CN109529037A - A kind of double-mode imaging photothermolumineseence probe and preparation method thereof and its application - Google Patents
A kind of double-mode imaging photothermolumineseence probe and preparation method thereof and its application Download PDFInfo
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- CN109529037A CN109529037A CN201811569193.7A CN201811569193A CN109529037A CN 109529037 A CN109529037 A CN 109529037A CN 201811569193 A CN201811569193 A CN 201811569193A CN 109529037 A CN109529037 A CN 109529037A
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- 229920001690 polydopamine Polymers 0.000 claims abstract description 25
- FBGGJHZVZAAUKJ-UHFFFAOYSA-N bismuth selenide Chemical compound [Se-2].[Se-2].[Se-2].[Bi+3].[Bi+3] FBGGJHZVZAAUKJ-UHFFFAOYSA-N 0.000 claims abstract 3
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims description 46
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- 230000000694 effects Effects 0.000 abstract description 26
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Classifications
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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
- A61K41/0052—Thermotherapy; Hyperthermia; Magnetic induction; Induction heating therapy
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K49/00—Preparations for testing in vivo
- A61K49/0002—General or multifunctional contrast agents, e.g. chelated agents
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K49/00—Preparations for testing in vivo
- A61K49/001—Preparation for luminescence or biological staining
- A61K49/0013—Luminescence
- A61K49/0017—Fluorescence in vivo
- A61K49/0019—Fluorescence in vivo characterised by the fluorescent group, e.g. oligomeric, polymeric or dendritic molecules
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K49/00—Preparations for testing in vivo
- A61K49/001—Preparation for luminescence or biological staining
- A61K49/0063—Preparation for luminescence or biological staining characterised by a special physical or galenical form, e.g. emulsions, microspheres
- A61K49/0069—Preparation for luminescence or biological staining characterised by a special physical or galenical form, e.g. emulsions, microspheres the agent being in a particular physical galenical form
- A61K49/0089—Particulate, powder, adsorbate, bead, sphere
- A61K49/0091—Microparticle, microcapsule, microbubble, microsphere, microbead, i.e. having a size or diameter higher or equal to 1 micrometer
- A61K49/0093—Nanoparticle, nanocapsule, nanobubble, nanosphere, nanobead, i.e. having a size or diameter smaller than 1 micrometer, e.g. polymeric nanoparticle
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K49/00—Preparations for testing in vivo
- A61K49/04—X-ray contrast preparations
- A61K49/0433—X-ray contrast preparations containing an organic halogenated X-ray contrast-enhancing agent
- A61K49/0447—Physical forms of mixtures of two different X-ray contrast-enhancing agents, containing at least one X-ray contrast-enhancing agent which is a halogenated organic compound
- A61K49/0476—Particles, beads, capsules, spheres
- A61K49/0485—Nanoparticles, nanobeads, nanospheres, nanocapsules, i.e. having a size or diameter smaller than 1 micrometer
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/51—Nanocapsules; Nanoparticles
- A61K9/5107—Excipients; Inactive ingredients
- A61K9/513—Organic macromolecular compounds; Dendrimers
- A61K9/5146—Organic macromolecular compounds; Dendrimers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyethylene glycol, polyamines, polyanhydrides
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- A—HUMAN NECESSITIES
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Abstract
The invention discloses a kind of double-mode imaging photothermolumineseence probe and preparation method thereof and its applications.The double-mode imaging photothermolumineseence probe includes nucleome and the clad for being coated on nucleome, the nucleome is optothermal material, the optothermal material includes bismuth selenide nano material, the material of the clad includes poly-dopamine, is combined with nir dye on the outer surface of the nucleome in the clad.The double-mode imaging photothermolumineseence probe double-mode imaging photothermolumineseence probe has strong photo-thermal effect, and structure and stable chemical performance, has the imaging of 2nd area of near-infrared and CT imaging function, can effectively inhibit the growth of tumour cell.And preparation method can effectively ensure that the double-mode imaging photothermolumineseence probe structure of preparation and the stabilization of performance, and condition is easily-controllable, effectively increases production efficiency, reduces economic cost.
Description
Technical field
The invention belongs to nano-probe technical field, in particular to a kind of double-mode imaging photothermolumineseence probe and preparation method thereof
And its application.
Background technique
The mankind and cancer struggle the past few decades in, can the diagnosing and treating accurately to cancer early stage be still one
A huge challenge.Since detection method sensitivity is low and non-specific, cause many cancers when being found to middle evening
Phase, at this time tumour has growed very big, and is transferred into each of body as metabolism has very big possibility
Organ and tissue.Therefore, it is very urgent can develop can multi-functional diagnostic and therapeutic method, to overcome single method
Deficiency.
With the development of nano material and nanosecond science and technology, developing has the multifunctional nano material of diagnosing and treating more next
More cause the research interest of people.On the one hand, integrate different imaging patterns be not only better than to single nano platform it is single
Imaging pattern, while can also more accurate boot diagnostic and treatment；On the other hand, since visible light penetration depth is limited, because
There is an urgent need to develop the luminous nano material in the near infrared region of penetration depth depth, the especially luminous nanoparticle in 2nd area of near-infrared for this
Son, and the nano material that 2nd area of near-infrared shines includes the nanoparticle of organic dyestuff doping, near-infrared quantum dots and upper conversion
Nanoparticle, but since the bio-toxicity of quantum dot is also controversial, and the luminous efficiency that up-conversion nano material is low
Limit its biologic applications.Also, the nano material of many multifunctions is played the part of in the treatment of disease as Nano medication
The carrier of drug or the characteristics of play itself alone under external physical stimulation, especially those are near infrared absorption
Inorganic nano-particle, they can convert near infrared light to heat and imaging and photo-thermal therapy in real time may be implemented.
Bismuth selenide (Bi2Se3) nano material is a kind of novel nano-material to grow up recent years, it can absorb close red
Outer smooth 808nm and be converted to thermal energy, Bi2Se3It is a kind of topological insulating materials, energy gap 0.3EV includes bismuth element in nanoparticle,
Atomic number is larger (Z=83), possesses high photoelectric absorption coefficient and X-ray attenuation coefficient, is much higher than iodine, gold, platinum.Therefore,
Their compound Bi2Se3Good effect may be shown in biomedicine field.However, Bi2Se3As nanometer diagnosis and treatment agent
In biologic applications, there is also many problems: being primarily due to Bi2Se3Unstability and easy to oxidize, limit in vitro and in vivo
Using；Secondly as lacking suitable surface modification also limits the ability that they reprint drug；Finally, how to construct close red
The luminous photo-thermal nanometer diagnosis and treatment agent in outer 2nd area, and the effect for enhancing its photo-thermal therapy to the greatest extent is also urgently to be resolved asks
Topic.
Summary of the invention
It is an object of the invention to overcome the above-mentioned deficiency of the prior art, provide a kind of double-mode imaging photothermolumineseence probe and
Preparation method, to solve existing bismuth selenide (Bi2Se3) nano material is unstable and the monistic technology of its biologic applications is asked
Topic.
In order to realize that the goal of the invention, one aspect of the present invention provide a kind of double-mode imaging photothermolumineseence probe.Including
Nucleome and the clad for being coated on nucleome, the nucleome are optothermal material, and the optothermal material includes bismuth selenide nano material, institute
The material for stating clad includes poly-dopamine, is combined with nir dye on the outer surface of the clad.
Another aspect of the present invention provides a kind of preparation method of double-mode imaging photothermolumineseence probe.The bimodulus at
As the preparation method of photothermolumineseence probe includes the following steps:
Photo-thermal nano material containing bismuth selenide is subjected to hybrid reaction in the auto polymerization reaction solution containing dopamine
Afterwards, it adds nir dye and carries out mixed processing, obtain double-mode imaging photothermolumineseence probe.
Another aspect of the invention provides a kind of nanometer of diagnosis and treatment agent.The nanometer diagnosis and treatment agent contain bimodulus of the present invention at
As photothermolumineseence probe or by double-mode imaging photothermolumineseence probe prepared by preparation method of the present invention.
Compared with prior art, double-mode imaging photothermolumineseence probe of the present invention, which uses, contains Bi2Se3Optothermal material is
Nucleome, so that the double-mode imaging photothermolumineseence probe can effectively absorb near infrared light and be converted to thermal energy and have height
Photoelectric absorption coefficient and X-ray attenuation coefficient；The nucleome, one side energy are coated using the clad containing poly-dopamine
It enough plays to Bi2Se3The protective effect of optothermal material improves Bi2Se3On the other hand the stability of optothermal material can also enhance
The connection function of nir dye improves the stability of nir dye connection；Moreover, the clad containing poly-dopamine can also
Enough the fuel factor of itself can play synergy photo-thermal effect between optothermal material nucleome, to assign the double-mode imaging photo-thermal
Luminescence probe has strong photo-thermal effect, so that the double-mode imaging photothermolumineseence probe has the imaging of 2nd area of near-infrared and CT imaging
Function can effectively inhibit the growth of tumour cell.
Double-mode imaging photothermolumineseence probe preparation method of the present invention by the auto polymerization reaction solution containing dopamine directly with
Photo-thermal nano material containing bismuth selenide carries out mixed processing and reacts, so that the poly- DOPA that polymerization reaction generates occurs for dopamine
Amine coats photo-thermal nano material, so that the nano material of core-shell structure is formed, so that the nucleome chemical property of core-shell structure
Stablize, and the clad containing poly-dopamine can also play synergy photo-thermal effect between optothermal material nucleome, to assign
The double-mode imaging photothermolumineseence probe is given with strong photo-thermal effect, and after being mixed with nir dye, can effectively made
Nir dye is connected on the surface of the poly-dopamine clad.And preparation method can effectively ensure that the double of preparation
The stabilization of photothermolumineseence probe structure and performance is imaged in mould, and condition is easily-controllable, effectively increases production efficiency, reduces economy
Cost.
Nanometer diagnosis and treatment agent of the present invention, due to containing double-mode imaging photothermolumineseence probe of the present invention, through can be used for
Boot diagnostic, and the double-mode imaging photothermolumineseence probe have strong photo-thermal effect, have 2nd area of near-infrared imaging and CT at
As function, therefore, it can be used as nanometer diagnosis and treatment drug, can effectively inhibit the growth of tumour cell.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples, in attached drawing:
Fig. 1 is the structural schematic diagram of double-mode imaging of embodiment of the present invention photothermolumineseence probe；
Fig. 2 is the process flow diagram of double-mode imaging of embodiment of the present invention photothermolumineseence probe preparation method；
Fig. 3 is the double-mode imaging photothermolumineseence probe and Bi that the embodiment of the present invention 1 provides2Se3The transmission electricity of nanoparticle
Mirror photo；Wherein, Fig. 3-a is the Bi for applying example 1 and providing2Se3The transmission electricity photo of nanoparticle, Fig. 3-b are what embodiment 1 provided
Double-mode imaging photothermolumineseence probe transmits electric photo；
Fig. 4 is the double-mode imaging photothermolumineseence probe that the embodiment of the present invention 1 provides and the phase that comparative example 1, comparative example 4 provide
Close the absorption spectrum curve figure of particle；Wherein, curve 1 is Bi in comparative example 12Se3Nanoparticle absorption spectrum curve, curve 2 are
Bi in comparative example 42Se3@PDA particle nanoparticle absorption spectrum curve, curve 3 are that double-mode imaging photothermolumineseence is visited in embodiment 1
Needle absorption spectrum curve, curve 4 are the absorption spectrum curve of 1 step d2 centrifuged supernatant of embodiment；
Fig. 5 is the double-mode imaging photothermolumineseence probe that the embodiment of the present invention 1 provides and the phase that comparative example 1, comparative example 4 provide
Close the spectral radiation curves figure of particle；Wherein, curve 1 is DYE spectral radiation curves in comparative example 3, and curve 2 is in embodiment 1
The double-mode imaging photothermolumineseence probe emission curve of spectrum；
Fig. 6 is the double-mode imaging photothermolumineseence probe experimental group that the embodiment of the present invention 1 provides and pair that comparative example 1-4 is provided
Than the cell survival rate for organizing external photo-thermal killing cell experiment each group.
Specific embodiment
In order to which technical problems, technical solutions and advantageous effects to be solved by the present invention are more clearly understood, below in conjunction with
Embodiment and attached drawing, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein only to
It explains the present invention, is not intended to limit the present invention.
The quality of each component noted in the disclosure of the embodiment of the present invention not only may refer to specifically containing for each component
Amount, can also indicate the proportionate relationship of quality between each component, therefore, as long as according to specification each component of the embodiment of the present invention
Content is scaled up or is reduced within specification of embodiment of the present invention scope of disclosure.Specifically, the embodiment of the present invention
Quality described in the specification can be mass unit well known to the chemical fields such as μ g, mg, g, kg.
On the one hand, the embodiment of the present invention provides a kind of double-mode imaging photothermolumineseence probe.The double-mode imaging photothermolumineseence
The structure of probe is as shown in Figure 1, Figure 3, is core-shell structure, nucleome 1 and the clad 2 for being coated on nucleome 1 is specifically included, in institute
That states clad 2 is combined with nir dye 3 on the outer surface of the nucleome 1.
Wherein, the nucleome 1 is optothermal material, and the optothermal material includes that bismuth selenide receives (Bi2Se3) rice material.In this way with
Contain Bi2Se3Optothermal material is as nucleome, so that the double-mode imaging photothermolumineseence probe can effectively absorb near-infrared
Light is simultaneously converted to thermal energy and with high photoelectric absorption coefficient and X-ray attenuation coefficient, has photo-thermal effect.In an embodiment
In, shown nucleome is flake nano structure, and the diameter of such as flake nano structure can be 50nm.In a particular embodiment,
The Bi2Se3For nanoparticle, transmission electron microscope photo is as shown in figure 3, such as Bi2Se3Nanometer sheet.In a particular embodiment, institute
State flake nano structure Bi2Se3Nanometer sheet, if nanometer sheet diameter is 50 nanometers, thickness is 2 nanometers average.
The material of shown clad 2 includes poly-dopamine, coats the nucleome 1 using the clad 2 containing poly-dopamine,
On the one hand it can play to Bi2Se3The protective effect of optothermal material improves Bi2Se3The stability of optothermal material, on the other hand also
The connection function of nir dye can be enhanced, improve the stability of nir dye connection；Third, the packet containing poly-dopamine
Coating 2 can also itself fuel factor synergy photo-thermal effect can be played between optothermal material nucleome 1, to assign described double
Photothermolumineseence probe, which is imaged, in mould has strong photo-thermal effect.In one embodiment, the thickness of the clad may be controlled to 8~10
Nanometer.
In another embodiment, the mass ratio of the nucleome 1 and the clad 2 may be controlled to 10:1.
The nir dye (DYE) 3 is incorporated in the outer surface of the clad 2.The nir dye 3 is due to being
It is directly incorporated on the surface of the clad 2 containing poly-dopamine, therefore, combination stability is good, and due to close red
The characteristic of outer dyestuff itself, can with clad 2 and containing playing synergy photo-thermal effect between bismuth selenide nanometer nucleome 1,
To assign the double-mode imaging photothermolumineseence probe with strong photo-thermal effect.
In one embodiment, the mass content of the nir dye 3 accounts for the photothermolumineseence nano-probe gross mass
5%.In a particular embodiment, the nir dye can with but not only include nir dye 1048.
In a further embodiment, double-mode imaging photothermolumineseence probe in the above embodiments further includes bio-compatible
The material of external coating is DSPE-mPEG.By adding the bio-compatible external coating, to enhance the double-mode imaging light
The biocompatibility of thermoluminescence probe.
Therefore, the probe of double-mode imaging photothermolumineseence described in the various embodiments described above is by being set as the cladding knot of core-shell type
Structure contains Bi by contained2Se3Between optothermal material nucleome 1, the clad 2 containing poly-dopamine and nir dye 3
Synergistic effect, effectively increases including Bi2Se3The stabilization and structural stability of photo-thermal nano material chemical property, and play photo-thermal
Effect enhancing, to assign the double-mode imaging photothermolumineseence probe with strong photo-thermal effect, so that the double-mode imaging photo-thermal
Luminescence probe has the nanometer diagnosis and treatment drug of 2nd area of near-infrared imaging and CT imaging function, can effectively inhibit the life of tumour cell
It is long.And it can be carried out by the correlated performance between optimization nucleome 1, clad 2 and nir dye 3, such as size, ingredient
Optimal control, can synergistic effect between further increasing nucleome 1, clad 2 and nir dye 3, to improve institute
State the photo-thermal effect of double-mode imaging photothermolumineseence probe.
On the other hand, on the basis of double-mode imaging photothermolumineseence probe described above, the embodiment of the invention also provides
A kind of preparation method of the double-mode imaging photothermolumineseence probe.The preparation of double-mode imaging photothermolumineseence probe of the embodiment of the present invention
Method flow is as shown in Fig. 2, it includes the following steps:
Photo-thermal nano material containing bismuth selenide mix simultaneously instead in the auto polymerization reaction solution containing dopamine
Ying Hou adds nir dye and carries out mixed processing, obtains double-mode imaging photothermolumineseence probe.
Wherein, the photo-thermal nano material is carried out to the mistake of mixed processing and reaction in the auto polymerization reaction solution of dopamine
Auto polymerization reaction can occur for Cheng Zhong, dopamine to generate poly-dopamine, to be coated on the photo-thermal nanometer material in reaction solution
Expect that surface forms clad.In one embodiment, the photo-thermal nano material and the dopamine are preferably 10 according to mass ratio:
1 ratio is added mixed processing.By the mixed proportion of both control, to realize that poly-dopamine coats the light completely
Hot nano material forms complete clad 2 as shown in Figure 1, and has thickness appropriate simultaneously, such as the thickness of clad
Control is 8-10 nanometers, to improve the photo-thermal nano material such as Bi being wrapped by2Se3The stability of optothermal material, and energy
Cooperate with Bi2Se3Optothermal material plays photo-thermal effect synergistic effect.In addition, the mixing and time for reacting should be adequately,
Such as 1 hour.
Specifically, the photo-thermal nano material is the light of nucleome 1 contained by double-mode imaging photothermolumineseence probe described above
Hot material no longer repeats the optothermal material correlated performance to save length.Wherein, the Bi2Se3It can be under
Bi in literary embodiment 12Se3Preparation method preparation.The dopamine can select dopamine hydrochloric acid reagent, and the auto polymerization is anti-
Answer solution can with but not just for PH=8 phosphate buffer solution, as long as enabling to dopamine that polymerization reaction occurs
Other solution are adapted to the embodiment of the present invention.
The addition of the nir dye can be incorporated on the surface of dopamine clad, to play itself and dopamine
Synergy photo-thermal effect is played between clad and photo-thermal nano material nucleome, to assign the double-mode imaging photothermolumineseence of preparation
Probe has strong photo-thermal effect.In one embodiment, the photo-thermal nano material and the nir dye can according to mass ratio
Think that the ratio of 20:1 is added the nir dye, or the mass content of the nir dye is made to account for described pair
The 5% of photothermolumineseence probe gross mass is imaged in mould, so that contaminating on the surface of dopamine clad in conjunction with suitable near-infrared
Material, to improve the synergistic function of the photo-thermal effect between them.Wherein, the nir dye is bimodulus described above
Nir dye 3 contained by photothermolumineseence probe is imaged.In addition, the time for the mixed processing that the nir dye carries out is added
It should be adequately such as 2 hours.
It further include being carried out to mixed liquor after nir dye is sufficiently mixed and is incorporated in the dopamine cover surface
The step of being separated by solid-liquid separation and washing, has obtained double-mode imaging photothermolumineseence probe.Wherein, separation of solid and liquid can with but not just for from
Heart separation, the method for washing, which can be, sufficiently washs sediment using deionized water such as washing three times, removes remaining mixing
Object solution.
It in a further embodiment, further include the double-mode imaging photothermolumineseence probe and DSPE-mPEG for obtaining upper step
Solution carry out mixed processing the step of.In this way, the DSPE-mPEG can be to described containing described in the nir dye
Clad is coated processing again, forms the double-mode imaging photothermolumineseence probe bio-compatible external coating, described in enhancing
The biocompatibility of double-mode imaging photothermolumineseence probe.In one embodiment, the double-mode imaging photothermolumineseence probe with it is described
DSPE-mPEG preferably can be added mixed processing according to mass ratio for the ratio of 1:1.
Therefore, the double-mode imaging photothermolumineseence probe preparation method passes through the control of processing step and process conditions, makes
The double-mode imaging photothermolumineseence probe that must be prepared is core-shell structure, effectively increases the chemistry of the photo-thermal nano material as nucleome
Performance is stablized, and the poly-dopamine clad that dopamine auto polymerization reaction generates can also itself fuel factor can be with photo-thermal material
Synergy photo-thermal effect is played between material nucleome and nir dye, so that assigning the double-mode imaging photothermolumineseence probe has
Strong photo-thermal effect.And preparation method condition is easily-controllable, effectively increases production efficiency, reduces economic cost.
In another aspect, the present invention is real on the basis of double-mode imaging photothermolumineseence probe described above and preparation method thereof
It applies example and additionally provides a kind of nanometer of diagnosis and treatment agent.The nanometer diagnosis and treatment agent contains double-mode imaging photothermolumineseence probe described above.When
So, processing contains except the double-mode imaging photothermolumineseence probe, can also contain and be conducive to the double-mode imaging photothermolumineseence spy
Needle is stable or effectively plays other reagents of other field of medicaments of its effect.Due to double-mode imaging photo-thermal as described above
Luminescence probe has the stability of structure and chemical property, and contains poly-dopamine clad, optothermal material by contained
Synergistic fuel factor is played between nucleome and nir dye and there is strong photo-thermal effect characteristic, therefore, nanometer diagnosis and treatment agent
The nanometer diagnosis and treatment drug that can be used as 2nd area of near-infrared imaging and CT imaging function, can effectively inhibit the growth of tumour cell.
Illustrated the present invention below by way of multiple specific embodiments embodiment double-mode imaging photothermolumineseence probe and its
Preparation method.
Embodiment 1
The present embodiment provides a kind of double-mode imaging photothermolumineseence probes and preparation method thereof.The double-mode imaging photothermolumineseence
The structure of probe is as shown in Figure 1, its transmission electron microscope photo is as shown in Figure 2.Bi2Se3Nanoparticle nucleome 1, be coated on it is described
Bi2Se3The dopamine clad 2 of nanoparticle nucleome 1 and the DYE-PEG for being incorporated in 2 outer surface of dopamine clad are closely red
Outer dyestuff functional component 3.
The preparation method of the double-mode imaging photothermolumineseence probe includes the following steps:
D1: synthesis Bi2Se3Nanometer sheet
Sodium borohydride is reacted first to obtain sodium hydrogen selenide solution by 2:1 with selenium powder；Then 0.5 gram of polyvinyl pyrrole is weighed
Alkanone is dissolved in 50 milliliters of glycerine, is added to 200 milliliters of round-bottomed flask, is being added to bismuth nitrate, is being stirred at room temperature, and is added
Heat is to 200 degrees Celsius；It is subsequently added into sodium hydrogen selenide solution, solution blackening, the bismuth selenide for forming polyvinylpyrrolidone cladding is received
Rice corpuscles reacts 10 minutes, and temperature drops to room temperature；Finally, product 12000rpm is centrifuged 10 minutes, washing three times, is dried in vacuo
Case is dried for standby.Its transmission electron microscope photo is as shown in Figure 3.
D2: the Bi of synthesis dopamine cladding2Se3Nanoparticle (Bi2Se3@PDA@DYE)
The dopamine hydrochloric acid reagent for weighing 50 milligrams, is dissolved in the phosphate buffer solution of 10 milliliters of PH=8, weighs
The Bi of 5mg2Se3Powder is added, and is stirred to react 1 hour, nir dye DYE is then added, and in stirring 2 hours, product was centrifuged,
It is washed with deionized three times.
D3: the nanoparticle Bi of DSPE-mPEG modification is prepared2Se3@PDA@DYE-PEG
The DSPE-mPEG for weighing 2mg is dissolved in 5ml deionized water, and the Bi of 2mg d2 preparation is then added2Se3@PDA@
DYE is stirred 24 hours, is then centrifuged for, is dispersed in phosphate buffer solution.
Embodiment 2
The present embodiment provides a kind of double-mode imaging photothermolumineseence probes and preparation method thereof.The double-mode imaging photothermolumineseence
The structure of probe is as shown in Figure 1, its transmission electron microscope photo is as shown in Figure 2.Bi2Se3Nanoparticle nucleome 1, be coated on it is described
Bi2Se3The dopamine clad 2 of nanoparticle nucleome 1 and the DYE-PEG for being incorporated in 2 outer surface of dopamine clad are closely red
Outer dyestuff functional component 3.
The preparation method of the double-mode imaging photothermolumineseence probe includes the following steps:
D1: synthesis Bi2Se3Nanometer sheet
Sodium borohydride is reacted first to obtain sodium hydrogen selenide solution by 2:1 with selenium powder；Then 0.5 gram of polyvinyl pyrrole is weighed
Alkanone is dissolved in 50 milliliters of glycerine, is added to 200 milliliters of round-bottomed flask, is being added to bismuth nitrate, is being stirred at room temperature, and is added
Heat is to 200 degrees Celsius；It is subsequently added into sodium hydrogen selenide solution, solution blackening, the bismuth selenide for forming polyvinylpyrrolidone cladding is received
Rice corpuscles reacts 10 minutes, and temperature drops to room temperature；Finally, product 12000rpm is centrifuged 10 minutes, washing three times, is dried in vacuo
Case is dried for standby.Its transmission electron microscope photo is as shown in Figure 3.
D2: the Bi of synthesis dopamine cladding2Se3Nanoparticle (Bi2Se3@PDA@DYE)
The dopamine hydrochloric acid reagent for weighing 50 milligrams, is dissolved in the phosphate buffer solution of 10 milliliters of PH=8, weighs
The Bi of 5mg2Se3Powder is added, and is stirred to react 1 hour, then according to Bi2Se3The ratio that mass ratio with nir dye is 20:1
Nir dye DYE is added in example, and in stirring 2 hours, product centrifugation was washed with deionized three times.
D3: the nanoparticle Bi of DSPE-mPEG modification is prepared2Se3@PDA@DYE-PEG
It weighs enough DSPE-mPEG to be dissolved in 5ml deionized water, the Bi of 2mg d2 preparation is then added2Se3@PDA@
DYE is stirred 24 hours, is then centrifuged for, is dispersed in phosphate buffer solution.
Comparative example 1
The Bi prepared according to the step d1 of embodiment 12Se3Nanoparticle.
Comparative example 2
Poly-dopamine in single 1 step d2 of embodiment is provided.
Comparative example 3
DYE in single 1 step d2 of embodiment is provided.
Comparative example 4
The Bi prepared in 1 step d2 of embodiment is provided2Se3@PDA particle.
The test of double-mode imaging photothermolumineseence probe correlated performance
By the double-mode imaging photothermolumineseence probe that embodiment 1-2 is provided and the related substances that comparative example provides respectively according to such as
Lower method carries out following correlated performance test and experiment:
1. transmission electron microscope analysis: the double-mode imaging photothermolumineseence probe that embodiment 1-2 is provided carries out transmission electron microscope analysis,
Wherein, the double-mode imaging photothermolumineseence probe that embodiment 1 provides transmits electric photo as shown in Fig. 3-b, step d1 preparation
Bi2Se3The transmission electricity photo of nanoparticle is as shown in Fig. 3-a.In addition, the double-mode imaging photothermolumineseence probe that embodiment 2 provides is saturating
Radio photo is approximate with Fig. 3-b.Electric photo is transmitted it is found that the Bi by those2Se3Nanoparticle is nanometer sheet, nanometer sheet diameter
For 50 rans, and double-mode imaging photothermolumineseence probe is nanoscale
2. absorption spectroanalysis: double-mode imaging photothermolumineseence probe and comparative example 1,4 that embodiment 1-2 is provided are provided
Substance carries out absorption spectroanalysis respectively.Wherein, the double-mode imaging photothermolumineseence probe of the offer of embodiment 1 and comparative example 1, comparison
The absorption spectrum curve difference of the particle provided in example 4 is as shown in Figure 4.In addition, the double-mode imaging photothermolumineseence that embodiment 2 provides
Probe absorption spectrum curve is approximate with Fig. 4 curve 3.Correlation curve 1-4 is it is found that double-mode imaging photothermolumineseence provided in this embodiment
Probe has relatively strong optical absorption characteristics in the section wavelength 900-1100.
3. emission spectrographic analysis: double-mode imaging photothermolumineseence probe and comparative example 1-4 that embodiment 1-2 is provided are provided
Substance carries out emission spectrographic analysis respectively.Wherein, it is mentioned in the double-mode imaging photothermolumineseence probe and comparative example 3 that embodiment 1 provides
The spectral radiation curves difference of the DYE of confession is as shown in Figure 5.In addition, the double-mode imaging photothermolumineseence probe that other embodiments provide
Spectral radiation curves are approximate with Fig. 3 curve 2, and the substance spectral radiation curves that comparative example provides are weak with curve 2.Comparison transmitting
The curve of spectrum is it is found that double-mode imaging photothermolumineseence probe emission spectrum provided in this embodiment is better than the hair of substance in comparative example
Penetrate spectrum.
4. external photo-thermal kills cell experiment: by the embodiment 1-2 double-mode imaging photothermolumineseence probe provided and comparative example
The substance that 1-4 is provided carries out external photo-thermal killing cell experiment respectively, and specific method is to kill cell experiment according to existing photo-thermal
Operation.Wherein, the contrast groups each group that the double-mode imaging photothermolumineseence probe experimental group and comparative example 1-4 that embodiment 1 provides provide
Cell survival rate it is as shown in Figure 6；Wherein, the cell survival rate of 1 experimental group of embodiment and 1 contrast groups of comparative example constitutes significantly
Sex differernce.The cell survival rate and Fig. 6 of the double-mode imaging photothermolumineseence probe experimental group of other embodiments offer are further provided
The survival rate of middle 1 experimental group of embodiment is close.By external photo-thermal killing cell experiment result it is found that bimodulus provided in this embodiment
Photothermolumineseence probe, which is imaged, has excellent photo-thermal effect, can be used as nanometer diagnosis and treatment drug, realize and effectively inhibit tumour cell
Growth.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (9)
1. a kind of double-mode imaging photothermolumineseence probe, including nucleome and the clad for being coated on nucleome, it is characterised in that: the core
Body is optothermal material, and the optothermal material includes bismuth selenide nano material, and the material of the clad includes poly-dopamine, in institute
It states and is combined with nir dye on the outer surface of clad.
2. double-mode imaging photothermolumineseence probe according to claim 1, it is characterised in that: the matter of the nucleome and clad
Amount is than being 10:1.
3. double-mode imaging photothermolumineseence probe according to claim 1, it is characterised in that: the quality of the nir dye
Content accounts for the 5% of the double-mode imaging photothermolumineseence probe gross mass；And/or
The nucleome is flake nano structure, and the diameter of the flake nano structure is 50 nanometers；And/or
The clad with a thickness of 8-10 nanometers.
4. double-mode imaging photothermolumineseence probe according to claim 1-3, it is characterised in that: the near-infrared dye
Material includes nir dye 1048.
5. double-mode imaging photothermolumineseence probe according to claim 1-3, it is characterised in that: the double-mode imaging
Photothermolumineseence probe further includes bio-compatible external coating, and the bio-compatible external coating is coated on to be contaminated containing the near-infrared
The clad of material, the material of the bio-compatible external coating are DSPE-mPEG.
6. a kind of preparation method of double-mode imaging photothermolumineseence probe, which comprises the steps of:
After photo-thermal nano material containing bismuth selenide is carried out hybrid reaction in the auto polymerization reaction solution containing dopamine, then
Nir dye is added and carries out mixed processing, obtains double-mode imaging photothermolumineseence probe.
7. preparation method according to claim 6, it is characterised in that: further include by double-mode imaging photothermolumineseence probe with
The solution of DSPE-mPEG carries out the step of mixed processing.
8. according to the described in any item preparation methods of claim 6-7, it is characterised in that: the photo-thermal nano material and described more
The mass ratio of bar amine is 10:1；
The mass ratio of the photo-thermal nano material and the nir dye is 20:1.
9. a kind of nanometer of diagnosis and treatment agent, it is characterised in that: visited containing the described in any item double-mode imaging photothermolumineseences of claim 1-5
Needle or the double-mode imaging photothermolumineseence probe prepared by the described in any item preparation methods of claim 6-8.
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