CN115286040A - Preparation method and application of cerium-doped tungsten oxide nanosphere light diagnosis and treatment agent - Google Patents
Preparation method and application of cerium-doped tungsten oxide nanosphere light diagnosis and treatment agent Download PDFInfo
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Abstract
The invention relates to the technical field of functional nano materials, and discloses a preparation method and application of a cerium-doped tungsten oxide nanosphere light diagnosis and treatment agent. The specific method comprises the steps of taking tungsten chloride as a tungsten source, cerium nitrate hexahydrate as a cerium source, n-propanol as a reaction solvent, regulating the doping amount of Ce, and heating for reacting for a period of time to prepare the W 18 O 49 -xCe nanospheres. The material has good crystallinity, the size of a single nanosphere is 90-110 nm, and the Ce ion-doped materialThe material shows excellent photodynamic performance under near infrared light, and simultaneously, under a simulated tumor microenvironment, the material is in contact with H in a tumor enrichment area 2 O 2 Oxidation-reduction reaction takes place to produce O 2 The photodynamic performance is obviously improved, the problem of oxygen deficiency of tumor parts is effectively solved, and the curative effect is improved. In addition, the compound has CT imaging function, and is a very potential photo-diagnosis and treatment agent in near infrared photodynamic therapy of cancer.
Description
Technical Field
The invention relates to the technical field of functional nano materials, and discloses a preparation method and application of a cerium-doped tungsten oxide nanosphere light diagnosis and treatment agent.
Background
Cancer is one of the most fatal diseases in the world, and a great deal of manpower, material resources and financial resources have been invested in the treatment thereof in the past. However, the conventional methods for treating cancer such as surgery, chemotherapy and radiotherapy have great limitations and have many well-known disadvantages, and thus development of new therapeutic means has great significance for cancer treatment.
Photodynamic therapy is one of the most widely applied phototherapy modes at present, and a photosensitizer generates intracellular active oxygen under the action of light excitation to selectively kill malignant cells. Malignant proliferation of cancer cells and abnormal growth of tumor blood vessels leads to O in tumor tissues 2 Inadequate supply, hypoxic Tumor Microenvironment (TME) impairs the efficacy of oxygen-dependent photodynamic therapy. Process consumption of large amounts of O during photodynamic therapy 2 Destroy tumor blood vessels and further block O 2 Supply, resulting in severe hypoxia of TME. Tumor neovascularization and hypoxia inducible factor (HIF-1 a) can induce recurrence and invasion of cancer cells. Therefore, the development of advanced materials and methods for photodynamic therapy of hypoxic tumors is of great scientific interest.
W 18 O 49 The tungsten oxide is a single-phase tungsten oxide with mixed valence, has good stability, has a large number of oxygen vacancies in the structure, can generate a local surface plasmon resonance effect, and has strong light absorption and photo-thermal conversion capability in a near infrared region. Meanwhile, the atomic number of tungsten is large, and the CT imaging diagnosis function can be realized. In recent years, there have been many students paired with W 18 O 49 The application in cancer therapy is studied.
The tumor-rich region has H relative to the normal tissue region 2 O 2 Ce ion has been shown to pass H under mildly acidic conditions 2 O 2 Exhibits peroxidase-like activity by converting H into 8729OH in physiological environment 2 O 2 Decomposition to O 2 And exhibits a catalase-like activity.
Based on the consideration, the invention adopts a one-step heating method to prepare W 18 O 49 The xCe nanosphere is used for characterizing and testing the sample performance through XRD, SEM, UV-Vis-NIR, photodynamic performance test and CT imaging test, so that the photo-diagnosis and treatment agent capable of solving the problem of oxygen deficiency of a tumor part in near infrared photodynamic therapy and realizing CT imaging is obtained.
Disclosure of Invention
In order to solve the defects of the prior art, the invention discloses a preparation method of a cerium-doped tungsten oxide nanosphere light diagnosis and treatment agent 18 O 49 -xCe nanospheres, which material has a very good crystallinity, the size of the individual nanospheres being between 90-110 mm. The material can effectively solve the problem of oxygen deficiency in photodynamic therapy, has the function of CT imaging, and is a very potential light diagnosis and treatment agent in near infrared photodynamic therapy of cancer.
The invention is realized by the following technical method:
a preparation method of a cerium-doped tungsten oxide nanosphere light diagnosis and treatment agent comprises the following steps:
according to the formula W 18 O 49 Molar doping ratio of-xCe weighted WCl providing tungsten source and cerium source 6 、Ce(NO 3 ) 3 ·6H 2 O, weighing the WCl 6 Dissolving the solid in n-propanol solvent, stirring until the solution is clear and NO solid exists, and then weighing and adding the weighed Ce (NO) 3 ) 3 ·6H 2 And O, continuously stirring until the solid is dissolved to obtain a clear mixed solution. Transferring the solution into a reaction kettle, and putting the reaction kettle into an oven for heating reaction. Taking out the reaction kettle after the reaction kettle is cooled to room temperature, carrying out centrifugal treatment on the solution after the reaction, washing the solid obtained by centrifugal separation, and drying to obtain the productTo W 18 O 49 -xCe nanospheres.
Preferably, the molar doping ratio x of Ce is 3-7%.
Preferably, the solution is stirred for 15-30 min, and the heating temperature is 200 DEG o And C, the reaction time is 24 h.
Preferably, the centrifugation condition is that the centrifugation rotating speed is 8000-10000 rpm, and the centrifugation time is 15-30 min.
Preferably, the washing condition is that the absolute ethyl alcohol and the deionized water are respectively washed for 3 times.
Preferably, the drying condition is that the drying temperature is 65 DEG o C。
Preferably, said W is formed 18 O 49 -xCe nanospheres are spherical in shape with dimensions between 90-110 mm.
The cerium-doped tungsten oxide nanosphere light diagnosis and treatment agent is applied to near-infrared light power treatment of cancers.
Compared with the prior art, the invention has the following advantages:
(1) The invention adopts a one-step heating method, the preparation method is simple, and the prepared W 18 O 49 The xCe nanosphere has high crystallinity, uniform appearance and size of 90-110 nm.
(2) The cerium ion doped tungsten oxide nanospheres provided by the invention have excellent photodynamic performance under near-infrared light, and simultaneously have excellent photodynamic performance with H in a tumor enrichment area under a simulated tumor microenvironment 2 O 2 Oxidation-reduction reaction to produce O 2 The photodynamic therapy agent has the advantages of obviously improving the photodynamic performance, effectively solving the problem of oxygen deficiency of tumor parts, improving the curative effect, having CT imaging capability and being a very potential photodynamic therapy agent in the near infrared photodynamic therapy of cancer.
Drawings
FIG. 1 shows W in example 1 18 O 49 XRD pattern of xCe sample.
FIGS. 2a, 2b and 2c show W in example 1 18 O 49 -3%Ce、W 18 O 49 -5%Ce、W 18 O 49 7% SEM picture of Ce samples.
FIG. 3 shows W in example 1 18 O 49 -3% energy profile of the ce sample.
FIG. 4 shows W in example 1 18 O 49 Ultraviolet-visible-near infrared absorption spectrum diagram of the xCe sample.
FIG. 5 shows W in example 1 18 O 49 And an absorption spectrum chart of DPBF of an xCe sample under the laser irradiation of a wavelength of 808 nm.
FIG. 6 shows W in example 1 18 O 49 And the absorption spectrum of DPBF of an xCe sample under the irradiation of laser with the wavelength of 1064 nm.
FIG. 7 shows W concentrations in example 1 18 O 49 -3% absorption spectrum of DPBF sample under 808 nm wavelength laser irradiation.
FIG. 8 shows W concentrations in example 1 18 O 49 -5% absorption spectrum of DPBF sample irradiated with laser light having a wavelength of 1064 nm.
FIG. 9 shows W in example 1 18 O 49 -3% absorption spectrum of DPBF from the Ce sample at different illumination times with laser light of 808 nm wavelength.
FIG. 10 shows W in example 1 18 O 49 -5% absorption spectrum of DPBF from Ce samples at different illumination times with laser light of 1064 nm wavelength.
FIG. 11 shows W in example 1 18 O 49 -3% absorption spectrum of DPBF from a sample of Ce irradiated with a laser with a wavelength of 808 nm in a simulated tumor microenvironment.
FIG. 12 shows W in example 1 18 O 49 -5% absorption spectrum of DPBF sample under irradiation with laser light of 1064 nm wavelength in a simulated tumor microenvironment.
FIG. 13 shows W concentrations in example 1 18 O 49 CT imaging of xCe samples.
Detailed Description
The invention is described in further detail below with reference to specific embodiment examples and the attached drawing of the specification, but the embodiments of the invention are not limited thereto.
Example 1: a preparation method of a cerium-doped tungsten oxide nanosphere light diagnosis and treatment agent comprises the following steps:
weighing 0.3 g of tungsten chloride solid, dissolving the tungsten chloride solid in 60 mL of n-propanol solvent, stirring until the solution is clear and no solid exists, then respectively adding 3%,5% and 7% of cerium nitrate hexahydrate according to the molar doping ratio into the solution, and continuously stirring until the solid is dissolved. The solution was transferred to a 100 mL reaction kettle, placed in an oven, at 200 deg.F o And reacting for 24 hours under the condition of C. Taking out after the reaction kettle is cooled to room temperature, centrifuging the reaction product for 15 min at the speed of 10000 rpm, washing the reaction product for 3 times by using absolute ethyl alcohol and deionized water respectively, and placing the centrifuged solid in 65 o C drying in a drying oven to obtain W 18 O 49 -xCe nanospheres (x =3%,5%, 7%).
FIG. 1 shows three kinds of W prepared in example 1 18 O 49 XRD pattern of xCe sample, as shown, XRD pattern of sample with pure phase W 18 O 49 The XRD patterns of the two parts are similar and correspond to a PDF card (JCPDS 71-2450). At 2 theta =23.5 o Has a distinct diffraction peak corresponding to W 18 O 49 And the sharp degree of the diffraction peak is reduced along with the increase of the doping concentration of Ce ions, and the diffraction peak has small angle shift because the Ce ions replace W 18 O 49 The position of the middle W atom causes lattice expansion.
FIGS. 2a, 2b, 2c are three W s prepared in example 1 18 O 49 SEM image of xCe sample, W doped with three Ce ion concentrations as shown 18 O 49 The size and the appearance of the nanospheres are similar, the appearance is uniform, and the size is 90-110 nm.
FIG. 3 is W prepared in example 1 18 O 49 -3% of the Ce sample, as shown in the figure, which contains a large amount of W element and a small amount of Ce element therein, demonstrating successful Ce ion doping.
Example 2: absorption spectrum analysis
FIG. 4 is W prepared in example 1 18 O 49 The ultraviolet-visible-near infrared absorption spectrum diagram of-xCe shows that the Ce ion doping only changes the light absorption intensity and does not change the position of an absorption peak, namely, the light absorption region does not move to the visible region. W is caused by the localized surface plasmon resonance effect 18 O 49 -xCe is inThe near infrared light region with larger tissue penetration depth has absorption, and the light absorption effect becomes better along with the increase of the wavelength. In the near infrared region, W 18 O 49 The light absorption effect was as high as-3% Ce.
Example 3: photodynamic performance study
Under dark conditions, W for example 1 18 O 49 And (4) carrying out a photodynamic performance test on an xCe sample. The centrifuge tube was vertically fixed, 3 mL of the sample solution was added thereto, 1 mg/mL of 1, 3-Diphenylisobenzofuran (DPBF) was added as an indicator solution, and the sample solution was vertically irradiated with 808 nm and 1064 nm lasers, respectively, to be completely exposed to the center of the irradiation range of the laser. During irradiation, the sample was more uniformly dispersed throughout the solution by magnetic stirring. After a certain period of light, the sample was removed and the supernatant was separated from the solid and used to test the absorbance.
FIG. 5 shows W in example 1 18 O 49 The absorption spectrum of DPBF of an xCe sample after being irradiated for 15 min under a laser of 808 nm shows that W is observed when the laser wavelength is 808 nm 18 O 49 The best photodynamic performance of the Ce samples-3%. FIG. 6 shows W in example 1 18 O 49 The absorption spectrum of DPBF of an xCe sample after being irradiated for 15 min under a 1064 nm laser beam, it can be seen that W is observed when the laser wavelength is 1064 nm 18 O 49 The best photodynamic performance of the Ce samples-5%.
By the above-mentioned investigation, preferably, W is investigated separately 18 O 49 -3% of the photodynamic properties of Ce at 808 nm laser and W 18 O 49 -5% photodynamic properties of ce under a 1064 nm laser.
The photodynamic performance of samples with different concentrations is studied, and FIG. 7 shows W with different concentrations when the illumination time is 15 min 18 O 49 -3% absorption spectrum of DPBF by laser at 808 nm of Ce, it can be seen that as W 18 O 49 -3% increase in Ce sample concentration, the absorption intensity of DPBF gradually decreases, which indicates that more singlet oxygen is generated. FIG. 8 shows W at different concentrations for 15 min of light 18 O 49 Absorption spectrum of DPBF at 1064 nm laser intensity in-5% Ce, from which W was observed 18 O 49 -5% Ce also in 1064 nm laser irradiation, which indicates W 18 O 49 -3%Ce，W 18 O 49 The photodynamic properties of the-5% Ce samples were concentration dependent.
Selecting 1 mg/mL sample, and studying the illumination performance of the sample under different illumination time, as shown in FIG. 9, wherein the laser wavelength is W under 808 nm illumination 18 O 49 -3% of the Ce sample, the absorption intensity of the DPBF solution decreased greatly at 5 min of light irradiation, more singlet oxygen was generated, the absorption intensity of the DPBF solution further decreased with the increase of the light irradiation time, and the DPBF absorption peak reached the level when the light irradiation time was 25 min, indicating that a large amount of singlet oxygen was generated in the solution at this time, and the DPBF was completely decomposed. Similarly, as shown in FIG. 10, W is measured at a laser wavelength of 1064 nm 18 O 49 -5% Ce produces a large amount of singlet oxygen under short-time illumination, and DPBF is completely decomposed when the illumination time is 25 min. From this, we can conclude that W 18 O 49 -3%Ce，W 18 O 49 -5% ce sample has good photodynamic properties.
In photodynamic therapy of tumors, O 2 Is indispensable, but in the actual treatment process, the tumor is just in an anoxic environment, so that the application of the photodynamic therapy is limited. The tumor-rich region presents H relative to the normal tissue region 2 O 2 And Ce ion can be reacted with H 2 O 2 React to produce O 2 And solves the problem of oxygen deficiency at tumor parts. The tumor microenvironment is now simulated to perform photodynamic testing on the sample. FIG. 11 shows W at 808 nm under laser irradiation for 15 min 18 O 49 -3% of Ce sample in addition to H 2 O 2 The comparison of the front and rear photodynamic performance shows that after 15 min of illumination, H is not added 2 O 2 W of (2) 18 O 49 -3% Ce sample solution, the DPBF solution light absorption intensity of which varies greatly, but the absorption peak does not tend to the level, at the time of addition of H 2 O 2 Then, the absorption peak of DPBF tended to level at the same time of light irradiation, indicating that DPBF was completely decomposed, compared with the case of no H addition 2 O 2 Previously generated more sheetsLinear oxygen, probably due to the addition of H 2 O 2 Then, ce is reacted with H 2 O 2 Reaction takes place to produce O 2 Participate in the photodynamic reaction. FIG. 12 shows W under 1064 nm laser irradiation for 15 min 18 O 49 -5% of Ce sample in addition to H 2 O 2 The same conclusion can be drawn by comparing the front and rear photodynamic properties, W 18 O 49 -5% Ce has the same properties. In summary, W 18 O 49 -3%Ce、W 18 O 49 -5% Ce has very good photodynamic properties, while Ce ions can interact with H in the tumor microenvironment 2 O 2 Reaction takes place to produce O 2 And solves the problem of oxygen deficiency in tumor photodynamic therapy.
Example 4: in vitro CT imaging study
Taking 1 mg/mL and 100 mg/mL of W 18 O 49 The xCe samples were subjected to CT imaging studies, as shown in FIG. 13, when W is 18 O 49 When the concentration of xCe is lower, the CT image is darker, and after the concentration is increased, the CT image becomes brighter. Along with the increase of the doping concentration of the Ce ions, the CT image has little change, which shows that the doping of the Ce ions has no obvious influence on the CT imaging effect, and W 18 O 49 -xCe has good CT imaging performance.
Claims (8)
1. A preparation method of a cerium-doped tungsten oxide nanosphere light diagnosis and treatment agent is characterized by comprising the following steps:
according to the formula W 18 O 49 Molar doping ratio of-xCe weighted WCl providing tungsten source and cerium source 6 、Ce(NO 3 ) 3 ·6H 2 Dissolving O in an n-propanol solvent, and stirring until the solid is dissolved to obtain a clear solution; transferring the solution into a reaction kettle, and putting the reaction kettle into a drying oven for heating reaction; taking out the reaction kettle after the reaction kettle is cooled to room temperature, centrifuging the solution after the reaction, washing the solid obtained by centrifugal separation, and drying to obtain W 18 O 49 -xCe nanospheres.
2. The method for preparing a cerium-doped tungsten oxide nanosphere as claimed in claim 1, wherein the molar doping ratio x of Ce is 3-7%.
3. The method for preparing cerium-doped tungsten oxide nanospheres as claimed in claim 1, wherein the solution is stirred for 15-30 min and heated at 200 deg.C o And C, the reaction time is 24 h.
4. The method for preparing a cerium-doped tungsten oxide nanosphere light diagnosis and treatment agent according to claim 1, wherein the centrifugation condition is that the centrifugation rotation speed is 8000-10000 rpm, and the centrifugation time is 15-30 min.
5. The method for preparing the cerium-doped tungsten oxide nanosphere light diagnosis and treatment agent according to claim 1, wherein the washing conditions are that absolute ethyl alcohol and deionized water are respectively washed for 3 times.
6. The method for preparing cerium-doped tungsten oxide nanospheres as claimed in claim 1, wherein the drying condition is a drying temperature of 65% o C。
7. The method for preparing cerium-doped tungsten oxide nanospheres as claimed in claim 1, wherein W is formed 18 O 49 -xCe nanospheres are spherical in shape with dimensions between 90-110 mm.
8. The use of the cerium-doped tungsten oxide nanospheres as claimed in claim 1 in near infrared photodynamic therapy of cancer.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116603518A (en) * | 2023-05-23 | 2023-08-18 | 昆明理工大学 | Ce-doped W18O49 photocatalytic material and preparation method and application thereof |
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| CN102921006A (en) * | 2012-11-13 | 2013-02-13 | 东华大学 | Application of tungsten oxide matrix nanometer materials in preparation of near-infrared light heat treatment drugs |
| CN113058589A (en) * | 2021-03-31 | 2021-07-02 | 桂林理工大学 | Ce-doped W18O49Nanowire photocatalyst and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102921006A (en) * | 2012-11-13 | 2013-02-13 | 东华大学 | Application of tungsten oxide matrix nanometer materials in preparation of near-infrared light heat treatment drugs |
| CN113058589A (en) * | 2021-03-31 | 2021-07-02 | 桂林理工大学 | Ce-doped W18O49Nanowire photocatalyst and preparation method thereof |
Non-Patent Citations (2)
| Title |
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| XUETING CHANG等: "Solvothermal synthesis of Ce-doped tungsten oxide nanostructures as visible-light-driven photocatalysts", 《NANOTECHNOLOGY》, vol. 22, pages 265603, XP020206852, DOI: 10.1088/0957-4484/22/26/265603 * |
| 龚林吉等: "多功能纳米材料在肿瘤放疗增敏中的应用", 《物理化学学报》, vol. 34, no. 2, pages 140 - 167 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116603518A (en) * | 2023-05-23 | 2023-08-18 | 昆明理工大学 | Ce-doped W18O49 photocatalytic material and preparation method and application thereof |
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