CN116395747A - Manganese tetraoxide-silver sulfide Janus structure nanocomposite and preparation method thereof - Google Patents
Manganese tetraoxide-silver sulfide Janus structure nanocomposite and preparation method thereof Download PDFInfo
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- -1 Manganese tetraoxide-silver sulfide Chemical compound 0.000 title claims abstract description 26
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000002105 nanoparticle Substances 0.000 claims abstract description 57
- 239000011572 manganese Substances 0.000 claims abstract description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 26
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 18
- 229910052709 silver Inorganic materials 0.000 claims abstract description 14
- 239000004332 silver Substances 0.000 claims abstract description 14
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- GPRLSGONYQIRFK-MNYXATJNSA-N triton Chemical compound [3H+] GPRLSGONYQIRFK-MNYXATJNSA-N 0.000 claims abstract description 12
- HYZQBNDRDQEWAN-LNTINUHCSA-N (z)-4-hydroxypent-3-en-2-one;manganese(3+) Chemical compound [Mn+3].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O HYZQBNDRDQEWAN-LNTINUHCSA-N 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
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- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 42
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 14
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 12
- VASIZKWUTCETSD-UHFFFAOYSA-N manganese(II) oxide Inorganic materials [Mn]=O VASIZKWUTCETSD-UHFFFAOYSA-N 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 229910052946 acanthite Inorganic materials 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 7
- 229940056910 silver sulfide Drugs 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 claims description 6
- 238000002390 rotary evaporation Methods 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical compound [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 claims description 5
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- 239000006185 dispersion Substances 0.000 claims description 4
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- 239000000243 solution Substances 0.000 abstract description 48
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- LQKOJSSIKZIEJC-UHFFFAOYSA-N manganese(2+) oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Mn+2].[Mn+2].[Mn+2].[Mn+2] LQKOJSSIKZIEJC-UHFFFAOYSA-N 0.000 abstract description 6
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- IZTQOLKUZKXIRV-YRVFCXMDSA-N sincalide Chemical compound C([C@@H](C(=O)N[C@@H](CCSC)C(=O)NCC(=O)N[C@@H](CC=1C2=CC=CC=C2NC=1)C(=O)N[C@@H](CCSC)C(=O)N[C@@H](CC(O)=O)C(=O)N[C@@H](CC=1C=CC=CC=1)C(N)=O)NC(=O)[C@@H](N)CC(O)=O)C1=CC=C(OS(O)(=O)=O)C=C1 IZTQOLKUZKXIRV-YRVFCXMDSA-N 0.000 description 2
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- LOKCTEFSRHRXRJ-UHFFFAOYSA-I dipotassium trisodium dihydrogen phosphate hydrogen phosphate dichloride Chemical compound P(=O)(O)(O)[O-].[K+].P(=O)(O)([O-])[O-].[Na+].[Na+].[Cl-].[K+].[Cl-].[Na+] LOKCTEFSRHRXRJ-UHFFFAOYSA-I 0.000 description 1
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Abstract
The invention discloses a manganese tetraoxide-silver sulfide Janus structure (Mn 3 O 4 ‑Ag 2 S) a nanocomposite and a preparation method thereof. Belonging to the technical field of material preparation. The composite material prepared by the method has uniform shape, average grain diameter of 5-15nm, good dispersity and good biocompatibility. The preparation method comprises the following steps: dissolving manganese acetylacetonate in oleylamine, stirring and heating under the protection of inert atmosphere, transferring the manganese tetraoxide nano particles obtained by centrifugation into a mixed solution containing triton and oleylamine, simultaneously adding a silver amine solution, fully stirring, then adding a thioacetamide solution, and heating and stirring the mixed solution. After the reaction, the mixture was cooled, washed with absolute ethanol, centrifuged, and dispersed in cyclohexane. Finally use
F-127 is subjected to surface modification, so that the nanocomposite has good biocompatibility. The nanocomposite prepared by the method has nuclear magnetic resonance enhancement effect in cancer treatment application and potential as a photosensitizer.
Description
Technical Field
The invention relates to a preparation method of a nanocomposite, in particular to a preparation method of a manganese tetraoxide-silver sulfide Janus structure nanocomposite, which is simple and stable and can be widely applied to the fields of biology and medicine.
Background
With the increasing population aging problems and increasing social pressure and environmental burden, serious challenges remain fundamentally for the diagnosis and treatment of cancer. Cancer consists of hundreds of different molecular diseases, which require that most patients have custom-made regulatory strategies during cancer treatment. Whereas personalized approaches are directed to specific cancer cells, they need to rely on the binding of appropriate molecular species, so-called molecular targeted therapies. Compared with a single domain particle structure, the Janus nano particle generally shows two opposite but non-mutually-influencing unique characteristics because of the asymmetric structure and functionalization, a multifunctional application platform from material science to biology and catalysis is provided for the Janus particle, and meanwhile, the Janus nano particle has excellent application prospect in the fields of engineering, stabilizers, self-pulling motors, sensors, drug delivery and the like due to the construction of various nano material combinations.
In recent years, various disciplines organically combine to provide various research ideas for diagnosis and treatment of cancers, so as to promote effective control of target people in different stages of cancer diseases, and realizing accurate diagnosis of early stages of cancer becomes a primary part in the disease treatment process.
Among them, molecular imaging of cancer requires highly sensitive conditions, because the concentration of abnormally expressed biomolecules in tumor tissue is typically very low (in the picomolar to nanomolar range). Nanoparticles are ideal agents to meet this requirement because nanomaterials integrate dual tumor treatment and imaging functions into a single system, organically unifying the advantages between disciplines, enabling the whole process from accurate data detection to complete lesion area imaging to personalized targeted therapy. Among them, janus nanoparticles not only integrate multiple properties of conventional composite nanoparticles due to relatively small surface free energy, but also retain intrinsic properties due to space structure limitations, and also receive a great deal of attention in the biomedical field due to the uniqueness of the composite particle interface. However, the preparation method is limited by precise equipment, complicated operation and severe reaction conditions, and cannot realize large-scale production, which sets a hindrance to the popularization of the preparation method in clinical application.
The present subject uses Ag 2 S-Mn 3 O 4 The Janus structure nano-particle is used as a target material, and a simple, economical and green synthesis means is provided for preparing a hetero-body structure with uniform size and morphology. And the two means of nuclear magnetic resonance imaging and photothermal treatment are combined to realize drug release in the cancer lesion area, so that the effects of diagnosis and treatment of the cancer with good synergy are finally achieved. The system analyzes the morphology, surface charge and other material properties of the material, and judges the biocompatibility, the photo-thermal conversion efficiency and the drug release capacity. In combination with in vitro cell experiments and in vivo animal experiments, ag was explored 2 S-Mn 3 O 4 The enhanced effect of the heterostructure as a contrast agent, the safety and effectiveness for cancer material treatment, find ways to further improve diagnostic and therapeutic effects, and ultimately explore nanoparticle-mediated cancer treatment-related mechanisms.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a manganese tetraoxide-silver sulfide Janus structure nanocomposite with nuclear magnetic resonance enhancement effect and enhanced photothermal and photodynamic curative effects and a preparation method thereof.
In order to solve the technical problems, the invention firstly provides a preparation method of a manganese tetraoxide-silver sulfide Janus structure nanocomposite, which comprises the following steps:
1) Adding manganese acetylacetonate into oleylamine, and performing ultrasonic treatment until powder is uniformly dispersed in a solution; heating reaction is carried out in inert atmosphere, after the reaction is finished, cooling is carried out to room temperature, and precipitation is obtained after centrifugal washing; dissolving the precipitate in dichloromethane again, ultrasonically processing to obtain clear solution, adding ethanol, centrifuging, and washing to obtain Mn 3 O 4 The nanoparticles precipitate and are redispersed in cyclohexane;
2) Mixing oleylamine and triton solution under heating at 50-70deg.C, stirring thoroughly, and dripping into the solution obtained in step 1) dispersed with trimanganese tetroxide (Mn) 3 O 4 ) NanoparticleCyclohexane solution, fully mixing and then dropwise adding silver ammonia solution; stirring and reacting for 30 to 90 minutes, adding thioacetamide solution, and reacting for a sufficient time at 50 to 70 ℃, wherein the whole process of the step 2) is carried out under the heating condition of 50 to 70 ℃;
3) Adding ethanol after the reaction is finished, and centrifugally washing to obtain Mn 3 O 4 -Ag 2 S nano particles, namely the nano material with the manganous oxide-silver sulfide Janus structure.
As a preferable scheme of the invention, in the step 1), the mass ratio of the oleylamine to the manganese acetylacetonate is 15:1-25:1.
As a preferable mode of the invention, the reaction temperature of the step 1) is 180-250 ℃ and the reaction time is 9-11 hours.
As a preferable scheme of the invention, in the step 2), the molar ratio of oleylamine to triton is 3.6:1-4.8:1, the molar ratio of triton to silver ions in silver ammonia solution is 130:1, and the molar ratio of manganous oxide in the manganous oxide nano-particles to silver ions in silver amine solution is 0.8-1.2:1, the molar ratio of silver ions in the silver ammonia solution to thioacetamide in the thioacetamide solution is 1:1.
As a preferred embodiment of the present invention, in the step 2), the reaction time is 16 to 30 hours after the thioacetamide solution is added.
The invention also provides Mn prepared by the method 3 O 4 -Ag 2 S Janus nanoparticles.
The invention also provides a device
F-127 coated Mn 3 O 4 -Ag 2 The preparation method of the S Janus nano particle comprises the following steps:
1) Mn obtained by the above method 3 O 4 -Ag 2 S Janus nano particles are dispersed in cyclohexane to obtain Mn 3 O 4 -Ag 2 S Janus nanoparticle dispersion;
2) Will be
F-127 is dissolved in chloroform, wherein, </u >>
F-127 and chloroform in a volume ratio of 1:10, and dropwise adding Mn obtained in the step 1) under stirring 3 O 4 -Ag 2 S Janus nanoparticle dispersion, stirring at room temperature; adding distilled water for rotary evaporation, evaporating chloroform and cyclohexane to obtain nanometer composite material with trimanganese tetroxide-silver sulfide Janus structure, namely +.>
F-127 coated Mn 3 O 4 -Ag 2 S Janus nanoparticles.
The invention also provides the manganese tetraoxide-silver sulfide Janus structure nano composite material prepared by the method, which is characterized in that the composite material has uniform appearance and an average grain diameter of 5-15 nm.
The invention also provides application of the manganese tetraoxide-silver sulfide Janus structure nanocomposite in preparation of a nuclear magnetic resonance imaging contrast agent, a photosensitizer or an antibacterial agent.
Compared with the prior art, the invention has the beneficial effects that:
(1) Mn prepared by the invention 3 O 4 -Ag 2 S Janus structure nano composite material with lower r 2 /r 1 Relaxation ratios have potential applications in magnetic resonance imaging contrast agents;
(2)Mn 3+ the compound also shows effective light synergistic effect in vitro, and has a certain photodynamic killing effect on tumor cells;
(3) Mn prepared by the invention 3 O 4 -Ag 2 S Janus structure nano composite material contains Ag 2 The S quantum dot has strong absorption capacity in a near infrared two-region, can effectively convert light into heat energy and is used for ablating tumor cells;
(4) The manganese tetraoxide-silver sulfide (Mn) 3 O 4 -Ag 2 S) the nanocomposite is regular in shape, has an average particle size of 5-15nm, and has good dispersibility;
(5) The invention has low requirement on experimental instruments, and the method is simple and easy to operate.
Drawings
FIG. 1 is a transmission electron microscope image of the product obtained in example 1 of the present invention.
FIG. 2 is a transmission electron microscope image of the product obtained in example 1 of the present invention.
FIG. 3 is a graph showing the dynamic light scattering size distribution of the product obtained in example 1 of the present invention.
FIG. 4 shows the Zeta potential of the product obtained in example 1 of the present invention.
FIG. 5 is an X-ray spectroscopy (EDS) image of the product obtained in example 1 of the present invention.
FIG. 6 is an X-ray diffraction pattern of the product obtained in example 1 of the present invention.
FIG. 7 is a graph showing the results of CCK-8 experiments on 4T1 cells using the product obtained in example 1 of the present invention.
FIG. 8 shows the product obtained in example 1 of the present invention at T 1 Magnetic resonance images under weighting.
FIG. 9 is a graph showing Mn concentration as a function of longitudinal relaxation rate of the product obtained in example 1 of the present invention.
FIG. 10 is a photo-thermal transfer image of the product obtained in example 1 of the present invention.
Detailed Description
The following examples are presented to those of ordinary skill in the art to make and evaluate the invention and are merely exemplary of the disclosure and are not intended to limit the scope. Although efforts have been made to ensure accuracy with respect to numbers (e.g., amounts, temperature, etc.), some errors and deviations should be accounted for. Unless otherwise indicated, temperatures are in units of degrees celsius or at ambient temperature.
Example 1
0.3g of manganese acetylacetonate (C) 10 H 14 MnO 4 ) And 7.6g of oleylamine; reacting the mixed liquid for 10 hours at 200 ℃ under inert atmosphere; after waiting for cooling to room temperature, 10ml of dimethylformamide was addedUltrasonic treatment of alkane to obtain clear solution; adding 40ml of ethanol, centrifuging at 9000rpm for 10 minutes, and re-dispersing the precipitate in 10ml of cyclohexane to finally obtain the manganese tetraoxide nano particles;
10ml of 90% concentration oleylamine and 4ml of biochemical reagent grade triton solution are stirred and mixed for 30 minutes at 50 ℃, 400 mu L of the prepared trimanganese tetroxide nano-particles dispersed in cyclohexane and 400 mu L of 0.02g/ml silver amine solution are sequentially added, and stirring is continued for 30 minutes; subsequently, 400. Mu.L of a saturated aqueous thioacetamide solution was added dropwise; the solution reacts for 24 hours under the condition, and after the solution is naturally cooled, the solution is washed by ethanol and centrifuged for 3 times; the nanoparticles were dispersed in 10ml of cyclohexane. By using
Surface modification of nanocomposite by F-127: taking 1 ml->
F-127 in 10ml of chloroform (CHCl) 3 ) Stirring for 30 minutes; 1ml of Mn dispersed in cyclohexane was taken 3 O 4 -Ag 2 S and 1ml of chloroform (CHCl) 3 ) Mixing, and gradually dripping into the solution after mixing; stirring at room temperature for 12 hours; adding 10ml distilled water for rotary evaporation, and evaporating chloroform; get the pass->
F-127 modified nanoparticles (++>
F-127 coated Mn 3 O 4 -Ag 2 S Janus nanoparticles). Fig. 1 is a transmission electron microscope picture of the product obtained in example 1 of the present invention, and fig. 2 is a transmission electron microscope picture of the product obtained in example 1 of the present invention, and it can be intuitively seen that the prepared nanoparticle has an obvious Janus structure. Fig. 3 is a graph showing the dynamic light scattering size distribution of the product obtained in example 1 of the present invention, which can illustrate that the prepared final nanoparticles have a uniform size distribution. FIG. 4For the Zeta potential of the product obtained in example 1 according to the present invention, it can be stated that the product is subjected to +.>
F-127 modified Mn 3 O 4 -Ag 2 The potential of the S nano-particles tends to be negative from positive values, which is beneficial to the circulation of the S nano-particles in organisms. FIG. 5 is an X-ray energy spectrum analysis (EDS) picture of the product obtained in example 1 of the present invention, which shows that the prepared nanoparticles contain four elements of Mn, ag and S. FIG. 6 is an X-ray diffraction pattern of the product obtained in example 1 of the present invention, which can illustrate that the prepared nanoparticles have significant Mn 3 O 4 And Ag 2 Diffraction peak of S. Fig. 8 and 9 are graphs of T1 weighted magnetic resonance images and concentrations as a function of longitudinal relaxation rate, respectively, of the product obtained in example 1 of the present invention measured at room temperature, illustrating that the prepared nanoparticles have a magnetic resonance imaging capability that is positively correlated to the concentrations. FIG. 10 shows the concentration of the product obtained in example 1 of the present invention at 1.2w/cm 2 The photo-thermal conversion diagram under 1064nm laser irradiation can show that the prepared nano particles have good absorption capacity in a near infrared region and can effectively convert light energy into heat energy.
Example two
0.3g of manganese acetylacetonate (C) 10 H 14 MnO 4 ) And 7.6g of oleylamine; reacting the mixed liquid for 10 hours at 200 ℃ under inert atmosphere; after cooling to room temperature, adding 10ml of dichloromethane, and performing ultrasonic treatment to obtain a clear solution; adding 40ml of ethanol, centrifuging at 9000rpm for 10 minutes, and re-dispersing the precipitate in 10ml of cyclohexane to finally obtain the manganese tetraoxide nano particles;
mixing 10ml of oleylamine and 4ml of triton solution at 50 ℃ for 30 minutes under stirring, sequentially adding 800 mu L of the prepared trimanganese tetroxide nanoparticles dispersed in cyclohexane and 400 mu L of silver amine solution, and continuously stirring for 30 minutes; subsequently, 400. Mu.L of a saturated aqueous thioacetamide solution was added dropwise; the solution reacts for 24 hours under the condition, and after the solution is naturally cooled, the solution is washed by ethanol and centrifuged for 3 times; the nanoparticles were dispersed in 10ml of cyclohexane. By using
Surface modification of nanocomposite by F-127: 1ml is taken
Example III
0.3g of manganese acetylacetonate (C) 10 H 14 MnO 4 ) And 7.6g of oleylamine; reacting the mixed liquid for 10 hours at 200 ℃ under inert atmosphere; after cooling to room temperature, adding 10ml of dichloromethane, and performing ultrasonic treatment to obtain a clear solution; adding 40ml of ethanol, centrifuging at 9000rpm for 10 minutes, and re-dispersing the precipitate in 10ml of cyclohexane to finally obtain the manganese tetraoxide nano particles;
10mL of oleylamine and 4mL of triton solution are stirred and mixed for 30 minutes at 70 ℃, 400 mu L of the prepared trimanganese tetroxide nano-particles dispersed in cyclohexane and 400 mu L of silver amine solution are sequentially added, and stirring is continued for 30 minutes; subsequently, 400. Mu.L of a saturated aqueous thioacetamide solution was added dropwise; the solution was reacted under this condition for 30 hours; washing with ethanol and centrifuging for 3 times; the nanoparticles were dispersed in 10ml of cyclohexane. By using
Surface modification of nanocomposite by F-127: 1ml is taken
F-127 in 10ml of chloroform (CHCl) 3 ) Stirring for 30 minutes; 1ml of Mn dispersed in cyclohexane was taken 3 O 4 -Ag 2 S and 1ml of chloroform (CHCl) 3 ) Mixing, and gradually dripping into the solution after mixing; stirring at room temperature for 12 hours; adding 10ml distilled water for rotary evaporation, and evaporating chloroform; get the pass->
F-127 modified nano particles with average particle diameter of 5-15nm have good dispersibility.
Comparative example one
0.3g of manganese acetylacetonate (C) 10 H 14 MnO 4 ) And 7.6g of oleylamine; reacting the mixed liquid for 10 hours at 200 ℃ under inert atmosphere; after cooling to room temperature, adding 10ml of dichloromethane, and performing ultrasonic treatment to obtain a clear solution; adding 40mL of ethanol, centrifuging at 9000rpm for 10 minutes, and re-dispersing the precipitate in 10mL of cyclohexane to finally obtain the manganese tetraoxide nano particles;
10mL of oleylamine and 4mL of triton solution are stirred and mixed for 30 minutes at normal temperature, 400 mu L of trimanganese tetroxide dispersed in cyclohexane and 400 mu L of silver amine solution are sequentially added, and stirring is continued for 30 minutes; subsequently, 400. Mu.L of a saturated aqueous thioacetamide solution was added dropwise; the solution reacts for 24 hours under the condition, and after the solution is naturally cooled, the solution is washed by ethanol and centrifuged for 3 times; the nanoparticles were dispersed in 10ml of cyclohexane. By using
Surface modification of nanocomposite by F-127: 1ml is taken
F-127 in 10ml of chloroform (CHCl) 3 ) Stirring for 30 minutes; 1ml of Mn dispersed in cyclohexane was taken 3 O 4 -Ag 2 S and 1ml of chloroform (CHCl) 3 ) Mixing, and gradually dripping into the solution after mixing; stirring at room temperature for 12 hours; 10ml of steam was addedRotary evaporation is carried out on distilled water, and chloroform is evaporated; get the pass->
F-127 modified nanoparticles. No trimanganese tetraoxide-silver sulfide Janus nanocomposite could be obtained by this comparative example.
Comparative example two
0.3g of manganese acetylacetonate (C) 10 H 14 MnO 4 ) And 7.6g of oleylamine; reacting the mixed liquid for 10 hours at 200 ℃ under inert atmosphere; after cooling to room temperature, adding 10ml of dichloromethane, and performing ultrasonic treatment to obtain a clear solution; adding 40mL of ethanol, centrifuging at 9000rpm for 10 minutes, and re-dispersing the precipitate in 10mL of cyclohexane to finally obtain the manganese tetraoxide nano particles;
10mL of oleylamine and 4mL of triton solution are stirred and mixed for 30 minutes at 50 ℃, 400 mu L of manganous oxide dispersed in cyclohexane and 400 mu L of silver amine solution are sequentially added, and then 400 mu L of saturated thioacetamide aqueous solution is directly added dropwise; the solution reacts for 24 hours under the condition, and after the solution is naturally cooled, the solution is washed by ethanol and centrifuged for 3 times; the nanoparticles were dispersed in 10ml of cyclohexane. By using
Surface modification of nanocomposite by F-127: taking 1 ml->
F-127 in 10ml of chloroform (CHCl) 3 ) In the process, the liquid crystal display device comprises a liquid crystal display device, stirring for 30 minutes; 1ml of Mn dispersed in cyclohexane was taken 3 O 4 -Ag 2 S and 1ml of chloroform (CHCl) 3 ) Mixing, and gradually dripping into the solution after mixing; stirring at room temperature for 12 hours; adding 10ml distilled water for rotary evaporation, and evaporating chloroform; get the pass->
F-127 modified nanoparticles. No trimanganese tetraoxide-silver sulfide Janus nanocomposite could be obtained by this comparative example.
Application example
4T1 (10) 5 Individual cells/well) were inoculated into 96-well plates with the appropriate medium and kept overnight at 37 ℃ and 5% carbon dioxide. After that, the culture medium is removed, re-use of phosphate buffered saline
(PBS) washing. The product of example 1 was subjected to a test
F-127 modified nanoparticles (0, 12, 25, 50, 75 and 100. Mu.g/mL) were dissolved in their culture medium. Each cell line was cultured with 100. Mu.L of SBT-MET in medium for 24 hours. Proliferation of cancer and normal cells was assessed by introducing 10 μl of cell count kit-8 (CCK 8) into each well of a 96-well plate and incubating at 37 ℃ for 2 hours. After completion, absorbance was recorded at 450 nm using a microplate reader. FIG. 7 shows the result of incubation of 4T1 cells with the product of example 1 of the present invention, which demonstrates that the prepared nanoparticles have good biocompatibility.
Final conclusion: the manganese tetraoxide-silver sulfide Janus structure nanocomposite has good biocompatibility under the concentration, and the nanocomposite prepared by the method has nuclear magnetic resonance enhancement effect and potential as a photosensitizer in cancer treatment application.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit of the invention.
Claims (9)
1. The preparation method of the manganese tetraoxide-silver sulfide Janus structure nanocomposite is characterized by comprising the following steps of:
1) Adding manganese acetylacetonate into oleylamine, and performing ultrasonic treatment until powder is uniformly dispersed in a solution; heating reaction in inert atmosphere, cooling to room temperature after the reaction is finished,obtaining a precipitate after centrifugal washing; dissolving the precipitate in dichloromethane again, ultrasonically processing to obtain clear solution, adding ethanol, centrifuging, and washing to obtain Mn 3 O 4 The nanoparticles precipitate and are redispersed in cyclohexane;
2) Mixing oleylamine and triton solution under heating at 50-70deg.C, stirring thoroughly, and dripping into the solution obtained in step 1) dispersed with trimanganese tetroxide (Mn) 3 O 4 ) The cyclohexane solution of the nano particles is fully mixed and then the silver ammonia solution is dripped; stirring and reacting for 30 to 90 minutes, adding thioacetamide solution, and reacting for a sufficient time at 50 to 70 ℃, wherein the whole process of the step 2) is carried out under the heating condition of 50 to 70 ℃;
3) Adding ethanol after the reaction is finished, and centrifugally washing to obtain Mn 3 O 4 -Ag 2 S nano particles, namely the nano material with the manganous oxide-silver sulfide Janus structure.
2. The preparation method according to claim 1, wherein in the step 1), the mass ratio of oleylamine to manganese acetylacetonate is 15:1-25:1.
3. The method according to claim 1, wherein the reaction temperature in step 1) is 180 to 250 ℃ and the reaction time is 9 to 11 hours.
4. The method according to claim 1, wherein in the step 2), the molar ratio of oleylamine to triton is 3.6:1-4.8:1, the molar ratio of triton to silver ions in silver ammonia solution is 130:1, and the molar ratio of manganous oxide in the manganous oxide nanoparticles to silver ions in silver amine solution is 0.8-1.2:1, the molar ratio of silver ions in the silver ammonia solution to thioacetamide in the thioacetamide solution is 1:1.
5. The process according to claim 1, wherein in step 2), the reaction time is 16 to 30 hours after the addition of the thioacetamide solution.
6. Mn obtainable by the process according to any one of claims 1 to 5 3 O 4 -Ag 2 S Janus nanoparticles.
7. PF127 wrapped Mn 3 O 4 -Ag 2 The S Janus nano particle is characterized in that the preparation method comprises the following steps:
1) Mn obtainable by the process according to any one of claims 1 to 5 3 O 4 -Ag 2 S Janus nano particles are dispersed in cyclohexane to obtain Mn 3 O 4 -Ag 2 S Janus nanoparticle dispersion;
2) Will be
F-127 is completely dissolved in chloroform, wherein, -/->
F-127 and chloroform in a mass ratio of 1:80-120, and dropwise adding Mn obtained in the step 1) under stirring 3 O 4 -Ag 2 S Janus nanoparticle dispersion wherein Mn 3 O 4 -Ag 2 S Janus nanoparticle and +.>
The mass ratio of F-127 is 1:10 3 Stirring at room temperature; adding distilled water for rotary evaporation, evaporating chloroform and cyclohexane to obtain nanometer composite material with trimanganese tetroxide-silver sulfide Janus structure, namely +.>
F-127 coated Mn 3 O 4 -Ag 2 SJanus nanoparticles.
8. The manganese tetraoxide-silver sulfide Janus structure nano composite material prepared by the method according to claim 7 is characterized in that the composite material is uniform in appearance and has an average particle size of 5-15 nm.
9. The use of the trimanganese tetroxide-silver sulfide Janus structural nanocomposite of claim 7 for the preparation of magnetic resonance imaging contrast agents, photosensitizers or antimicrobial agents.
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