CN108069458A - A kind of ultra micro nano-level sphere bismuth tungstate crystal grain and preparation method and application - Google Patents
A kind of ultra micro nano-level sphere bismuth tungstate crystal grain and preparation method and application Download PDFInfo
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- CN108069458A CN108069458A CN201711436059.5A CN201711436059A CN108069458A CN 108069458 A CN108069458 A CN 108069458A CN 201711436059 A CN201711436059 A CN 201711436059A CN 108069458 A CN108069458 A CN 108069458A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K41/00—Medicinal preparations obtained by treating materials with wave energy or particle radiation ; Therapies using these preparations
- A61K41/0052—Thermotherapy; Hyperthermia; Magnetic induction; Induction heating therapy
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K41/00—Medicinal preparations obtained by treating materials with wave energy or particle radiation ; Therapies using these preparations
- A61K41/0057—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
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K49/00—Preparations for testing in vivo
- A61K49/04—X-ray contrast preparations
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a kind of ultra micro nano-level sphere bismuth tungstate crystal grain, which is spherical structure, and particle size is 4 6nm, 36.2 ± 2.4mV of surface potential.Bismuth tungstate crystal grain of the present invention can be used in CT imaging research and oncotherapy, and cell compatibility is good, to animal nonhazardous, can be widely applied for medical research, has widened the application field of bismuth tungstate due to special planform.
Description
Technical field
The present invention relates to a kind of bismuth tungstate materials, and in particular to a kind of ultra micro nano-level sphere bismuth tungstate crystal grain.
Background technology
Bismuth tungstate (Bi2WO6) it is most one of simple compounds in Aurivillius structural materials.Possess as piezoelectricity, ferroelectricity,
The physical and chemical performances such as pyroelectricity and catalysis, make it have widely in numerous areas such as ionic semiconductor, ferromagnetic material, catalysis
Using.Bismuth tungstate is applied to processing organic dye waste water, noxious material waste water, sky as a kind of preferable catalysis material
Gas purification etc..
1999, Kudo etc. was by the bismuth tungstates of solid state reaction kinetics, in Ag NO3In the case of as sacrifice agent,
Bi2WO6It can carry out photocatalytic water and generate O2So that it starts to show up prominently in catalytic field.The Bi of the reports such as Zou synthesis2WO6Can
See under light to organic matter CHCl3And CH3CHO generates degradation, and so far, people start to have carried out it extensive research.Due to partly leading
The performance of body nano material and its pattern, size etc. have significant associations, therefore the nano material for preparing different-shape obtains
The common recognition of more and more researchers.The pattern of the bismuth tungstate synthesized at present mainly has nest like, flower-shaped, sheet, tire-like etc..Though
Right document is it has been reported that many methods can prepare the different bismuth tungstate nano material of appearance structure, but the geomery prepared
Greatly, water solubility is bad, bio-compatibility is poor etc. so that bismuth tungstate rarely has the report applied in terms of medicine.
The content of the invention
The purpose of the present invention is to solve defects in the prior art, provide a kind of bismuth tungstate suitable for medicine
Material.
In order to achieve the above object, the present invention provides a kind of ultra micro nano-level sphere bismuth tungstate crystal grain, bismuth tungstate crystalline substances
Grain is spherical structure, particle size the 4-6nm, ± 2.4mV of surface potential -36.2.
The present invention also provides the preparation methods of above-mentioned bismuth tungstate crystal grain, comprise the following steps：
(1) 0.2mmol Bi (NO are taken3)3·5H2O is dissolved in 5-10mL nitric acid；
(2)0.1mmol Na2WO4·2H2O is dissolved in 45-75mL distilled water, and is added to the solution of step (1) preparation
In, form suspension；
(3) suspension prepared by step (2) is heated to 100-120 DEG C, reacted 50-80 minutes；
(4) 0.2-0.4mL NH are taken3·H2O and 0.1mL-0.3mL oleic acid is added in the product after step (3) is reacted, and is risen
Temperature reacts 50-80min to 170-200 DEG C；
(5) product of step (4) after reaction is centrifuged, collects yellow mercury oxide, and respectively cleaned with absolute ethyl alcohol and PBS
3 times；
(6) precipitation after step (5) is cleaned adds in the KMnO of 50-100mL 10mg/mL4In, when ultrasonic 6-10 is small, obtain
To the bismuth tungstate nano-particle of carboxyl modified, PBS cleaning 3 times is centrifuged to get the bismuth tungstate crystal grain.
It after the completion of preparation, is freeze-dried, is preserved at 4 DEG C.
The present invention also provides application of the above-mentioned bismuth tungstate crystal grain in terms of CT imagings.
Comprise the following steps specifically, carrying out CT imagings：
(1) configuration injection solution：The Bismuth tungstate nanocrystal is taken to be dissolved in PBS solution configuration injection solution, injects solution
The concentration of middle tungsten is 50mM；
(2) intratumor injection：The 40 μ L of injection solution that step (1) is prepared is taken to carry out intratumor injection；
(3) CT is imaged：After intratumor injection 3h, CT imagings are carried out, CT imagings are using AM General 750HD CT instrument, X-ray
Voltage be 70KV, 400 μ A of electric current.
The present invention also provides application of the above-mentioned bismuth tungstate crystal grain in terms of tumor is prepared.
It is specifically application of the above-mentioned bismuth tungstate crystal grain in terms of preparing for photo-thermal therapy material.
Or application of the above-mentioned bismuth tungstate crystal grain in terms of preparing for optical dynamic therapy medicine.
Or use in conjunction of the above-mentioned bismuth tungstate crystal grain in terms of photo-thermal therapy and optical dynamic therapy.
The present invention has the following advantages compared with prior art：The bismuth tungstate that the present invention is prepared is ultra micro nano-level sphere
Material can be dissolved in PBS solution, form colloidal solution, and keep stable state more than 7 days.The tungsten that the present invention is prepared
Sour bismuth material can be applied to CT imaging research and oncotherapy due to special planform, and cell compatibility is good, right
Animal nonhazardous, can be widely applied for medical research, widen the application field of bismuth tungstate.
Description of the drawings
Fig. 1 is chemical equation prepared by bismuth tungstate crystal grain of the present invention；
Fig. 2 is TEM (transmission electron microscope) figure of bismuth tungstate crystal grain of the present invention；
Fig. 3 is the grain size distribution of bismuth tungstate crystal grain of the present invention；
Fig. 4 is the dynamic light scattering diagram of bismuth tungstate crystal grain of the present invention；
Fig. 5 is bismuth tungstate crystal grain stability curve in PBS of the present invention；
Fig. 6 is bismuth tungstate crystal grain stability curve in serum of the present invention；
Fig. 7 is the EDS phenograms of W elements in bismuth tungstate crystal grain of the present invention；
Fig. 8 is the EDS phenograms of Bi elements in bismuth tungstate crystal grain of the present invention；
Fig. 9 is cell compatibility test result of the bismuth tungstate crystal grain of the present invention to cervical cancer cell (HeLa)；
Figure 10 is cell compatibility test result of the bismuth tungstate crystal grain of the present invention to people's venous endothelial cell (HUVEC)；
Figure 11 is the HE colored graphs of each internal organs after bismuth tungstate crystal grain intratumor injection of the present invention；
Figure 12,13 are blood biochemical analysis chart after bismuth tungstate crystal grain intratumor injection of the present invention；
In Figure 12,13, LYM- cent lymphocytes, NEU- neutrophil leucocyte percentages, EOS- eosinophils,
MON- monocyte ratios, RBC- red-cell counts, ALT- glutamic-pyruvic transaminase, TBIL- total bilirubins, CRE- creatinines, the total eggs of TP-
In vain, BUN- blood urea nitrogens, PLT- platelet counts；
Figure 14 is bismuth tungstate crystal grain CT imaging effect figures of the present invention；
In Figure 14, Untreated be direct CT imaging reference group, Bi2WO6For Bi2WO6CT imagings after intratumor injection
Experimental group, Iodixanol are the control group that clinical common Iodixanol carries out CT imagings；
Figure 15 is the design sketch that photo-thermal therapy is carried out using bismuth tungstate crystal grain of the present invention；
Figure 16 is the temperature changing curve diagram that photo-thermal therapy is carried out using bismuth tungstate crystal grain of the present invention；
Figure 17 is HeLa cells after different disposal, ROS/hypoxia detection probes treated laser confocal scanning
Micrograph；
Figure 18 is the contrast schematic diagram of tumor volume change under different disposal in photo-thermal therapy and optical dynamic therapy combination；
Figure 19 is animal tumor disappearance quantity contrast schematic diagram under different disposal in photo-thermal therapy and optical dynamic therapy combination；
Figure 20 is animal survival rate comparison signal under different disposal in photo-thermal therapy and optical dynamic therapy combination treatment tumour
Figure.
Specific embodiment
The present invention is described in detail below in conjunction with the accompanying drawings.
Product prepares embodiment 1
As shown in Figure 1, the preparation method of ultra micro nanometer spherical bismuth tungstate crystal grain of the present invention is as follows：
(1) 0.2mmol Bi (NO are taken3)3·5H2O is dissolved in 5-10mL nitric acid
(2)0.1mmol Na2WO4·2H2O is dissolved in 45-75mL distilled water, and is added to the solution of step (1) preparation
In, form suspension；
(3) suspension prepared by step (2) is heated to 100-120 DEG C, reacted 50-80 minutes；
(4) 0.2-0.4mL NH are taken3·H2O and 0.1mL-0.3mL oleic acid is added in the product after step (3) is reacted, and is risen
Temperature reacts 50-80min to 170-200 DEG C；
(5) product of step (4) after reaction is centrifuged, collects yellow mercury oxide, and respectively cleaned with absolute ethyl alcohol and PBS
3 times；
(6) precipitation after step (5) is cleaned adds in the KMnO of 50-100mL 10mg/mL4In, when ultrasonic 6-10 is small, obtain
To bismuth tungstate nano-particle (the carboxylic acid-functionalized Bi of carboxyl modified2WO6NPs), PBS cleaning 3
Time, it centrifuges to get the bismuth tungstate crystal grain.
(7) after the completion of preparing, it is freeze-dried, is preserved at 4 DEG C.
Performance detection embodiment 2
It is as follows that characterization result is carried out to the bismuth tungstate crystal grain of above-described embodiment synthesis：
As shown in Fig. 2, TEM the results show nanometers bismuth tungstate is Homogeneous Circular particle.
As shown in figure 3, the grain size of the bismuth tungstate crystal grain to being prepared counts, grain size 4-6nm, the result is dynamic
It is verified in state light scattering diagram (as shown in Figure 4).It is preserved simultaneously in PBS and serum, can still grain size be kept to stablize.Such as
Shown in Fig. 5, Fig. 6.
By carrying out EDS elemental analyses to nanometer bismuth tungstate, it is found that W, Bi largely exist, as shown in Figure 7, Figure 8.
Cell compatibility embodiment 3
The nanometer wolframic acid of various concentration is added in cervical cancer cell (HeLa) and people's venous endothelial cell (HUVEC)
Bismuth, concentration are calculated according to the W in nanometer bismuth tungstate.
Respectively for 24 hours and 48h, cell viability MTT tests are carried out, as a result as Fig. 9, Figure 10 are shown：Nanometer Bi2WO6To cell
It is nontoxic.
Animal toxicity embodiment 4
Tumor model intratumor injection nanometer Bi2WO6Afterwards, and 808 laser illumination is used 8 minutes.Its important organ is carried out
HE is dyed, and is not found tissue abnormalities, as shown in figure 11.Biochemical analysis is carried out to blood, every liver, kidney index are normal
In the range of, as shown in Figure 12,13.
Explanation：Nanometer Bi2WO6It applies, animal body will not be had adverse effect in animal body.
CT imaging effects embodiment 5
Animal model for tumour is built：The right oxter injection HeLa tumour cells of mouse, canceration, mouse tumor occur for injection site
Growth is apparent, and gross tumor volume is more than 500mm3For success animal model, it is applied in following research.
Bi2WO6Nano material intratumor injection：40μL of Bi2WO6Nano material (concentration of tungsten is 50mM), control group is
Clinically used 40 μ L of Iodixanol (concentration of iodine is 100mM).
After intratumor injection 3h, carry out CT imagings, instrument be AM General 750HD CT instrument, X-ray voltage 70KV, electric current
400μA。
It is seen from figure 14 that after nanometer Bi2WO6 intratumor injections, tumour is clearly displayed, and effect ratio faces
Common Iodixanol will also be got well on bed.
Photo-thermal therapy effect example 6
Photo-thermal therapy method is to utilize the material with high light thermal conversion efficiency, is injected into inside of human body, utilizes target
Tropism identification technology is gathered near tumor tissues, and is converted luminous energy under the irradiation of external light source (being usually near infrared light)
A kind of therapy of cancer cell is killed for thermal energy.
Mouse tumor model intratumor injection nanometer bismuth tungstate irradiates 20 points of (808nm, 1W/cm2) using laser irradiation device
Clock, it can be seen that after intratumor injection nanometer bismuth tungstate, photo-thermal effect is apparent (as shown in figure 15), and rate of rise in temperature is fast, 3
Or so minute just rises to 48 degrees Celsius (as shown in figure 16).
Optical dynamic therapy 7
Using light come treat disease before thousands of years with regard to oneself through occur, but photodynamic therapy until eighties of last century just be people
It is known.Optical dynamic therapy is to be converted luminous energy to tissue oxygen using photosensitizer and generate the cytotoxic singlet oxygen of tool, should
Therapy has many advantages, such as that toxic side effect is small, tumor-selective is good, is a kind of therapeutic strategy of great potential.Oxygen is that light power is controlled
The raw material for the treatment of, it is the singlet oxygen with cellkilling capacity that can be activated under laser irradiation by photosensitive drug, each so as to treat
The diseases such as kind tumour.
Oxygen is the critical materials that optical dynamic therapy works, and it is with cell that can be activated under laser irradiation by photosensitive drug
The singlet oxygen of killing ability, so as to treat tumour, and the oxygen content in most solid tumors is low all than normal structure
It is more, this is because tumour cell metabolic disorder in vain contain, another major reason is the oxygen consumption and vessel closure of photodynamic reaction
The effect of effect has been further exacerbated by the weary oxygen of solid tumor, these reasons result in photo-dynamical medicine is severely limited.By near
The development of 30 years, almost all of research all concentrate on the local oxygen content for how improving tumour, but related improvement light power oxygen
The research of supply is still without breakthrough.
Participation in the present invention in the optical dynamic therapy of nanometer bismuth tungstate without oxygen, directly by water H2O (OH-) is converted
For OH.To prove this point, different modes are respectively adopted and carry out HeLaxibao processing：Untreated is directly progress ROS/
Hypoxia detection probes treated reference group；ICG+Laser is pair of laser treatment with irradiation after photo-dynamical medicine ICG processing
Than group, processing procedure is：Using photo-dynamical medicine ICG (concentration 1mg/mL, 100 μ L of dosage) intratumor injection 2 it is small when after, 808 swash
Light device (1W/cm2) irradiate 10 minutes；W18O49+ Laser is W18O49Contrast groups that treated, processing procedure are：Using W18O49
After when (concentration 1mg/mL, 100 μ L of dosage) intratumor injection 2 is small, 808 laser (1W/cm2) irradiate 10 minutes；Bi2WO6+Laser
To use nanometer bismuth tungstate Bi of the present invention2WO6Experimental group that treated, processing procedure are：Using Bi2WO6(concentration 1mg/mL is used
Measure 100 μ L) intratumor injection 2 it is small when after, 808 laser (1W/cm2) irradiate 10 minutes；HeLa cells are after different disposal, ROS/
Treated that laser confocal scanning micrograph is as shown in figure 17 for hypoxia detection probes.
As can be seen from Figure 17, for photo-dynamical medicine (ICG, common drug) during tumor, weary oxygen is more tight
Weight；In W18O49Treatment under, equally also generate weary oxygen.And nanometer Bi2WO6Only there is ROS (active oxygen) to increase, not
There is the situation that weary oxygen aggravates.
Illustrate a nanometer Bi2WO6Can weary oxygen enough be overcome, optical dynamic therapy is carried out under hypoxia.
Photo-thermal therapy, optical dynamic therapy use in conjunction effect example 8
Animal model for tumour is built：The right oxter injection HeLa tumour cells of mouse, canceration, mouse tumor occur for injection site
Growth is apparent, and gross tumor volume is more than 500mm3For success animal model, it is applied in following research.
Grouping：Physiological saline group, ICG groups, W18O49Group and nanometer Bi2WO6Group, every group 8.
Processing：Drug is configured to 1mg/mL, intratumor injection 100 μ L, 8 it is small when after, 808 laser (1W/cm2) irradiation 8
Minute.
As a result：As shown in figure 18, nanometer Bi2WO6The tumour of group is reduced, other each groups are all increased (P<0.05).
And nanometer Bi2WO6The tumour that group has 5 animals (totally 8) almost disappears, as shown in figure 19.When the survival rate of animal and survival
Between be considerably longer than other groups, as shown in figure 20.
Claims (7)
1. a kind of ultra micro nano-level sphere bismuth tungstate crystal grain, it is characterised in that：The bismuth tungstate crystal grain is spherical structure, and grain size is big
Small is 4-6nm, ± 2.4 mV of surface potential -36.2.
2. the preparation method of bismuth tungstate crystal grain described in claim 1, it is characterised in that：Comprise the following steps：
（1）Take 0.2 mmol Bi (NO3)3•5H2O is dissolved in 5-10mL nitric acid
（2）0.1 mmol Na2WO4•2H2O is dissolved in 45-75mL distilled water, and is added to step（1）The solution of preparation
In, form suspension；
（3）By step（2）The suspension of preparation is heated to 100-120 DEG C, reacts 50-80 minutes；
（4）Take 0.2-0.4 mL NH3•H2O and 0.1 mL-0.3mL oleic acid add in step（3）In product after reaction, and heat up
To 170-200 DEG C, 50-80min is reacted；
（5）By step（4）Product centrifugation after reaction is collected yellow mercury oxide, and is respectively cleaned 3 times with absolute ethyl alcohol and PBS；
（6）By step（5）Precipitation after cleaning adds in the KMnO of 10 mg/mL of 50-100 mL4In, when ultrasonic 6-10 is small, obtain
To the bismuth tungstate nano-particle of carboxyl modified, PBS cleaning 3 times is centrifuged to get the bismuth tungstate crystal grain.
3. application of the bismuth tungstate crystal grain in terms of CT imagings described in claim 1.
4. application according to claim 3, it is characterised in that：CT imagings are carried out to comprise the following steps：
（1）Configuration injection solution：The Bismuth tungstate nanocrystal is taken to be dissolved in PBS solution configuration injection solution, injects tungsten in solution
Concentration be 50mM；
（2）Intratumor injection：Take step（1）The 40 μ L of injection solution being prepared carry out intratumor injection；
（3）CT is imaged：After intratumor injection 3h, CT imagings are carried out, CT imagings use AM General 750HD CT instrument, X-ray
Voltage is 70KV, 400 μ A of electric current.
5. application of the bismuth tungstate crystal grain described in claim 1 in terms of tumor is prepared.
6. application according to claim 5, it is characterised in that：The bismuth tungstate crystal grain is used to prepare photo-thermal therapy material.
7. application according to claim 5, it is characterised in that：The bismuth tungstate crystal grain is used to prepare Visudyne
Object.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112107597A (en) * | 2020-10-30 | 2020-12-22 | 北京理工大学 | Copper tungstate nanodot medicine, preparation method and application in mouse tumor model |
| CN115282164A (en) * | 2022-08-11 | 2022-11-04 | 江南大学附属医院 | Application of novel non-metal surface plasma in preparation of pancreatic cancer prevention and treatment product |
-
2017
- 2017-12-26 CN CN201711436059.5A patent/CN108069458A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| CHAO ZHANG等: "Multifunctional Bi2WO6 Nanoparticles for CT-Guided Photothermal and Oxygen-free Photodynamic Therapy", 《ACS APPLIED MATERIALS & INTERFACES》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112107597A (en) * | 2020-10-30 | 2020-12-22 | 北京理工大学 | Copper tungstate nanodot medicine, preparation method and application in mouse tumor model |
| CN115282164A (en) * | 2022-08-11 | 2022-11-04 | 江南大学附属医院 | Application of novel non-metal surface plasma in preparation of pancreatic cancer prevention and treatment product |
| CN115282164B (en) * | 2022-08-11 | 2024-01-19 | 江南大学附属医院 | Application of novel nonmetallic surface plasma in preparation of pancreatic cancer prevention and treatment products |
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Application publication date: 20180525 |