AU2021102201A4 - Polydopamine-platinum granular nanomaterial doped with moo2 and preparation method thereof - Google Patents
Polydopamine-platinum granular nanomaterial doped with moo2 and preparation method thereof Download PDFInfo
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 31
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- QXYJCZRRLLQGCR-UHFFFAOYSA-N dioxomolybdenum Chemical compound O=[Mo]=O QXYJCZRRLLQGCR-UHFFFAOYSA-N 0.000 claims abstract description 86
- 239000002105 nanoparticle Substances 0.000 claims abstract description 57
- 239000000243 solution Substances 0.000 claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 27
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 21
- 230000000694 effects Effects 0.000 claims abstract description 21
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 21
- 239000001301 oxygen Substances 0.000 claims abstract description 21
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 claims abstract description 20
- 229920001690 polydopamine Polymers 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001514 detection method Methods 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 10
- 238000001069 Raman spectroscopy Methods 0.000 claims abstract description 9
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 claims abstract description 8
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 8
- 229960001149 dopamine hydrochloride Drugs 0.000 claims abstract description 8
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 7
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 238000011065 in-situ storage Methods 0.000 claims abstract description 6
- 239000001965 potato dextrose agar Substances 0.000 claims abstract description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 10
- 238000003786 synthesis reaction Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000003860 storage Methods 0.000 claims description 9
- 229920002678 cellulose Polymers 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000002474 experimental method Methods 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 6
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims description 6
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 125000003396 thiol group Chemical group [H]S* 0.000 claims description 6
- 239000010931 gold Substances 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 3
- 238000000502 dialysis Methods 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000003384 imaging method Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000005580 one pot reaction Methods 0.000 claims description 3
- 230000011664 signaling Effects 0.000 claims description 3
- 238000004729 solvothermal method Methods 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 238000003828 vacuum filtration Methods 0.000 claims description 3
- 229910001868 water Inorganic materials 0.000 claims description 3
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 abstract description 16
- 229960003638 dopamine Drugs 0.000 abstract description 8
- 206010028980 Neoplasm Diseases 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 210000004881 tumor cell Anatomy 0.000 abstract description 3
- 230000012202 endocytosis Effects 0.000 abstract description 2
- 230000002708 enhancing effect Effects 0.000 abstract description 2
- 238000001149 thermolysis Methods 0.000 abstract description 2
- 238000010586 diagram Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 210000004027 cell Anatomy 0.000 description 5
- 238000007626 photothermal therapy Methods 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000010970 precious metal Substances 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 201000011510 cancer Diseases 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- 239000011943 nanocatalyst Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 230000001225 therapeutic effect Effects 0.000 description 2
- 206010021143 Hypoxia Diseases 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical class [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000007954 hypoxia Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000002091 nanocage Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000008685 targeting Effects 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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- 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
- A61K49/005—Fluorescence in vivo characterised by the carrier molecule carrying the fluorescent agent
- A61K49/0054—Macromolecular compounds, i.e. oligomers, polymers, dendrimers
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- 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
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- 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
- A61K41/0057—Photodynamic therapy with a photosensitizer, i.e. agent able to produce reactive oxygen species upon exposure to light or radiation, e.g. UV or visible light; photocleavage of nucleic acids with an agent
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- 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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- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
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Abstract
The present disclosure provides a polydopamine-platinum granular nanomaterial doped
with MoO2 and a preparation method thereof, belonging to the technical field of nanomaterials,
which includes MPDPs nanoparticles. The MPDPs nanoparticles include MoO2 nanoparticles,
Tris-HCl, dopamine hydrochloride powder, deionized water, PDA@MoO2 solution and
chloroplatinic acid aqueous solution, the MoO2 nanoparticles include H2 02 , MoS2 powder and
ethanol. With respect to the polydopamine-platinum granular nanomaterial doped with MoO2
and the preparation method thereof, platinum particles on the surface of polydopamine particles
are reduced in situ to synthesize the final MO 2@PDA@Pt (MPDPs) nanoparticles, the
synthesized MPDPs nanoparticles are designed to have the functions of surface enhanced
Raman effect, photo-thermal effect and oxygen-producing effect simultaneously, and the size of
the synthesized MPDPs nanoparticles is about 40 nm, so that they can enter tumor cells through
endocytosis to realize the detection and treatment of cancers; the platinum particles can take the
effects of enhancing SERS, photo-thermolysis and oxygen production, thus expanding the
application of the present technology.
DRAWINGS
.0 vohrna 0 o-)jalj
ISO' ~ 1111=8.5
Fig.1I
Fig. 2
A-B
go
-40
40 5
S20 1
0.1 0.25 0.75 I 2 4 . 7.0 73 L 8 .5B' 9.0
SConcentration of dopamine (mg) PH
2 mg/inL 4 mg/niL 6mg'19mL
concentration of1-LPtC.
Fig. 3
Description
.0 vohrna 0 o-)jalj
ISO' ~ 1111=8.5
Fig.1I
Fig. 2 A-B
go -40
40 5 S20 1
0.1 0.25 0.75 I 2 4 . 7.0 73 L 8 .5B' 9.0 SConcentration of dopamine (mg) PH
2 mg/inL 4 mg/niL 6mg'19mL concentration of1-LPtC.
Fig. 3
POLYDOPAMINE-PLATINUM GRANULAR NANOMATERIAL DOPED WITHMoO2AND PREPARATION METHOD THEREOF
The present disclosure relates to the technical field of nanomaterials, and specifically relates
to a polydopamine-platinum granular nanomaterial doped with MoO2 and a preparation method
thereof.
J By means of the technology of localized surface plasmon resonance (LSPR), nanomaterials
can effectively concentrate and amplify the incident light near their surface under resonance
excitation, and the near-field enhancement performance of nanomaterials also confers the plasma
nanomaterials a capacity of absorbing light. Because of superior optical properties, nano-sized
plasma materials have great potential applications in photocatalysis, photothermal therapy (PTT)
and surface-enhanced Raman scattering (SERS). Nanostructured precious metal materials
including Au nanocages, Ag nanocrystals and Pd nanosheets, as routine plasma nanomaterials,
have attracted extensive scientific attention. The above materials have carried out effective
amplification treatment on LSPR, but there are still some serious defects in plasmon precious
metal nanomaterials, such as high cost, poor biocompatibility and poor stability, thus limiting
o their practical applications inevitably.
Zhan Y. et al. have prepared molybdenum dioxide nanoparticles with superior properties by
a hydrothermal synthesis method. Because of strong localized surface plasmon resonance (LSPR)
properties and near-infrared (NIR) absorption properties, these particles have the best SERS
sensitivity compared with other semiconductor nanostructures when they are used as the
substrate for surface-enhanced Raman scattering (SERS) to detect trace molecules including
R6G, CV and IR780; at the same time, due to high photothermal conversion efficiency, they can
also be used in photothermal therapies to ablate cancer cells efficiently (Nanoscale 2018, 10,
pp5998-6004). Lan S.Y. et, al. have constructed a BPQDs hybrid nanocatalyst targeting
hepatocarcinoma cells, which is synthesized by entrapping black phosphorus quantum dots
(BPQD) in a mesoporous silica skeleton and then synthesizing Pt nanoparticles (PtNPs) in situ, finally synthesizing the BPQDs hybrid nanocatalyst; the resulting nanosystem shows excellent photothermal and oxygen-producing properties, and the produced oxygen can improve the efficiency of photodynamics therapy (PDT) in hypoxia environment, which has good therapeutic effects on hepatocarcinoma cells (ACS. Appl. Mater. Interfaces 2019, 11, pp 9804-9813).
The present disclosure is intended to design a polydopamine-platinum granular
nanomaterial doped with MoO2 , which has the functions of surface enhanced Raman effect,
photo-thermal effect and oxygen supplying effect within cells simultaneously, thereby realizing
the detection and therapeutic effects of tumor cells.
J SUMMARY I. Technical problems to be solved
To overcome the above defects of the prior art, the present disclosure provides a
polydopamine-platinum granular nanomaterial doped with MoO2 and a preparation method
thereof, thereby overcoming some serious defects still in plasmon precious metal nanomaterials,
such as high cost, poor biocompatibility and poor stability, which may limit their practical
applications inevitably.
1. Technical solutions
To achieve the above purposes, the present disclosure provides the following technical
solutions: a polydopamine-platinum granular nanomaterial doped with MoO2 including MPDPs
o nanoparticles, the MPDPs nanoparticles include MoO2 nanoparticles, Tris-HCl, dopamine
hydrochloride powder, deionized water, PDA@MoO 2 solution and chloroplatinic acid aqueous
solution, the MoO2 nanoparticles include H 2 0 2 , MoS2 powder and ethanol.
A preparation method of the polydopamine-platinum granular nanomaterial doped with
MoO2, including the following steps:
Si. Synthesis of MoO2 nanoparticles:
Preparation of molybdenum oxide nanomaterials by one-pot solvothermal method: 1.6 mL
H20 2 is added into 30 mL ethanol containing 30 mg MoS2 powder and stirred for 15 min, the
resulting mixture is then transferred into a Teflon-lined autoclave and heated for 5 h, to get
blue-green products; the products are cooled to room temperature and then collected, dialyzed in
1000D of dialysis bags in deionized water for 48 h, then filtered in vacuum through cellulose ester membrane, the collected suspension is then freeze-dried to prepare molybdenum dioxide, and the resulting powder is stored at low temperature finally.
S2. Synthesis of MPDPs nanoparticles:
Firstly, 10 mg MoO 2 powder is dissolved in 10 mM Tris-HCl (pH=8.5), 0.75 mg dopamine
hydrochloride powder is added into 10 mL MoO2 solution of 1 mg/mL and stirred at room temperature, dispersed by centrifugation and then re-dissolved in deionized water; 5 mL of the
PDA@MoO 2 solution is added into 0.7 mL chloroplatinic acid aqueous solution (4 mg/mL) and
reacted with stirring in an oil bath for 24 h so as to reduce Pt particles on the surface of
polydopamine in situ; at the end of the reaction, they are centrifuged and washed, then dispersed
J in deionized water for storage.
S3. Photothermal experiments:
To verify the photothermal enhancement effect of MPDPs nanoparticles, experiments are
conducted using an 808 nm infrared laser and a handheld thermosensitive imaging detector:
firstly, under the same conditions, deionized water, MoO2 solution, PDA@MoO2 solution and
MPDPs nanoparticles are irradiated with a laser (1.2 W/cm 2 ) for 10 min respectively, and photographed in turn to record the temperature changes per minute; then the laser irradiation is
stopped, and photographs are taken every 1 min to record the cooling temperature of MPDPs
nanoparticles; the above operations are repeated for five times to plot a cooling curve and calculate the photothermal conversion efficiency.
o S4. SERS detection: To verify the SERS enhancement effect of MPDPs nanoparticles, DNAs with one end
marked with mercapto groups and the other end marked with Cy5 Raman signaling molecules
are assembled on the surface of MPDPs nanoparticles through the action of mercapto
group-quinonyl; 1 L of the MPDPs nanoparticles assembled with DNAs marked with Cy5 are
dropped on a gold glass plate, dried and subjected to SERS detection by a 633 nm laser of a laser Raman spectrometer.
S5. Oxygen-producing detection:
To verify the oxygen-producing effect of MPDPs nanoparticles, the content of oxygen
produced is determined for different components with a dissolved oxygen analyzer.
As a further solution of the present disclosure: the heating temperature of the autoclave in
Si is 180°C, and the pore diameter of the cellulose ester membrane used for vacuum filtration in
S Iis 0.22 Im.
As a further solution of the present disclosure: the storage temperature for powder in Si is -20 0 C.
As a further solution of the present disclosure: the time for stirring the MoO 2 solution and the dopamine hydrochloride powder in S2 is 4 h, and the temperature of the oil bath in S2 is
90 0 C. As a further solution of the present disclosure: the final storage temperature for finished
products in S2 is 40 C.
S III. Beneficial effects
Compared with the prior art, the beneficial effects of the present disclosure are in that:
1. With respect to the polydopamine-platinum granular nanomaterial doped with MoO 2 and
the preparation method thereof, by taking advantage of self-polymerization property of
dopamine under alkaline conditions, MoO2 nanoparticles are added during the polymerization of
dopamine so that the dopamine can self-polymerize to polydopamine nanomaterials doped with
MoO2, then the platinum particles on the surface of polydopamine particles are reduced in situ to synthesize the final MoO2@PDA@Pt (MPDPs) nanoparticles; the synthesized MPDPs
nanoparticles have the functions of surface enhanced Raman effect, photo-thermal effect and oxygen-producing effect simultaneously, and the size of the synthesized MPDPs nanoparticles is
o about 40 nm, so that they can enter tumor cells through endocytosis to realize the detection and
treatment of cancers; the platinum particles can take the effects of enhancing SERS,
photo-thermolysis and oxygen production, thus expanding the application of the present
technology.
BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a schematic diagram showing the synthesis of MPDPs according to an example of
the present disclosure;
Fig. 2 shows TEM characterization diagrams and color changing diagrams in the synthesis
course of MPDPs nanoparticles according to an example of the present disclosure;
Fig. 3 is a diagram showing the experimental condition optimization in the synthesis course of MPDPs nanoparticles according to an example of the present disclosure;
Fig. 4 shows XPS characterization diagrams of MPDPs nanoparticles according to an
example of the present disclosure;
Fig. 5 shows detection diagrams on photothermal, SERS and oxygen production of MPDPs
nanoparticles according to an example of the present disclosure.
DETAILED DESCRIPTION The technical solutions of the present disclosure will be further described in detail in
combination with specific examples as below.
J As shown in Figs. 1-5, the present disclosure provides a technical solution: a
polydopamine-platinum granular nanomaterial doped with MoO 2 including MPDPs
nanoparticles, the MPDPs nanoparticles include MoO 2 nanoparticles, Tris-HCl, dopamine
hydrochloride powder, deionized water, PDA@MoO2 solution and chloroplatinic acid aqueous
solution, the MoO2 nanoparticles include H202, MoS2 powder and ethanol. Compared with other
semiconductor phases, MoO2 has excellent performances, including higher chemical stability,
melting point and conductivity, and its metallic properties are far stronger than the
semiconductor properties. The properties of materials are closely dependent on their growth
forms and microstructures. Because of electron vacancies induced by a large amount of oxygen
with enough concentration, plasma MoO2nanomaterials can display stronger LSPR effects. In
o combination with the factors of high binding stability and low cost, nano-structured plasma
MoO2materials can be used as promising alternatives of precious metal materials for SERS and
as PTT application materials.
A preparation method of the polydopamine-platinum granular nanomaterial doped with
MoO2, including the following steps:
Si. Synthesis of MoO2 nanoparticles:
Preparation of molybdenum oxide nanomaterials by one-pot solvothermal method: 1.6 mL
H20 2 is added into 30 mL ethanol containing 30 mg MoS2 powder and stirred for 15 min, the
resulting mixture is then transferred into a Teflon-lined autoclave and heated for 5 h, to get
blue-green products. As a typical metal oxide, molybdenum oxide has attracted much attention
because of its chemical and physical properties. Different kinds of molybdenum oxides appear in different stages of synthesis, for example, from molybdenum dioxide (MoO 2 ) with greatly reduced content of molybdenum, to molybdenum oxide (MoO3x, 2<x<3) with more reduced content of molybdenum, and further to totally stoichiometric molybdenum trioxide (MoO 3 ).
With the oxidation of Mo4+ ions to Mo" and Mo* ions, the color changes from dark-blue to
light-blue, green, and yellow. The products are cooled to room temperature and then collected,
dialyzed in 1000D of dialysis bags in deionized water for 48 h, then filtered in vacuum through
cellulose ester membrane with a pore diameter of 0.22 m, thereby filtering out larger purities
from the products; the collected suspension is then freeze-dried to prepare molybdenum dioxide,
and the resulting powder is stored at low temperature finally.
J S2. Synthesis of MPDPs nanoparticles:
Firstly, 10 mg MoO 2 powder is dissolved in 10 mM Tris-HCl at different pH (pH=6.5, 7.0,
7.5, 8.0, 8.5, 9.0); different amounts of dopamine hydrochloride powder (0.1 mg, 0.25 mg, 0.5
mg, 0.75 mg, 1 mg and 2 mg) is added into 10 mL MoO2 solution of 1 mg/mL and stirred at
room temperature, dispersed by centrifugation and then re-dissolved in deionized water; 5 mL of
the PDA@MoO2 solution is added into 0.7 mL chloroplatinic acid aqueous solutions of different
concentrations (2 mg/mL, 4 mg/mL and 6 mg/mL) and reacted with stirring in an oil bath for 24
h so as to reduce Pt particles on the surface of polydopamine in situ; at the end of the reaction,
they are centrifuged and washed, then dispersed in deionized water for storage. Through
experimental verification, Tris-HCl at pH=8.5, 0.75 mg of dopamine hydrochloride powder and
o4 mg/mL of chloroplatinic acid aqueous solution are finally selected. S3. Photothermal experiments:
To verify the photothermal enhancement effect of MPDPs nanoparticles, experiments are
conducted using an 808 nm infrared laser and a handheld thermosensitive imaging detector:
firstly, under the same conditions, deionized water, MoO2 solution, PDA@MoO 2 solution and
MPDPs nanoparticles are irradiated with a laser (1.2 W/cm 2 ) for 10 min respectively, and
photographed in turn to record the temperature changes per minute; then the laser irradiation is
stopped, and photographs are taken every 1 min to record the cooling temperature of MPDPs
nanoparticles; the above operations are repeated for five times to plot a cooling curve and
calculate the photothermal conversion efficiency.
The calculating formula of photothermal conversion efficiency in S3 is shown as below: he s(T_ -T, u-Qdis h I mi e C ,i
) s(h u
Aso =Co e L e CNc,
S4. SERS detection:
To verify the SERS enhancement effect of MPDPs nanoparticles, DNAs with one end
marked with mercapto groups and the other end marked with Cy5 Raman signaling molecules
are assembled on the surface of MPDPs nanoparticles through the action of mercapto
J group-quinonyl; 1 L of the MPDPs nanoparticles assembled with DNAs marked with Cy5 are
dropped on a gold glass plate, dried and subjected to SERS detection by a 633 nm laser of a laser
Raman spectrometer. The reason for detection by SERS is in that they have the best SERS
sensitivity compared with other semiconductor nanostructures. In addition, due to the high
photothermal conversion efficiency, they can also be used in photothermal therapies to ablate
cancer cells efficiently.
S5. Oxygen-producing detection:
To verify the oxygen-producing effect of MPDPs nanoparticles, the content of oxygen
produced is determined for different components with a dissolved oxygen analyzer.
In particular, the heating temperature of the autoclave in Si is 180°C, the pore diameter of
the cellulose ester membrane used for vacuum filtration in S Iis 0.22 [m.
In particular, the storage temperature for powder in Si is -20°C.
In particular, the time for stirring the MoO2 solution and the dopamine hydrochloride
powder in S2 is 4 h, and the temperature of the oil bath in S2 is 90°C.
In particular, the final storage temperature for finished products in S2 is 4°C.
In the description of the present disclosure, it should be noted that unless otherwise
specified and limited, the terms "installation", "linking", "connection" should be understood
broadly. For example, the connection can be fixed, detachable, or integral; the connection may
be mechanical connection or electric connection; the connection may be direct connection, or indirect connection through an intermediate, or the internal communication between two elements. For ordinary technicians in the field, the specific meanings of the above terms in the present disclosure can be understood according to specific circumstances.
The preferred implementation of the present disclosure has been illustrated in detail above,
but the present disclosure is not limited to the above implementation. Various changes can be
made within the knowledge range of ordinary technicians in the field without deviating from the
principle of the present disclosure.
Claims (5)
1. A polydopamine-platinum granular nanomaterial doped with MoO2, comprising MPDPs
nanoparticles, wherein: the MPDPs nanoparticles comprise MoO2 nanoparticles, Tris-HCl,
dopamine hydrochloride powder, deionized water, PDA@MoO 2 solution and chloroplatinic acid
aqueous solution, the MoO2 nanoparticles comprise H 2 0 2 , MoS2 powder and ethanol.
2. A preparation method of the polydopamine-platinum granular nanomaterial doped with
MoO2, wherein, comprising the following steps:
Si. Synthesis of MoO2 nanoparticles:
Preparation of molybdenum oxide nanomaterials by one-pot solvothermal method: 1.6 mL
H20 2 is added into 30 mL ethanol containing 30 mg MoS2 powder and stirred for 15min, the
resulting mixture is then transferred into a Teflon-lined autoclave and heated for 5 h, to get
blue-green products; the products are cooled to room temperature and then collected, dialyzed in
1000D of dialysis bags in deionized water for 48 h, then filtered in vacuum through cellulose
ester membrane, the collected suspension is then freeze-dried to prepare molybdenum dioxide,
and the resulting powder is stored at low temperature finally;
S2. Synthesis of MPDPs nanoparticles:
Firstly, 10 mg MoO2 powder is dissolved in 10 mM Tris-HCl (pH=8.5), 0.75 mg dopamine
hydrochloride powder is added into 10 mL MoO2 solution of 1 mg/mL and stirred at room
temperature, dispersed by centrifugation and then re-dissolved in deionized water; 5 mL of the
PDA@MoO 2 solution is added into 0.7 mL chloroplatinic acid aqueous solution (4 mg/mL) and
reacted with stirring in an oil bath for 24 h so as to reduce Pt particles on the surface of
polydopamine in situ; at the end of the reaction, they are centrifuged and washed, then dispersed
in deionized water for storage;
S3. Photothermal experiments:
To verify the photothermal enhancement effect of MPDPs nanoparticles, experiments are
conducted using an 808 nm infrared laser and a handheld thermosensitive imaging detector:
firstly, under the same conditions, deionized water, MoO2 solution, PDA@MoO 2 solution and
MPDPs nanoparticles are irradiated with a laser (1.2 W/cm 2 ) for 10 min respectively, and photographed in turn to record the temperature changes per minute; then the laser irradiation is stopped, and photographs are taken every 1 min to record the cooling temperature of MPDPs nanoparticles; the above operations are repeated for five times to plot a cooling curve and calculate the photothermal conversion efficiency;
S4. SERS detection:
To verify the SERS enhancement effect of MPDPs nanoparticles, DNAs with one end
marked with mercapto groups and the other end marked with Cy5 Raman signaling molecules
are assembled on the surface of MPDPs nanoparticles through the action of mercapto
group-quinonyl; 1 L of the MPDPs nanoparticles assembled with DNAs marked with Cy5 are
dropped on a gold glass plate, dried and subjected to SERS detection by a 633 nm laser of a laser
Raman spectrometer.
S5. Oxygen-producing detection:
To verify the oxygen-producing effect of MPDPs nanoparticles, the content of oxygen
produced is determined with a dissolved oxygen analyzer under different conditions.
3. The preparation method of the polydopamine-platinum granular nanomaterial doped with
MoO2 according to claim 2, wherein: the heating temperature of the autoclave in Si is 180°C,
and the pore diameter of the cellulose ester membrane used for vacuum filtration in S Iis 0.22
[m.
4. The preparation method of the polydopamine-platinum granular nanomaterial doped with
MoO2 according to claim 2, wherein: the storage temperature for powder in S Iis -20°C.
5. The preparation method of the polydopamine-platinum granular nanomaterial doped with
MoO2 according to claim 2, wherein: the time for stirring the MoO2 solution and the dopamine
hydrochloride powder in S2 is 4 h, and the temperature of the oil bath in S2 is 90°C;
wherein: the final storage temperature for finished products in S2 is 4°C.
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DRAWINGS 27 Apr 2021
Fig. 1 2021102201
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Fig. 5 Fig. 4 Page 2/2
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| CN113368238B (en) * | 2021-06-07 | 2022-08-02 | 青岛科技大学 | h-BN/MoS capable of realizing targeted photothermal and chemical synergistic treatment 2 Nano probe and preparation method and application thereof |
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| CN108408780A (en) * | 2018-03-12 | 2018-08-17 | 南京邮电大学 | A kind of Transition-metal dichalcogenide nanometer sheet and preparation method thereof of poly-dopamine modification |
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