
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| CN102895987A (en) * | 2012-10-12 | 2013-01-30 | 中南大学 | Method for preparing Au/g-C3N4 composite-type micro-nano material |
| CN104475140A (en) * | 2014-11-07 | 2015-04-01 | 江苏大学 | Silver-modified carbon nitride composite photocatalytic material and preparation method thereof |
| CN109225303A (en) * | 2018-10-23 | 2019-01-18 | 江苏大学 | A kind of dimensional thinlayer Au/g-C3N4The Preparation method and use of composite photo-catalyst |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102895987A (en) * | 2012-10-12 | 2013-01-30 | 中南大学 | Method for preparing Au/g-C3N4 composite-type micro-nano material |
| CN104475140A (en) * | 2014-11-07 | 2015-04-01 | 江苏大学 | Silver-modified carbon nitride composite photocatalytic material and preparation method thereof |
| CN109225303A (en) * | 2018-10-23 | 2019-01-18 | 江苏大学 | A kind of dimensional thinlayer Au/g-C3N4The Preparation method and use of composite photo-catalyst |
Non-Patent Citations (8)
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Application publication date: 20191206 |