CN106238719A - A kind of preparation method of the ghost satellite shape structure nano photosensitizer with chirality - Google Patents
A kind of preparation method of the ghost satellite shape structure nano photosensitizer with chirality Download PDFInfo
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- CN106238719A CN106238719A CN201610580266.7A CN201610580266A CN106238719A CN 106238719 A CN106238719 A CN 106238719A CN 201610580266 A CN201610580266 A CN 201610580266A CN 106238719 A CN106238719 A CN 106238719A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
Abstract
The preparation method of a kind of ghost satellite shape structure nano photosensitizer with chirality, belongs to material chemistry technical field.The present invention includes the synthesis of golden nanometer particle, the synthesis of Nano silver grain, gold silver nanoparticle modifying DNA 1, DNA2 respectively, two kinds modify after the assembling of nanoparticle, the galactic nucleus gold assembled is defended star topology and is carried out Glavanic reaction and prepare ghost satellite shape nanostructured and obtain having the ghost satellite shape structure nano photosensitizer of chirality by modifying D cysteine.The invention provides the assemble method of the ghost satellite shape structure nano assembly with chirality, prepare the ghost satellite structure nanometric photosensitizer with rival's property that structure is homogeneous, and demonstrate its ability efficiently producing singlet oxygen with photosensitizer.
Description
Technical field
The present invention relates to the preparation method of a kind of ghost-satellite shape structure nano photosensitizer with chirality, belong to material
Technical field of chemistry.
Background technology
Chirality is a kind of the most peculiar but also common phenomenon in nature, is applied to Material Field and prepares chirality nanometer material
Material, especially chiral metal nano material is currently causing the extensive concern of people.Owing to chiral metal nano material has
Unique dimensional effect and optical effect so that it is be essentially different from the chirality of molecular dimension, can be asymmetry organic synthesis, raw
Thing application etc. provide new opportunity, so how obtain and have the nanostructured always scientist of visible ray scalable chirality and exert
The direction of power.
Photosensitizer is in photochemical reaction, and luminous energy is transferred on some reactants insensitive to visible ray to improve
Or expand the material of its photosensitive property.Photosensitizer must meet following condition: first (1) oneself can be irradiated by light activation;(2) at body
System has enough concentration, and the photon of q.s can be absorbed;(3) energy of oneself is must be able to pass to reactant.
It is assembled into ghost-satellite shape nanostructured by nano material self assembly and there is the assembly of chirality, realize
It produces the ability of singlet oxygen efficiently, as photosensitizer.
Summary of the invention
It is an object of the invention to the combination by D-Cys Yu ghost-satellite shape nanostructured, obtain that there is chirality
Ghost-satellite structure nanometric photosensitizer.
Technical scheme, the preparation method of a kind of ghost-satellite shape structure nano photosensitizer with chirality, bag
Include the synthesis of gold silver nanoparticle, the assembling of galactic nucleus-Jin Wei star topology, ghost-defend the preparation of star topology and modify D-half
The preparation of the ghost of cystine-defend star topology, the ghost-satellite shape structure nano photosensitizer modifying D-Cys produces single
The mensuration of line state oxygen ability;
Specifically comprise the following steps that
(1) synthesis of 15nm golden nanometer particle: synthesize by reduction of sodium citrate synthetic method;In the conical flask of clean 250mL
Add 195mL ultra-pure water, add the chlorauric acid solution of 5mL mass concentration 0.4%, be stirred and heated to boiling, after 7-8min, add 4.8mL
The citric acid three sodium solution of mass concentration 1%, to solution from colourless become claret after, stop heating, continue stirring, until cold
But to room temperature, the golden nanometer particle that particle diameter is 15nm is i.e. obtained;
(2) synthesis of 18-20nm Nano silver grain: taking 20mL ultra-pure water with 5mL mass concentration is the polyvinylpyrrolidone of 1%
It is mixed in conical flask, then adds the sodium borohydride aqueous solution of 0.6mL 0.1mol/L and the Fructus Citri Limoniae that mass fraction is 1% of 0.6mL
Acid trisodium, and carry out ice bath protection;Then, by dense to aqueous povidone solution and 5mL mass that 5mL mass concentration is 1%
Degree is to join in above-mentioned solution with the speed syringe pump of 30mL/h while of the silver nitrate aqueous solution of 0.17%, notices that limit is stirred
Mix limit to add, after end to be added, be positioned over 80 DEG C of water-bath 2h and i.e. obtain the Nano silver grain of yellow solution, i.e. 18-20nm;
(3) assembling of galactic nucleus-gold satellite structure:
A, the solution of gold nanoparticles of the 1mL that step (1) is prepared gained are centrifuged 10min with 10000rpm, remove supernatant, precipitation
It is resuspended in the phosphate buffer of 100 μ L pH=7.5,10mM, obtains golden nanometer particle PB solution, standby;
B, the silver nano-particle solution of gained 1mL is prepared by step (2) it is centrifuged 15min with 7500rpm, remove supernatant, precipitation weight
It is suspended from the Tris-HCl buffer of 200 μ L pH=7.5,10mM, obtains Nano silver grain Tris-HCl solution, standby;
C, take golden nanometer particle PB solution 100 μ L prepared by step a, be added thereto to 2 μ L, 10 μMs the mixing of DNA1 solution all
Even;Take 200 μ L Nano silver grain Tris-HCl solution prepared by step b, be added thereto to 2 μ L, the DNA2 solution mixing of 100 μMs
Uniformly, 37 DEG C are rocked reaction 12h, respectively obtain Au-DNA1 complex and Ag-DNA2 complex;
D, by step c gained Au-DNA1 complex with 10000rpm be centrifuged 10min, Ag-DNA2 complex with 7500rpm be centrifuged
15min, removes the DNA of the most unnecessary non-coupling of supernatant, then both precipitations is mixed in the Tris-of 100 μ L pH7.5 10mM
In HCl, rock and be allowed to fully hybridize, react 12h, i.e. obtain galactic nucleus-Jin Wei star topology assembly;
(4) preparation of ghost-defend star topology: the 100 μ L galactic nucleus-Jin Wei star topology assemblies prepared in step (3) are molten
In liquid, add the HAuCl of 1 μ L, 10mM4Solution, is sufficiently mixed, and makes silver and HAuCl4There is Galvanic reaction, fully shake
5s, makes ghost-satellite shape structure nano assembly;8000rpm is centrifuged 15min, is resuspended in 100 μ L pH=9 10mM's
In Tris-HCl solution, i.e. obtain ghost-satellite shape structure nano assembly;
(5) preparation of the ghost of D-Cys-defend star topology it is modified with: the pH that is resuspended in prepared at 100 μ L step (4) is
In ghost in the Tris-HCl solution of 9-satellite shape structure nano assembly, add the D-Cys of 10 μ L 300 μMs, fill
Dividing mixing concussion 15min, 7500rpm is centrifuged 15min afterwards, i.e. obtains the adjustable ghost of chirality-satellite shape structure nano group
Dress body;Its CD value can be recorded by circular dichroism instrument, and characterize its ghost-defend star topology by transmission electron microscope;
(6) ghost-satellite shape structure nano photosensitizer modifying D-Cys produces the mensuration of singlet oxygen ability: by step
(5) material obtained in is centrifuged and is resuspended in the PBS solution of same volume, mixes with singlet oxygen fluorescence probe, is placed in
Illumination 20min under 532nm right-hand circularly polarized light, detects its emission spectrum under 504nm excites by fluorescence spectrophotometer afterwards.
Described DNA sequence is DNA1:5 '-AAAAAGCAGT TGATCCTTTG GAT-3 ';DNA2:5 '-AAAAAATCCA
AAGGATCAAC TGC-3’。
Beneficial effects of the present invention: the invention provides the system of the ghost-satellite shape structure nano photosensitizer with chirality
Preparation Method, and demonstrated this ghost-satellite shape structure nano photosensitizer under illumination condition and have and efficiently produce singlet oxygen
Ability.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture of ghost-satellite shape structure nano photosensitizer.
Fig. 2 is the circular dichroism figure of ghost-satellite shape structure nano photosensitizer.
Fig. 3 is the singlet oxygen fluorescence probe fluorescence of the ghost-satellite shape structure nano photosensitizer modifying D-cysteine
Spectrogram.
Detailed description of the invention
Embodiment 1
Chloroazotic acid soaked overnight all used by all of glass apparatus, and distilled water cleans, and dries standby.The water used in experiment is
The Milli-Q ultra-pure water of 18.2M Ω.
(1) synthesis of golden nanometer particle: the synthesis of 15nm golden nanometer particle: synthesize by reduction of sodium citrate synthetic method;?
The conical flask of clean 250mL adds 195mL ultra-pure water, adds the chlorauric acid solution of 5mL mass concentration 0.4%, be stirred and heated to
Boiling, add the citric acid three sodium solution of 4.8mL mass concentration 1% after 7-8min, to solution from colourless become claret after, stop
Heating, continuing stirring, until being cooled to room temperature, i.e. obtaining the golden nanometer particle that particle diameter is 15nm;
(2) synthesis of 18-20nm Nano silver grain: taking 20mL ultra-pure water with 5mL mass concentration is the polyvinylpyrrolidone of 1%
It is mixed in conical flask, then adds the sodium borohydride aqueous solution of 0.6mL 0.1mol/L and the Fructus Citri Limoniae that mass fraction is 1% of 0.6mL
Acid trisodium, and carry out ice bath protection.Then, by dense to aqueous povidone solution and 5mL mass that 5mL mass concentration is 1%
Degree is to join in above-mentioned solution with the speed syringe pump of 30mL/h while of the silver nitrate aqueous solution of 0.17%, notices that limit is stirred
Mix limit to add, after end to be added, be positioned over 80 DEG C of water-bath 2h and i.e. obtain the Nano silver grain of yellow solution, i.e. 18nm-20nm;
(3) assembling of galactic nucleus-gold satellite structure:
A, the solution of gold nanoparticles of the 1mL that step (1) is prepared gained are centrifuged 10min with 10000rpm, remove supernatant, precipitation
It is resuspended in the phosphate buffer of 100 μ L pH=7.5,10mM, obtains golden nanometer particle PB solution, standby;
B, the silver nano-particle solution of gained 1mL is prepared by step (2) it is centrifuged 15min with 7500rpm, remove supernatant, precipitation weight
It is suspended from the Tris-HCl buffer of 200 μ L pH=7.5,10mM, obtains Nano silver grain Tris-HCl solution, standby;
C, take golden nanometer particle PB solution 100 μ L prepared by step a, be added thereto to 2 μ L, 10 μMs the mixing of DNA1 solution all
Even;Take 200 μ L Nano silver grain Tris-HCl solution prepared by step b, be added thereto to 2 μ L, the DNA2 solution mixing of 100 μMs
Uniformly, 37 DEG C are rocked reaction 12h, respectively obtain Au-DNA1 complex and Ag-DNA2 complex;
D, by step c gained Au-DNA1 complex with 10000rpm be centrifuged 10min, Ag-DNA2 complex with 7500rpm be centrifuged
15min, removes the DNA of the most unnecessary non-coupling of supernatant, then both precipitations is mixed in the Tris-of 100 μ L pH7.5 10mM
In HCl, rock and be allowed to fully hybridize, react 12h, i.e. obtain galactic nucleus-gold satellite shape assembly;
DNA1:5 '-AAAAAGCAGT TGATCCTTTG GAT-3 '
DNA2:5 '-AAAAAATCCA AAGGATCAAC TGC-3 '
(4) preparation of ghost-defend star topology: the 100 μ L galactic nucleus-Jin Wei star topology assemblies prepared in step (3) are molten
In liquid, add the HAuCl of 1 μ L, 10mM4Solution, is sufficiently mixed, and makes silver and HAuCl4There is Galvanic reaction, fully shake
5s, makes ghost-satellite shape structure nano assembly;8000rpm is centrifuged 15min, is resuspended in 100 μ L pH=9 10mM's
In Tris-HCl solution, i.e. obtain ghost-satellite shape structure nano assembly;
(5) preparation of the ghost of D-Cys-defend star topology it is modified with: the pH that is resuspended in prepared at 100 μ L step (4) is
In ghost in the Tris-HCl solution of 9-satellite shape structure nano assembly, add the D-Cys of 10 μ L 300 μMs, fill
Dividing mixing concussion 15min, 7500rpm is centrifuged 15min afterwards, i.e. obtains the adjustable ghost of chirality-satellite shape structure nano group
Dress body;Its CD value can be recorded by circular dichroism instrument, and characterize its ghost-defend star topology by transmission electron microscope;
(6) ghost-satellite shape structure nano photosensitizer being modified with D-Cys produces the ability of singlet oxygen: by step
(5) ghost that the material D-Cys that obtains in is modified-defend star topology is centrifuged 10min in 8000rpm, and is resuspended in same
In the PBS solution of volume, it is added thereto to 5 μMs of singlet oxygen fluorescence probes, is placed in illumination under 532nm right-hand circularly polarized light
20min, detects its emission spectrum under 504nm excites by fluorescence spectrophotometer afterwards.The ghost-defend modified with D-Cys
The singlet oxygen fluorescence probe fluorescence spectrum figure of star topology is as shown in Figure 3.
Claims (2)
1. the preparation method of ghost-satellite shape structure nano photosensitizer with chirality, it is characterised in that include that gold silver is received
The synthesis of rice corpuscles, the assembling of galactic nucleus-Jin Wei star topology, ghost-defend the preparation of star topology and modify D-Cys
The preparation of ghost-defend star topology, the ghost-satellite shape structure nano photosensitizer modifying D-Cys produces singlet oxygen energy
The mensuration of power;
Step is as follows:
(1) synthesis of 15nm golden nanometer particle: synthesize by reduction of sodium citrate synthetic method;In the conical flask of clean 250mL
Add 195mL ultra-pure water, add the chlorauric acid solution of 5mL mass concentration 0.4%, be stirred and heated to boiling, after 7-8min, add 4.8mL
The citric acid three sodium solution of mass concentration 1%, to solution from colourless become claret after, stop heating, continue stirring, until cold
But to room temperature, the golden nanometer particle that particle diameter is 15nm is i.e. obtained;
(2) synthesis of 18-20nm Nano silver grain: taking 20mL ultra-pure water with 5mL mass concentration is the polyvinylpyrrolidone of 1%
It is mixed in conical flask, then adds the sodium borohydride aqueous solution of 0.6mL 0.1mol/L and the Fructus Citri Limoniae that mass fraction is 1% of 0.6mL
Acid trisodium, and carry out ice bath protection;Then, by dense to aqueous povidone solution and 5mL mass that 5mL mass concentration is 1%
Degree is to join in above-mentioned solution with the speed syringe pump of 30mL/h, while stirring the while of the silver nitrate aqueous solution of 0.17%
Add, after end to be added, be positioned over 80 DEG C of water-bath 2h and i.e. obtain the Nano silver grain of yellow solution, i.e. 18-20nm;
(3) assembling of galactic nucleus-Jin Wei star topology:
A, the solution of gold nanoparticles of the 1mL that step (1) is prepared gained are centrifuged 10min with 10000rpm, remove supernatant, precipitation
It is resuspended in the phosphate buffer of 100 μ L pH=7.5,10mM, obtains golden nanometer particle PB solution, standby;
B, the silver nano-particle solution of gained 1mL is prepared by step (2) it is centrifuged 15min with 7500rpm, remove supernatant, precipitation weight
It is suspended from the Tris-HCl buffer of 200 μ L pH=7.5,10mM, obtains Nano silver grain Tris-HCl solution, standby;
C, take golden nanometer particle PB solution 100 μ L prepared by step a, be added thereto to 2 μ L, 10 μMs the mixing of DNA1 solution all
Even;Take 200 μ L Nano silver grain Tris-HCl solution prepared by step b, be added thereto to 2 μ L, the DNA2 solution mixing of 100 μMs
Uniformly, 37 DEG C are rocked reaction 12h, respectively obtain Au-DNA1 complex and Ag-DNA2 complex;
D, by step c gained Au-DNA1 complex with 10000rpm be centrifuged 10min, Ag-DNA2 complex with 7500rpm be centrifuged
15min, removes the DNA of the most unnecessary non-coupling of supernatant, then both precipitations is mixed in the Tris-of 100 μ L pH7.5 10mM
In HCl, rock and be allowed to fully hybridize, react 12h, i.e. obtain galactic nucleus-Jin Wei star topology assembly;
(4) preparation of ghost-defend star topology: the 100 μ L galactic nucleus-Jin Wei star topology assemblies prepared in step (3) are molten
In liquid, add the HAuCl of 1 μ L, 10mM4Solution, is sufficiently mixed, and makes silver and HAuCl4There is Galvanic reaction, fully shake
5s, makes ghost-satellite shape structure nano assembly;8000rpm is centrifuged 15min, is resuspended in 100 μ L pH=9 10mM's
In Tris-HCl solution, i.e. obtain ghost-satellite shape structure nano assembly;
(5) preparation of the ghost of D-Cys-defend star topology it is modified with: the pH that is resuspended in prepared at 100 μ L step (4) is
In ghost in the Tris-HCl solution of 9-satellite shape structure nano assembly, add the D-Cys of 10 μ L 300 μMs, fill
Dividing mixing concussion 15min, 7500rpm is centrifuged 15min afterwards, i.e. obtains the adjustable ghost of chirality-satellite shape structure nano group
Dress body;Record its CD value by circular dichroism instrument, and characterize its ghost-defend star topology by transmission electron microscope;
(6) ghost-satellite shape structure nano photosensitizer modifying D-Cys produces the mensuration of singlet oxygen ability: by step
(5) material obtained in is centrifuged and is resuspended in the PBS solution of same volume, mixes with singlet oxygen fluorescence probe, is placed in
Illumination 20min under 532nm right-hand circularly polarized light, detects its emission spectrum under 504nm excites by fluorescence spectrophotometer afterwards.
The most according to claim 1, have the preparation method of the ghost-satellite shape structure nano photosensitizer of chirality, its feature exists
In: described DNA sequence is DNA1:5 '-AAAAAGCAGT TGATCCTTTG GAT-3 ';DNA2:5 '-AAAAAATCCA
AAGGATCAAC TGC-3’。
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CN104588678A (en) * | 2015-01-09 | 2015-05-06 | 中国科学院合肥物质科学研究院 | Preparation method of gold-silver composite nanoring |
CN105127413A (en) * | 2015-09-18 | 2015-12-09 | 温州大学 | Precious metal nanoring and preparation method thereof |
CN105621352A (en) * | 2015-12-31 | 2016-06-01 | 江南大学 | Preparing method of gold nanometer particle single-layer film with chirality |
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WO2013136167A1 (en) * | 2012-03-16 | 2013-09-19 | Nanosensing Technologies, Inc. | Composite metallic solar cells |
CN103163076A (en) * | 2013-02-26 | 2013-06-19 | 江南大学 | Method for detecting L-cysteine concentration by applying of circular dichroism |
CN103157811A (en) * | 2013-03-13 | 2013-06-19 | 江南大学 | Preparing method of gold-silver core-shell structure - gold dimer chirality assembly body |
CN104237136A (en) * | 2014-09-29 | 2014-12-24 | 江南大学 | Ultra-sensitive detection method of ochratoxin A based on gold core-silver satellite chiral assembly body |
CN104259477A (en) * | 2014-09-29 | 2015-01-07 | 江南大学 | Method of liquid-phase preparation for chirality silver nano-chain |
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