CN106860865A - A kind of Ni0.85Se nano materials and its preparation method and application - Google Patents
A kind of Ni0.85Se nano materials and its preparation method and application Download PDFInfo
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 88
- 239000011669 selenium Substances 0.000 claims abstract description 76
- 239000003446 ligand Substances 0.000 claims abstract description 10
- 238000007626 photothermal therapy Methods 0.000 claims abstract description 8
- 239000003937 drug carrier Substances 0.000 claims abstract description 5
- AOJJSUZBOXZQNB-TZSSRYMLSA-N Doxorubicin Chemical compound O([C@H]1C[C@@](O)(CC=2C(O)=C3C(=O)C=4C=CC=C(C=4C(=O)C3=C(O)C=21)OC)C(=O)CO)[C@H]1C[C@H](N)[C@H](O)[C@H](C)O1 AOJJSUZBOXZQNB-TZSSRYMLSA-N 0.000 claims description 28
- 229940079593 drug Drugs 0.000 claims description 26
- 239000003814 drug Substances 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 19
- 239000007864 aqueous solution Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 229940009456 adriamycin Drugs 0.000 claims description 12
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- NLZOGIZKBBJWPB-UHFFFAOYSA-N [Na].[SeH2] Chemical compound [Na].[SeH2] NLZOGIZKBBJWPB-UHFFFAOYSA-N 0.000 claims description 7
- 150000002815 nickel Chemical class 0.000 claims description 6
- 229920002125 Sokalan® Polymers 0.000 claims description 5
- 239000004584 polyacrylic acid Substances 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 4
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 4
- 238000011275 oncology therapy Methods 0.000 claims description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 4
- 239000012279 sodium borohydride Substances 0.000 claims description 4
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 4
- 239000012498 ultrapure water Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- KIUKXJAPPMFGSW-DNGZLQJQSA-N (2S,3S,4S,5R,6R)-6-[(2S,3R,4R,5S,6R)-3-Acetamido-2-[(2S,3S,4R,5R,6R)-6-[(2R,3R,4R,5S,6R)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylic acid Chemical compound CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 KIUKXJAPPMFGSW-DNGZLQJQSA-N 0.000 claims description 2
- 102000009027 Albumins Human genes 0.000 claims description 2
- 108010088751 Albumins Proteins 0.000 claims description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 2
- VSJKWCGYPAHWDS-FQEVSTJZSA-N camptothecin Chemical compound C1=CC=C2C=C(CN3C4=CC5=C(C3=O)COC(=O)[C@]5(O)CC)C4=NC2=C1 VSJKWCGYPAHWDS-FQEVSTJZSA-N 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 229920002674 hyaluronan Polymers 0.000 claims description 2
- 229960003160 hyaluronic acid Drugs 0.000 claims description 2
- 229940078494 nickel acetate Drugs 0.000 claims description 2
- IPLJNQFXJUCRNH-UHFFFAOYSA-L nickel(2+);dibromide Chemical compound [Ni+2].[Br-].[Br-] IPLJNQFXJUCRNH-UHFFFAOYSA-L 0.000 claims description 2
- BFSQJYRFLQUZKX-UHFFFAOYSA-L nickel(ii) iodide Chemical compound I[Ni]I BFSQJYRFLQUZKX-UHFFFAOYSA-L 0.000 claims description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 2
- ULGZDMOVFRHVEP-RWJQBGPGSA-N Erythromycin Chemical compound O([C@@H]1[C@@H](C)C(=O)O[C@@H]([C@@]([C@H](O)[C@@H](C)C(=O)[C@H](C)C[C@@](C)(O)[C@H](O[C@H]2[C@@H]([C@H](C[C@@H](C)O2)N(C)C)O)[C@H]1C)(C)O)CC)[C@H]1C[C@@](C)(OC)[C@@H](O)[C@H](C)O1 ULGZDMOVFRHVEP-RWJQBGPGSA-N 0.000 claims 2
- 108010006654 Bleomycin Proteins 0.000 claims 1
- 229960001561 bleomycin Drugs 0.000 claims 1
- OYVAGSVQBOHSSS-UAPAGMARSA-O bleomycin A2 Chemical compound N([C@H](C(=O)N[C@H](C)[C@@H](O)[C@H](C)C(=O)N[C@@H]([C@H](O)C)C(=O)NCCC=1SC=C(N=1)C=1SC=C(N=1)C(=O)NCCC[S+](C)C)[C@@H](O[C@H]1[C@H]([C@@H](O)[C@H](O)[C@H](CO)O1)O[C@@H]1[C@H]([C@@H](OC(N)=O)[C@H](O)[C@@H](CO)O1)O)C=1N=CNC=1)C(=O)C1=NC([C@H](CC(N)=O)NC[C@H](N)C(N)=O)=NC(N)=C1C OYVAGSVQBOHSSS-UAPAGMARSA-O 0.000 claims 1
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- YWMAPNNZOCSAPF-UHFFFAOYSA-N Nickel(1+) Chemical compound [Ni+] YWMAPNNZOCSAPF-UHFFFAOYSA-N 0.000 abstract 1
- 229940006444 nickel cation Drugs 0.000 abstract 1
- -1 selenium anion Chemical class 0.000 abstract 1
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- STQGQHZAVUOBTE-UHFFFAOYSA-N 7-Cyan-hept-2t-en-4,6-diinsaeure Natural products C1=2C(O)=C3C(=O)C=4C(OC)=CC=CC=4C(=O)C3=C(O)C=2CC(O)(C(C)=O)CC1OC1CC(N)C(O)C(C)O1 STQGQHZAVUOBTE-UHFFFAOYSA-N 0.000 description 1
- 206010008342 Cervix carcinoma Diseases 0.000 description 1
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- STQGQHZAVUOBTE-VGBVRHCVSA-N daunorubicin Chemical compound O([C@H]1C[C@@](O)(CC=2C(O)=C3C(=O)C=4C=CC=C(C=4C(=O)C3=C(O)C=21)OC)C(C)=O)[C@H]1C[C@H](N)[C@H](O)[C@H](C)O1 STQGQHZAVUOBTE-VGBVRHCVSA-N 0.000 description 1
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- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
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Classifications
-
- 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
- A61K45/00—Medicinal preparations containing active ingredients not provided for in groups A61K31/00 - A61K41/00
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K49/00—Preparations for testing in vivo
- A61K49/22—Echographic preparations; Ultrasound imaging preparations ; Optoacoustic imaging preparations
- A61K49/221—Echographic preparations; Ultrasound imaging preparations ; Optoacoustic imaging preparations characterised by the targeting agent or modifying agent linked to the acoustically-active agent
-
- 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
- A61K9/5115—Inorganic compounds
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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
- A61K9/5138—Organic macromolecular compounds; Dendrimers obtained by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyvinyl pyrrolidone, poly(meth)acrylates
-
- 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
- A61K9/5161—Polysaccharides, e.g. alginate, chitosan, cellulose derivatives; Cyclodextrin
-
- 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
- A61K9/5169—Proteins, e.g. albumin, gelatin
Abstract
The invention discloses a kind of Ni0.85Se nano materials and its preparation method and application, it obtain dispersiveness Ni well by the presence of hydrophilic ligand, by lower valency selenium anion and nickel cation stirring hybrid reaction, being then centrifuged for, dialysing0.85Se nano materials.Gained nano material of the invention has very strong near infrared absorption characteristic, and near infrared light effectively can be converted into heat energy, with very strong photo-thermal conversion efficiency and preferable photo and thermal stability, can be used in the photo-thermal therapy of tumour；And present invention gained nano material is also used as pharmaceutical carrier for the chemotherapy of tumour, or for photoacoustic imaging, so as to be implemented as the therapeutic alliance as guiding photo-thermal therapy and chemotherapy.
Description
Technical field
Prepared the invention belongs to nano material and biomedical sector, and in particular to a kind of Ni0.85Se nano materials and its
Preparation method and application.
Background technology
In recent years, nano material has obtained the attention of scientist in the application of biomedical aspect, especially medical diagnosis on disease,
The aspects such as prevention from suffering from the diseases, drug therapy all obtain very big progress.Nano material causes single in the development of biomedical aspect
Realize that various functions become possible to simultaneously in system, can simultaneously realize that the multi-functional nanometer material for diagnosing and treating is current
One of focus of research.The realization of diagnosis and treatment integration, can significantly improve the therapeutic effect of tumour.
Near infrared light have the advantages that penetration into tissue it is strong, to tissue almost not damaged, be a kind of in biomedical sector
Preferable light source.Near infrared light wants to play in vivo diagnosis and treatment effect, it is necessary to there is good absorption to receive near infrared light
Rice material converts thereof into heat energy, so as to can be used for the photoresponse treatment of tumor locus and real time imagery.It would therefore be highly desirable to develop base
In the nano material of near infrared light response, and possess it while realizing that (such as optical dynamic therapy, photo-thermal therapy) is treated in photoresponse
With the ability of photoresponse imaging (such as optical imagery, photoacoustic imaging).
Ni0.85Se is a kind of critically important semi-conducting material, there is excellent electromagnetism and physical and chemical performance, is existed
The fields such as solar cell, catalysis, ultracapacitor, sensor, conducting material have a wide range of applications.At present,
Ni0.85The synthetic method of Se mainly has hydrothermal/solvent thermal synthesis method, solid-phase synthesis, ultrasonic, machine-alloying, change
Learn vapour deposition process etc..Complicated synthetic method, cumbersome surface modification, poor biocompatibility etc., limits Ni0.85Se
Application of the nano material in biomedical aspect.Up to the present, also without Ni0.85Se nano materials tumor thermal therapy,
Report in terms of chemotherapy and photoacoustic imaging.Therefore, a kind of simple method one-step synthesis favorable dispersibility of green is developed
Ni0.85Se nano materials, and study it there is important researching value in the application of biomedical aspect.
The content of the invention
The present invention is to avoid the weak point existing for above-mentioned prior art, there is provided a kind of Ni0.85Se nano materials and
Its preparation method and application, it is intended to there is good biocompatibility and the preferably Ni of dispersiveness by one-step synthesis method0.85Se
Nano material, and use it for the photo-thermal therapy and chemotherapy and photoacoustic imaging of tumour.
The present invention solves technical problem, adopts the following technical scheme that：
The present invention discloses a kind of Ni first0.85Se nano materials, its particle diameter is 2~50nm, and there is hydrophilic ligand on surface
Modification.Described hydrophilic ligand is at least one in albumin, polyacrylic acid and hyaluronic acid.
Above-mentioned Ni0.85The preparation method of Se nano materials, comprises the following steps：
(1) under inert gas shielding, selenium powder and sodium borohydride are dissolved in water, are well mixed, be then restored to molten
Liquid is colourless, obtains sodium hydrogen selenide solution；
(2) mixed aqueous solution of hydrophilic ligand and nickel salt is added drop-wise in the sodium hydrogen selenide solution, then at room temperature
Stirring 5min~2h, centrifugation obtains Ni0.85Se nano materials；
(3) by the Ni0.85Se nano materials are placed in ultra-pure water the 24h that dialyses, and a water is changed every 3~4h, that is, obtain
Ni0.85The aqueous solution of Se nano materials.
Wherein, the nickel salt is at least one in nickel chloride, nickel acetate, nickel nitrate, nickelous bromide and nickel iodide.
Wherein, the ratio between amount of material of selenium powder and sodium borohydride is 1：3, the ratio between amount of material of nickel salt and selenium powder is 1：1.
The present invention further discloses above-mentioned Ni0.85Se applications to nanostructures, i.e., for as pharmaceutical carrier, passing through
Suction-operated loads cancer therapy drug；And/or for as photo-thermal therapy agent；And/or for the contrast agent as photoacoustic imaging.
Wherein, the cancer therapy drug is cis-platinum, adriamycin, camptothecine, daunorubicin, vincaleukoblastinum, TAM and Bo Lai
At least one in mycin.
Beneficial effects of the present invention are embodied in：
1st, the present invention passes through the one-step synthesis method Ni of favorable dispersibility under conditions of normal-temperature water phase0.85Se nanometers of material
Material, synthetic method is simply green, is easy to industrialization；
2nd, the Ni prepared by the present invention0.85Se nano materials have good biocompatibility, have near infrared region
Stronger absorption, there is photo-thermal conversion efficiency higher, and with good photo and thermal stability, the photo-thermal that can be used for tumour is controlled
Treatment, photoacoustic imaging；
3rd, the Ni prepared by the present invention0.85Se nano materials can be as pharmaceutical carrier, to anticancer by way of absorption
Medicine is loaded, gained Ni0.85Se Nano medication compounds have the insoluble drug release that pH is responded, and can be used for the chemotherapy of tumour.
Brief description of the drawings
Fig. 1 is the Ni that hydrophilic ligand modification is whether there is in embodiment 1 and embodiment 20.85Se nano materials are disperseed in water
The contrast of property；
Fig. 2 is the gained Ni of embodiment 20.85The x-ray diffraction pattern of Se nano materials；
Fig. 3 is the gained Ni of embodiment 20.85The transmission electron microscope picture of Se nano materials；
Fig. 4 is various concentrations Ni0.85The UV-visible absorption spectrum of the aqueous solution of Se nano materials；
Fig. 5 is various concentrations Ni0.85The aqueous solution of Se nano materials irradiates the heating curve of 10min under 808nm laser
Figure；
Fig. 6 is Ni0.85The aqueous solution of Se nano materials irradiates the light thermostable effect figure of 5 times repeatedly under 808nm laser；
Fig. 7 is injection Ni in Mice Body0.85Photoacoustic imaging comparison diagram before and after Se nano materials；
Fig. 8 is free adriamycin, Ni0.85Se Nano medications compound is under the phosphate buffer that pH is 7.4 and 5.0
Drug release patterns；
Fig. 9 is that mtt assay characterizes free adriamycin, Ni after pre-irradiation0.85Se nano materials and Ni0.85Se Nano medications are combined
Thing is to Hela cytoactives figure (a is that laser irradiates 0min, and b is that laser irradiates 5min).
Specific embodiment
Embodiments of the invention are elaborated below, following embodiments are entered under premised on technical solution of the present invention
Row is implemented, and gives detailed implementation method and specific operating process, but protection scope of the present invention is not limited to following realities
Apply example.
The Ni that embodiment 1, surface is modified without hydrophilic ligand0.85The preparation of Se nano materials
(1) under inert gas shielding, 0.1mmol selenium powders and 0.3mmol sodium borohydrides are dissolved in 80mL water, are mixed
Uniformly, it is restored to solution colourless, obtains sodium hydrogen selenide solution；
(2) step (1) gained selenium hydrogen will in the mixed solution of 0.1mmol nickel chlorides dissolving 20mL ultra-pure waters, be added dropwise over
Change sodium solution, 5min is stirred at room temperature, be centrifuged, obtain Ni0.85Se nano materials
(3) by Ni0.85Se nano materials are placed in ultra-pure water the 24h that dialyses, and a water is changed every 3~4h, that is, obtain black
Ni0.85The aqueous solution of Se nano materials.
Embodiment 2, surface has the Ni that polyacrylic acid is modified0.85The preparation of Se nano materials
(1) under inert gas shielding, 0.1mmol selenium powders and 0.3mmol sodium borohydrides are dissolved in 80mL water, are mixed
Uniformly, it is restored to solution colourless, obtains sodium hydrogen selenide solution；
(2) 0.1mmol nickel chlorides are dissolved in the mixed solution of 100 μ L polyacrylic acid solutions and 20mL ultra-pure waters, by
Step (1) gained sodium hydrogen selenide solution is added dropwise to, 5min is stirred at room temperature, be centrifuged, obtain Ni0.85Se nano materials
(3) by Ni0.85Se nano materials are placed in ultra-pure water the 24h that dialyses, and a water is changed every 3~4h, that is, obtain black
Ni0.85The aqueous solution of Se nano materials.
As shown in figure 1, comparative example 1 (right side sample bottle in figure) and embodiment 2 (left side sample bottle in figure) are obtained
Ni0.85The aqueous solution of Se nano materials understands that surface does not have the Ni that hydrophilic ligand is modified0.85Se nano materials are in water
Dispersiveness is very poor, in precipitated form, and has the Ni of polyacrylic acid modification0.85Se nano materials have good dispersiveness in water.
Fig. 2 is the gained Ni of embodiment 20.85The x-ray diffraction pattern of Se nano materials, card corresponding with standard card 18-0888
Bright product is Ni0.85Se。
Fig. 3 is the gained Ni of embodiment 20.85The transmission electron microscope picture of Se nano materials, it can be seen that primer size is homogeneous, averagely
Particle diameter is in 10nm or so.
Fig. 4 is various concentrations Ni0.85The UV-visible absorption spectrum of the aqueous solution of Se nano materials.As can be seen that
Under relatively low concentration, Ni0.85Se nano materials just have near infrared absorption higher, show that it can be used near infrared light induction
Photo-thermal therapy, photoacoustic imaging.
Embodiment 3, photo-thermal heats up and tests
Take the Ni of various concentrations (0~500 μM) in 3mL embodiments 20.85The aqueous solution of Se nano materials is placed in granularity pond
In, by the probe immersion solution of digital display thermometer, with 808nm lasers with the power illumination 10min of 2W, recorded in every 10 seconds
Temperature for solution, test various concentrations Ni0.85The photo-thermal heating curve of Se nano materials, is as a result shown in Fig. 5.As can be seen that
Under the irradiation of 808nm laser, Ni0.85Se nano materials can reach temperature higher under relatively low concentration, show Ni0.85Se
Nano material can apply to the photo-thermal therapy of tumour.
Fig. 6 is Ni0.85The Se nano materials aqueous solution irradiates the light thermostable effect figure of 5 times repeatedly under 808nm laser.Tool
Body takes the Ni of 340 μM of 3mL concentration0.85The aqueous solution of Se nano materials is placed in granularity pond, then with 808nm lasers with 2W's
Power illumination 10min, then turns off 808nm lasers, allows it to naturally cool to initial temperature, is remembered with thermometer in the process
Record the change of temperature, so circulation 5 times.As can be seen that Ni0.85Se nano materials have good photo and thermal stability.
Embodiment 4, Ni0.85The live body photoacoustic imaging of Se nano materials
Take 100 μ L Ni0.85The aqueous solution (concentration is 5M) of Se nano materials is by intravenous injection to being inoculated with human cervical cancer 1
The female BAl BIc of tumour/C nude mices (body weight is 20g) in vivo, and carries out photoacoustic imaging scanning after 0h, 4h is injected to it, with
This size to observe the change and optoacoustic intensity level of injecting front and rear mouse tumor image areas.
Fig. 7 is injection Ni in Mice Body0.85Photoacoustic imaging comparison diagram before and after Se nano materials, it can be seen that without injection
Ni0.85During Se nano materials, mouse tumor position can only see very faint photoacoustic signal；And inject Ni0.85Se nano materials
After 4h, mouse tumor locus it can be seen that very strong photoacoustic signal, shows Ni0.85Se nano materials can be as tumour
Photoacoustic imaging contrast agent.
Embodiment 5, Ni0.85The preparation of Se Nano medication compounds
By the Ni of 3mg0.85Se nano materials and 0.3mg adriamycins are dispersed in 3mL phosphate buffers (pH=7.4),
Then it is placed on magnetic stirring apparatus, lucifuge stirring 24h.10min is centrifuged with the rotating speed of 9000rpm/min again, milli-Q water is used
For several times, unadsorbed Doxorubicin solution is separated, that is, obtains Ni0.85Se Nano medication compounds, it is dispersed in 3mL phosphoric acid again
In salt buffer (pH=7.4), preserve stand-by at 4 DEG C of lucifuge.
Take the Ni of the above-mentioned preparations of 1mL0.85Se Nano medication compounds are placed in bag filter, are then individually placed to equipped with 30mL
During pH value is the centrifuge tube of 7.4 and 5.0 phosphate buffer, then it is placed in 37 DEG C of shaking table.At regular intervals, Cong Zhongqu
Go out 3mL supernatants, and be added thereto to the phosphate solution of equivalent.Calculated by measuring the fluorescent value of adriamycin in supernatant
The release conditions of different adriamycins.For the ease of comparing, test and 1mL Ni0.85Contained adriamycin in Se Nano medication compounds
Insoluble drug release situation of the pure Doxorubicin solution of equivalent under pH value 7.4.
Fig. 8 is free adriamycin, Ni0.85Se Nano medications compound is under the phosphate buffer that pH is 7.4 and 5.0
Drug release patterns, it can be seen that Ni0.85Se Nano medication compounds, it is possible to achieve the insoluble drug release of pH responses, pH value is got over
It is low, insoluble drug release it is more.Show Ni0.85Se can be used for the chemotherapy of tumour as pharmaceutical carrier.
Fig. 9 is that mtt assay characterizes free adriamycin, Ni after pre-irradiation0.85Se nano materials and Ni0.85Se Nano medications are combined
Thing is to Hela cytoactives figure (a is that laser irradiates 0min, and b is that laser irradiates 5min).
Specifically test mode is：By the aqueous solution of free adriamycin, Ni0.85The Se nano materials aqueous solution and Ni0.85Se nanometers
Medicinal composition is separately added into culture medium, and culture medium a, b, c are designated as respectively.The concentration of adriamycin and training in wherein culture medium a
Support Ni in base c0.85The concentration of adriamycin is identical in Se Nano medication compounds, Ni in culture medium b0.85The concentration of Se nano materials
With Ni in culture medium c0.85Se Nano medication compounds Ni0.85The concentration of Se nano materials is consistent.Then 808nm laser is used respectively
Irradiation 0min and 5min.
In Fig. 9 a during laser irradiation 0min, dissociate adriamycin and Ni0.85Se Nano medication compound water solutions are thin to Hela
The influence of born of the same parents is close, and Ni0.85The Se nano materials aqueous solution is minimum to Hela impact cells.Knowable to Fig. 9 b, 808nm laser is used
After with 2W power illuminations 5min, under comparable sodium, Ni0.85Se Nano medications compound compares Ni0.85Se nano materials, free Ah
The cell killing of mycin is bigger, generates 1+1>2 effect, shows Ni0.85Se Nano medications compound is to photo-thermal-chemotherapy combined
Treatment tumour has good curative effect.
Exemplary embodiment of the invention is the foregoing is only, is not intended to limit the invention, it is all of the invention
Any modification, equivalent and improvement made within spirit and principle etc., should be included within the scope of the present invention.
Claims (7)
1. a kind of Ni0.85Se nano materials, it is characterised in that：The Ni0.85The particle diameter of Se nano materials is 2~50nm, described
Ni0.85The surface of Se nano materials has hydrophilic ligand to modify.
2. Ni according to claim 10.85Se nano materials, it is characterised in that：Described hydrophilic ligand be albumin,
At least one in polyacrylic acid and hyaluronic acid.
3. the Ni described in a kind of claim 1 or 20.85The preparation method of Se nano materials, it is characterised in that comprise the following steps：
(1) under inert gas shielding, selenium powder and sodium borohydride are dissolved in water, be well mixed, be then restored to solution without
Color, obtains sodium hydrogen selenide solution；
(2) mixed aqueous solution of hydrophilic ligand and nickel salt is added drop-wise in the sodium hydrogen selenide solution, is then stirred at room temperature
5min~2h, centrifugation obtains Ni0.85Se nano materials；
(3) by the Ni0.85Se nano materials are placed in ultra-pure water the 24h that dialyses, and a water is changed every 3~4h, that is, obtain
Ni0.85The aqueous solution of Se nano materials.
4. preparation method according to claim 3, it is characterised in that：The nickel salt be nickel chloride, nickel acetate, nickel nitrate,
At least one in nickelous bromide and nickel iodide.
5. preparation method according to claim 3, it is characterised in that：The ratio between amount of material of selenium powder and sodium borohydride is 1：
3, the ratio between amount of material of nickel salt and selenium powder is 1：1.
6. the Ni described in a kind of claim 1 or 20.85Se applications to nanostructures, it is characterised in that：For as pharmaceutical carrier,
Cancer therapy drug is loaded by suction-operated；And/or for as photo-thermal therapy agent；And/or for the radiography as photoacoustic imaging
Agent.
7. application according to claim 6, it is characterised in that：The cancer therapy drug is cis-platinum, adriamycin, camptothecine, soft
At least one in erythromycin, vincaleukoblastinum, TAM and bleomycin.
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| CN112619670A (en) * | 2020-12-22 | 2021-04-09 | 台州学院 | Preparation method of Ni85Se 100/carbon nanotube composite |
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| CN112619670A (en) * | 2020-12-22 | 2021-04-09 | 台州学院 | Preparation method of Ni85Se 100/carbon nanotube composite |
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