CN106238719B - A kind of preparation method with chiral ghost satellite shape structure nano sensitising agent - Google Patents
A kind of preparation method with chiral ghost satellite shape structure nano sensitising agent Download PDFInfo
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- CN106238719B CN106238719B CN201610580266.7A CN201610580266A CN106238719B CN 106238719 B CN106238719 B CN 106238719B CN 201610580266 A CN201610580266 A CN 201610580266A CN 106238719 B CN106238719 B CN 106238719B
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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
- G01—MEASURING; TESTING
- 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
A kind of preparation method with chiral ghost satellite shape structure nano sensitising agent, belongs to material chemistry technical field.The present invention includes the synthesis of golden nanometer particle, the synthesis of Nano silver grain, gold and silver nano-particle difference modifying DNA 1, DNA2, the assembling of nano-particle after two kinds of modifications, the galactic nucleus gold assembled defend star topology progress Glavanic reactions and ghost satellite shape nanostructured are prepared and is obtained by modifying D cysteines with chiral ghost satellite shape structure nano sensitising agent.The invention provides the assemble method of the ghost satellite shape structure nano assembly with chirality, the homogeneous ghost satellite structure nanometric photosensitizer with rival's property of structure is prepared, and demonstrate the ability of its efficient generation singlet oxygen with sensitising agent.
Description
Technical field
The present invention relates to a kind of preparation method with chiral ghost-satellite shape structure nano sensitising agent, belong to material
Technical field of chemistry.
Background technology
Chirality is phenomenon a kind of not only peculiar but also common in nature, is applied to Material Field and prepares chiral nanometer material
Material, especially chiral metal nano material is currently causing the extensive concern of people.Because chiral metal nano material has
Unique dimensional effect and optical effect, makes it be essentially different from the chirality of molecular dimension, can be asymmetry organic synthesis, raw
The new opportunities of offer such as thing application, so how to obtain with the adjustable chiral nanostructured of visible ray is always that scientist exerts
The direction of power.
Sensitising agent is in photochemical reaction, luminous energy is transferred on some reactants insensitive to visible ray to improve
Or expand the material of its photosensitive property.Sensitising agent must meet following conditions：(1) oneself can be irradiated by light activation first；(2) in body
There is enough concentration in system, and the photon of sufficient amount can be absorbed；(3) energy transmission oneself is must be able to reactant.
There is chiral assembly to be assembled into ghost-satellite shape nanostructured by nano material self assembly, to realize
Its efficient ability for producing singlet oxygen, as sensitising agent.
The content of the invention
The purpose of the present invention is the combination by D-Cys and ghost-satellite shape nanostructured, obtains having chirality
Ghost-satellite structure nanometric photosensitizer.
Technical scheme, a kind of preparation method with chiral ghost-satellite shape structure nano sensitising agent, bag
Include the synthesis of gold and silver nano-particle, the assembling of galactic nucleus-Jin Wei star topologies, ghost-defend the preparation of star topology and modify D- half
The preparation of the ghost of cystine-defend star topology, modify D-Cys ghost-satellite shape structure nano sensitising agent produce it is single
The measure of line state oxygen ability；
Comprise the following steps that：
（1）The synthesis of 15nm golden nanometer particles：Synthesized with reduction of sodium citrate synthetic method；In the 250mL of cleaning taper
Add 195mL ultra-pure waters in bottle, add the chlorauric acid solution of 5mL mass concentrations 0.4%, be stirred and heated to boiling, add after 7-8min
The citric acid three sodium solution of 4.8mL mass concentrations 1%, to solution from it is colourless be changed into claret after, stop heating, continue to stir, directly
To room temperature is cooled to, that is, obtain the golden nanometer particle that particle diameter is 15nm；
（2）The synthesis of 18-20nm Nano silver grains：Take the polyvinyl pyrrole that 20mL ultra-pure waters and 5mL mass concentrations are 1%
Alkanone is mixed in conical flask, then adds 0.6mL 0.1mol/L sodium borohydride aqueous solution and 0.6mL mass fraction to be 1%
Trisodium citrate, and carry out ice bath protection；Then, by aqueous povidone solution and 5mL matter of the 5mL mass concentrations for 1%
The silver nitrate aqueous solution that amount concentration is 0.17% is added in above-mentioned solution with 30mL/h speed with syringe pump simultaneously, is paid attention to
Add while stirring, after end to be added, be positioned over 80 DEG C of water-bath 2h and obtain yellow solution, i.e. 18-20nm nano grain of silver
Son；
（3）The assembling of galactic nucleus-golden satellite structure：
A, by step（1）The solution of gold nanoparticles for preparing the 1mL of gained centrifuges 10min with 10000rpm, removes supernatant,
Precipitation be resuspended in 100 μ L pH=7.5,10mM phosphate buffer in, obtain golden nanometer particle PB solution, it is standby；
B, by step（2）The silver nano-particle solution for preparing gained 1mL centrifuges 15min with 7500rpm, removes supernatant, sinks
Form sediment be resuspended in 200 μ L pH=7.5,10mM Tris-HCl buffer solutions in, obtain Nano silver grain Tris-HCl solution, it is standby；
C, the μ L of golden nanometer particle PB solution 100 for taking step a to prepare, 2 μ L, the mixing of 10 μM of DNA1 solution are added thereto
Uniformly；The 200 μ L Nano silver grain Tris-HCl solution for taking step b to prepare, add 2 μ L, 100 μM of DNA2 solution mixes thereto
Close uniformly, 37 DEG C are rocked reaction 12h, respectively obtain Au-DNA1 complexs and Ag-DNA2 complexs；
D, Au-DNA1 complexs obtained by step c are centrifuged into 10min with 10000rpm, Ag-DNA2 complexs are with 7500rpm
15min is centrifuged, it is the unnecessary DNA not being coupled to remove supernatant, then precipitates both and is mixed in 100 μ L pH7.5 10mM's
In Tris-HCl, rock and be allowed to fully hybridize, react 12h, that is, obtain galactic nucleus-Jin Wei star topology assemblies；
（4）The preparation of ghost-defend star topology：In step（3）In obtained 100 μ L galactic nucleus-Jin Wei star topologies assembling
In liquid solution, 1 μ L, 10mM HAuCl are added4Solution, it is sufficiently mixed, makes silver and HAuCl4Generation Galvanic reacts, fully shake
5s is swung, makes ghost-satellite shape structure nano assembly；8000rpm centrifuges 15min, is resuspended in the 10mM of 100 μ L pH=9
Tris-HCl solution in, that is, obtain ghost-satellite shape structure nano assembly；
（5）It is modified with the preparation of the ghost of D-Cys-defend star topology：In 100 μ L steps（4）What is prepared is resuspended in
PH is the Guang ammonia of D- half that 300 μM of 10 μ L are added in ghost-satellite shape structure nano assembly in 9 Tris-HCl solution
Acid, concussion 15min is sufficiently mixed, 7500rpm centrifuges 15min afterwards, produces chiral adjustable ghost-defend star topology and receives
Rice assembly；Its CD value can be measured by circular dichroism instrument, and its ghost-defend star topology is characterized by transmission electron microscope；
（6）Ghost-satellite shape structure nano the sensitising agent for modifying D-Cys produces the measure of singlet oxygen ability：Will
Step（5）In obtained material centrifuge and be resuspended in the PBS solution of same volume, mixed with singlet oxygen fluorescence probe, and
Illumination 20min under 532nm right-hand circularly polarized lights is placed in, detects its emission spectrum in the case where 504nm is excited with XRF afterwards.
The DNA sequence dna 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 ghost-satellite shape structure nano sensitising agent with chirality
Preparation Method, and demonstrated the ghost-satellite shape structure nano sensitising agent under illumination condition and produced singlet oxygen with efficient
Ability.
Brief description of the drawings
Fig. 1 is the transmission electron microscope picture of ghost-satellite shape structure nano sensitising agent.
Fig. 2 is the circular dichroism figure of ghost-satellite shape structure nano sensitising agent.
Fig. 3 is the singlet oxygen fluorescence probe fluorescence for the ghost-satellite shape structure nano sensitising agent for modifying D-cysteine
Spectrogram.
Embodiment
Embodiment 1
All glass apparatus all use chloroazotic acid soaked overnight, distilled water cleaning, dry standby.The water used in experiment is
18.2M Ω Milli-Q ultra-pure waters.
（1）The synthesis of golden nanometer particle：The synthesis of 15nm golden nanometer particles：Synthesized with reduction of sodium citrate synthetic method；
Add 195mL ultra-pure waters in clean 250mL conical flask, add the chlorauric acid solution of 5mL mass concentrations 0.4%, be stirred and heated to
Boiling, after 7-8min plus 4.8mL mass concentrations 1% citric acid three sodium solution, to solution from it is colourless be changed into claret after, stop
Heating, continues to stir, until being cooled to room temperature, that is, obtains the golden nanometer particle that particle diameter is 15nm；
（2）The synthesis of 18-20nm Nano silver grains：Take the polyvinyl pyrrole that 20mL ultra-pure waters and 5mL mass concentrations are 1%
Alkanone is mixed in conical flask, then adds 0.6mL 0.1mol/L sodium borohydride aqueous solution and 0.6mL mass fraction to be 1%
Trisodium citrate, and carry out ice bath protection.Then, by aqueous povidone solution and 5mL matter of the 5mL mass concentrations for 1%
The silver nitrate aqueous solution that amount concentration is 0.17% is added in above-mentioned solution with 30mL/h speed with syringe pump simultaneously, is paid attention to
Add while stirring, after end to be added, be positioned over 80 DEG C of water-bath 2h and obtain yellow solution, i.e. 18nm-20nm silver nanoparticle
Particle；
（3）The assembling of galactic nucleus-golden satellite structure：
A, by step（1）The solution of gold nanoparticles for preparing the 1mL of gained centrifuges 10min with 10000rpm, removes supernatant,
Precipitation be resuspended in 100 μ L pH=7.5,10mM phosphate buffer in, obtain golden nanometer particle PB solution, it is standby；
B, by step（2）The silver nano-particle solution for preparing gained 1mL centrifuges 15min with 7500rpm, removes supernatant, sinks
Form sediment be resuspended in 200 μ L pH=7.5,10mM Tris-HCl buffer solutions in, obtain Nano silver grain Tris-HCl solution, it is standby；
C, the μ L of golden nanometer particle PB solution 100 for taking step a to prepare, 2 μ L, the mixing of 10 μM of DNA1 solution are added thereto
Uniformly；The 200 μ L Nano silver grain Tris-HCl solution for taking step b to prepare, add 2 μ L, 100 μM of DNA2 solution mixes thereto
Close uniformly, 37 DEG C are rocked reaction 12h, respectively obtain Au-DNA1 complexs and Ag-DNA2 complexs；
D, Au-DNA1 complexs obtained by step c are centrifuged into 10min with 10000rpm, Ag-DNA2 complexs are with 7500rpm
15min is centrifuged, it is the unnecessary DNA not being coupled to remove supernatant, then precipitates both and is mixed in 100 μ L pH7.5 10mM's
In Tris-HCl, rock and be allowed to fully hybridize, react 12h, that is, obtain galactic nucleus-golden satellite shape assembly；
DNA1：5’-AAAAAGCAGT TGATCCTTTG GAT-3’
DNA2：5’-AAAAAATCCA AAGGATCAAC TGC-3’
（4）The preparation of ghost-defend star topology：In step（3）In obtained 100 μ L galactic nucleus-Jin Wei star topologies assembling
In liquid solution, 1 μ L, 10mM HAuCl are added4Solution, it is sufficiently mixed, makes silver and HAuCl4Generation Galvanic reacts, fully shake
5s is swung, makes ghost-satellite shape structure nano assembly；8000rpm centrifuges 15min, is resuspended in the 10mM of 100 μ L pH=9
Tris-HCl solution in, that is, obtain ghost-satellite shape structure nano assembly；
（5）It is modified with the preparation of the ghost of D-Cys-defend star topology：In 100 μ L steps（4）What is prepared is resuspended in
PH is the Guang ammonia of D- half that 300 μM of 10 μ L are added in ghost-satellite shape structure nano assembly in 9 Tris-HCl solution
Acid, concussion 15min is sufficiently mixed, 7500rpm centrifuges 15min afterwards, produces chiral adjustable ghost-defend star topology and receives
Rice assembly；Its CD value can be measured by circular dichroism instrument, and its ghost-defend star topology is characterized by transmission electron microscope；
（6）Ghost-satellite shape structure nano the sensitising agent for being modified with D-Cys produces the ability of singlet oxygen：Will step
Suddenly（5）In obtained ghost-the defend star topology of material D-Cys modification centrifuge 10min in 8000rpm, and be resuspended in same
In the PBS solution of sample volume, 5 μM of singlet oxygen fluorescence probes are added thereto, are placed in illumination under 532nm right-hand circularly polarized lights
20min, detect its emission spectrum in the case where 504nm is excited with XRF afterwards.The ghost modified with D-Cys-defend
The singlet oxygen fluorescence probe fluorescence spectra of star topology is as shown in Figure 3.
Claims (2)
1. a kind of preparation method with chiral ghost-satellite shape structure nano sensitising agent, it is characterised in that received including gold and silver
The synthesis of rice corpuscles, the assembling of galactic nucleus-Jin Wei star topologies, ghost-defend the preparation of star topology and modify D-Cys
The preparation of ghost-defend star topology, the ghost-satellite shape structure nano sensitising agent for modifying D-Cys produce singlet oxygen energy
The measure of power；
Step is as follows：
（1）The synthesis of 15nm golden nanometer particles：Synthesized with reduction of sodium citrate synthetic method；In the 250mL of cleaning conical flask
Add 195mL ultra-pure waters, add the chlorauric acid solution of 5mL mass concentrations 0.4%, be stirred and heated to boiling, add 4.8mL after 7-8min
The citric acid three sodium solution of mass concentration 1%, to solution from it is colourless be changed into claret after, stop heating, continue to stir, until cold
But to room temperature, that is, the golden nanometer particle that particle diameter is 15nm is obtained；
（2）The synthesis of 18-20nm Nano silver grains：Take the polyvinylpyrrolidone that 20mL ultra-pure waters and 5mL mass concentrations are 1%
It is mixed in conical flask, then adds the lemon that 0.6mL 0.1mol/L sodium borohydride aqueous solution and 0.6mL mass fraction are 1%
Sour trisodium, and carry out ice bath protection；Then, it is 5mL mass concentrations is dense for 1% aqueous povidone solution and 5mL mass
Spend the silver nitrate aqueous solution for 0.17% while be added to 30mL/h speed with syringe pump in above-mentioned solution, while stirring
Add, after end to be added, be positioned over 80 DEG C of water-bath 2h and obtain yellow solution, i.e. 18-20nm Nano silver grain；
（3）The assembling of galactic nucleus-Jin Wei star topologies：
A, by step（1）The solution of gold nanoparticles for preparing the 1mL of gained centrifuges 10min with 10000rpm, removes supernatant, precipitation
Be resuspended in 100 μ L pH=7.5,10mM phosphate buffer in, obtain golden nanometer particle PB solution, it is standby；
B, by step（2）The silver nano-particle solution for preparing gained 1mL centrifuges 15min with 7500rpm, removes supernatant, precipitation weight
Be suspended from 200 μ L pH=7.5,10mM Tris-HCl buffer solutions in, obtain Nano silver grain Tris-HCl solution, it is standby；
C, the μ L of golden nanometer particle PB solution 100 for taking step a to prepare, 2 μ L, the mixing of 10 μM of DNA1 solution are added thereto
It is even；The 200 μ L Nano silver grain Tris-HCl solution for taking step b to prepare, 2 μ L, the mixing of 100 μM of DNA2 solution are added thereto
Uniformly, 37 DEG C are rocked reaction 12h, respectively obtain Au-DNA1 complexs and Ag-DNA2 complexs；
D, Au-DNA1 complexs obtained by step c are centrifuged into 10min with 10000rpm, Ag-DNA2 complexs are centrifuged with 7500rpm
15min, it is the unnecessary DNA not being coupled to remove supernatant, then both are precipitated to the Tris- for being mixed in 100 μ L pH7.5 10mM
In HCl, rock and be allowed to fully hybridize, react 12h, that is, obtain galactic nucleus-Jin Wei star topology assemblies；
（4）The preparation of ghost-defend star topology：In step（3）In obtained 100 μ L galactic nucleus-Jin Wei star topology assemblies it is molten
In liquid, 1 μ L, 10mM HAuCl are added4Solution, it is sufficiently mixed, makes silver and HAuCl4Generation Galvanic reacts, fully shaking
5s, make ghost-satellite shape structure nano assembly；8000rpm centrifuges 15min, is resuspended in the 10mM's of 100 μ L pH=9
In Tris-HCl solution, that is, obtain ghost-satellite shape structure nano assembly；
（5）It is modified with the preparation of the ghost of D-Cys-defend star topology：In 100 μ L steps（4）Prepare the pH that is resuspended in be
In ghost-satellite shape structure nano assembly in 9 Tris-HCl solution, 300 μM of 10 μ L D-Cys are added, are filled
Divide mixing concussion 15min, 7500rpm centrifuges 15min afterwards, produces chiral adjustable ghost-satellite shape structure nano group
Fill body；Its CD value is measured by circular dichroism instrument, and its ghost-defend star topology is characterized by transmission electron microscope；
（6）Ghost-satellite shape structure nano the sensitising agent for modifying D-Cys produces the measure of singlet oxygen ability：By step
（5）In obtained material centrifuge and be resuspended in the PBS solution of same volume, mix, be placed in singlet oxygen fluorescence probe
Illumination 20min under 532nm right-hand circularly polarized lights, detect its emission spectrum in the case where 504nm is excited with XRF afterwards.
2. having the preparation method of chiral ghost-satellite shape structure nano sensitising agent according to claim 1, its feature exists
In：The DNA sequence dna is DNA1：5’-AAAAAGCAGT TGATCCTTTG GAT-3’； DNA2：5’-AAAAAATCCA
AAGGATCAAC TGC-3’。
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| US20140102536A1 (en) * | 2012-03-16 | 2014-04-17 | Nanosensing Technologies, Inc. | Composite Metallic Solar Cells |
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| CN103163076A (en) * | 2013-02-26 | 2013-06-19 | 江南大学 | Method for detecting L-cysteine concentration by applying of circular dichroism |
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