CN114804207B - Synthetic method for tumor radiotherapy material - Google Patents
Synthetic method for tumor radiotherapy material Download PDFInfo
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- CN114804207B CN114804207B CN202210460541.7A CN202210460541A CN114804207B CN 114804207 B CN114804207 B CN 114804207B CN 202210460541 A CN202210460541 A CN 202210460541A CN 114804207 B CN114804207 B CN 114804207B
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- tungstate
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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
- A61K41/0038—Radiosensitizing, i.e. administration of pharmaceutical agents that enhance the effect of radiotherapy
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P35/00—Antineoplastic agents
Abstract
The invention discloses a synthesis method of a tumor radiotherapy material, which comprises the following steps: s1, crushing wolframite powder to 300-320 meshes, adding wolframite powder into caustic soda to obtain sodium tungstate, and adding calcium chloride into the sodium tungstate to synthesize calcium tungstate; s2, placing calcium tungstate and ultrapure water into a reaction kettle, stirring and dissolving at a rotating speed of 600-800r/min for 60-100min to obtain an aqueous solution A; s3, adding gadolinium salt water solution into the reaction kettle, and stirring and reacting at the rotating speed of 600-800r/min for 60-100min to obtain gadolinium tungstate solution. According to the synthetic method for the tumor radiotherapy material, the gadolinium tungstate absorbs X rays, and the gadolinium and tungsten atoms have higher atomic numbers and have strong absorption capacity on the X rays, so that the gadolinium polytungstate nanocluster has good radiotherapy sensitization effect; meanwhile, the gadolinium and tungsten have stable properties, the gadolinium tungstate nanocluster has very small size and can be rapidly discharged out of the body through the kidney, so that the toxic and side effects caused by long-term accumulation of the gadolinium tungstate nanocluster in the body are greatly reduced, and the effect of the gadolinium tungstate nanocluster is superior to that of other traditional radiosensitizers.
Description
Technical Field
The invention relates to the technical field of tumor radiotherapy, in particular to a synthesis method of a tumor radiotherapy material.
Background
Radiation therapy is one of three main therapeutic strategies for clinically treating localized solid tumors, with more than 50% of patients receiving radiation therapy during cancer fight; however, the high intensity of radiation during treatment not only kills tumor cells, but also causes unavoidable damage to normal tissues around them; therefore, how to develop a radiation sensitizer with excellent performance to maximize the radiation dose to cancer cells and reduce the damage to normal cells is a difficult problem to be solved;
through searching, the invention patent with the Chinese patent number of 201910508639.3 discloses an atomic accurate gold nanocluster material radiotherapy sensitizer, belongs to the crossing field of nano material chemistry and biochemistry, and synthesizes gold nanoclusters with high yield and excellent fluorescence performance and accurate atomic size by taking levonorgestrel with good biocompatibility as a protective ligand through a room-temperature volatilization one-pot method. The chemical formula of the nano gold cluster is as follows: C168H216 Au8O16 (abbreviated as Au8 NC) belongs to a triclinic system, and the space group is chiral space group P1. The gold nanocluster has stronger yellow-green fluorescence at room temperature, and the fluorescence quantum yield is 58.7%; it has a small size (2 nm) and good dispersibility, and can be used for bright cell imaging. The nano gold cluster material can be used as a radiotherapy sensitizer to play a role in radiotherapy sensitization.
The radiotherapy sensitizer provided by the scheme has poor X-ray absorption effect and large toxic and side effects, so that a synthetic method for a tumor radiotherapy material is provided to solve the problem.
Disclosure of Invention
The invention aims to provide a synthesis method for tumor radiotherapy materials, which aims to overcome the problems that the radiation sensitizer has poor absorption effect on X rays and large toxic and side effects.
The invention adopts the following technical scheme for realizing the technical purpose: a synthetic method for tumor radiotherapy materials comprises the following steps:
s1, crushing wolframite powder to 300-320 meshes, adding wolframite powder into caustic soda to obtain sodium tungstate, and adding calcium chloride into the sodium tungstate to synthesize calcium tungstate;
s2, placing calcium tungstate and ultrapure water into a reaction kettle, stirring and dissolving at a rotating speed of 600-800r/min for 60-100min to obtain an aqueous solution A;
s3, adding gadolinium salt water solution into the reaction kettle, and stirring and reacting at the rotating speed of 600-800r/min for 60-100min to obtain gadolinium tungstate solution;
s4, cooling the gadolinium tungstate solution to room temperature, crystallizing, recrystallizing and filtering to obtain gadolinium tungstate crystals;
s5, adding glycerol, divalent manganese and silicon oxide into gadolinium tungstate crystal, heating to 200-300 ℃, and stirring at a rotating speed of 100-200r/min for reacting for 100-150min to obtain a reactant B;
s6, placing the reactant B in an ultrasonic dispersing instrument, treating for 100-120min under the condition that the ultrasonic frequency is 55-60kHz, dispersing the liquid, and then irradiating the dispersing liquid with ultraviolet light for 3-4d to obtain the inorganic nanocluster containing gadolinium tungstate.
Preferably, the concentration of the caustic soda is 30-35%.
As an optimization, the ratio of the calcium tungstate to the ultrapure water is 3:10.
as optimization, before gadolinium salt water solution is added, glacial acetic acid is firstly dripped into a reaction kettle to adjust the pH value to 7.5-7.9.
Preferably, the gadolinium tungstate, the glycerol, the divalent manganese and the silicon oxide are screened by a screen mesh with 200-250 meshes before being mixed.
As optimization, the gadolinium tungstate, the glycerol, the divalent manganese and the silicon oxide are in parts by weight:
50-90 parts of gadolinium tungstate, 30-40 parts of glycerol, 10-15 parts of divalent manganese and 7-13 parts of silicon oxide.
Preferably, the wavelength of the ultraviolet rays is 200-280nm.
The invention has the following beneficial effects:
1. according to the synthetic method for the tumor radiotherapy material, the gadolinium tungstate absorbs X rays, and the gadolinium and tungsten atoms have higher atomic numbers and have strong absorption capacity on the X rays, so that the gadolinium polytungstate nanocluster has good radiotherapy sensitization effect; meanwhile, the gadolinium and tungsten have stable properties, the gadolinium tungstate nanocluster has very small size and can be rapidly discharged out of the body through the kidney, so that the toxic and side effects caused by long-term accumulation of the gadolinium tungstate nanocluster in the body are greatly reduced, and the effect of the gadolinium tungstate nanocluster is superior to that of other traditional radiosensitizers.
2. According to the synthetic method of the material for tumor radiotherapy, the absorption capacity of the material to X rays is further improved by adding other mixtures into gadolinium tungstate, so that the damage of radiotherapy to human bodies is further reduced.
Detailed Description
In the following, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A synthetic method for tumor radiotherapy materials comprises the following steps:
s1, crushing wolframite powder to 300 meshes, removing impurities from the wolframite powder, adding the wolframite powder into 1.5 times of caustic soda to obtain sodium tungstate, and adding calcium chloride into the sodium tungstate to synthesize calcium tungstate;
s2, placing calcium tungstate and ultrapure water into a reaction kettle, stirring and dissolving for 60min at a rotating speed of 600r/min to obtain an aqueous solution A;
s3, adding gadolinium salt water solution into the reaction kettle, and stirring and reacting for 60min at the rotating speed of 600r/min to obtain gadolinium tungstate solution;
s4, cooling the gadolinium tungstate solution to room temperature, crystallizing, recrystallizing, filtering to obtain gadolinium tungstate crystals, flushing the gadolinium tungstate crystals by using ultrapure water, and then drying;
s5, adding glycerol, divalent manganese and silicon oxide into gadolinium tungstate crystals, heating to 200 ℃, and stirring at a rotating speed of 100r/min for reacting for 100min to obtain a reactant B;
s6, placing the reactant B in an ultrasonic dispersing instrument, treating for 100 minutes under the condition that the ultrasonic frequency is 55kHz, dispersing the liquid, and then irradiating the dispersing liquid for 3 days by using ultraviolet light to obtain the inorganic nanocluster containing gadolinium tungstate.
The concentration of caustic soda was 30%.
The ratio of calcium tungstate to ultrapure water is 3:10.
before gadolinium salt water solution is added, glacial acetic acid is firstly added into the reaction kettle in a dropwise manner to adjust the pH to 7.5.
Before mixing gadolinium tungstate, glycerol, divalent manganese and silicon oxide, sieving with a 200-mesh sieve is needed to accelerate mixing.
The gadolinium tungstate, the glycerol, the divalent manganese and the silicon oxide are prepared from the following components in parts by weight:
50 parts of gadolinium tungstate, 30 parts of glycerol, 10 parts of divalent manganese and 7 parts of silicon oxide.
The wavelength of the ultraviolet light was 200nm.
Example 2
A synthetic method for tumor radiotherapy materials comprises the following steps:
s1, crushing wolframite powder to 320 meshes, removing impurities from the wolframite powder, adding the wolframite powder into 1.5 times of caustic soda to obtain sodium tungstate, and adding calcium chloride into the sodium tungstate to synthesize calcium tungstate;
s2, placing calcium tungstate and ultrapure water into a reaction kettle, stirring and dissolving for 100min at a rotating speed of 800r/min to obtain an aqueous solution A;
s3, adding gadolinium salt water solution into the reaction kettle, and stirring and reacting for 100min at a rotating speed of 800r/min to obtain gadolinium tungstate solution;
s4, cooling the gadolinium tungstate solution to room temperature, crystallizing, recrystallizing, filtering to obtain gadolinium tungstate crystals, flushing the gadolinium tungstate crystals by using ultrapure water, and then drying;
s5, adding glycerol, divalent manganese and silicon oxide into gadolinium tungstate crystals, heating to 300 ℃, and stirring at a rotating speed of 200r/min for reaction for 150min to obtain a reactant B;
s6, placing the reactant B in an ultrasonic dispersing instrument, treating for 120min under the condition that the ultrasonic frequency is 60kHz, dispersing the liquid, and then irradiating the dispersing liquid with ultraviolet light for 4d to obtain the inorganic nanocluster containing gadolinium tungstate.
The concentration of caustic soda was 35%.
The ratio of calcium tungstate to ultrapure water is 3:10.
before gadolinium salt water solution is added, glacial acetic acid is firstly added into the reaction kettle in a dropwise manner to adjust the pH to 7.9.
Gadolinium tungstate, glycerol, divalent manganese, and silica are screened using a 250 mesh screen before mixing.
The gadolinium tungstate, the glycerol, the divalent manganese and the silicon oxide are prepared from the following components in parts by weight:
90 parts of gadolinium tungstate, 40 parts of glycerol, 15 parts of divalent manganese and 13 parts of silicon oxide.
The wavelength of the ultraviolet light was 280nm.
Gadolinium tungstate can be used for treating hypoxic tumors by emitting X-rays/photons, compton electrons, positive and negative electron pairs, auger electrons, etc. under high-energy radiation, and generating radiochemistry (free radicals or ionization). On one hand, gadolinium tungstate can perform oxidation-reduction reaction with glutathione in cells, so that the content level of the glutathione in the cells is reduced, the consumption of active oxygen substances by the glutathione is reduced, more and more effective active oxygen substances are generated, the double-strand damage of DNA is more serious, and the enhanced radiotherapy effect is achieved. On the other hand, the gadolinium polytungstate nanocluster synthesized by gadolinium tungstate has very small size and can be rapidly discharged out of the body through the kidney, so that the toxic and side effects caused by long-term accumulation of the gadolinium polytungstate nanocluster in the body are greatly reduced, and the effect of the gadolinium polytungstate nanocluster is superior to that of other traditional radiosensitizers.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A method for synthesizing a tumor radiotherapy material, comprising the steps of:
s1, crushing wolframite powder to 300-320 meshes, adding wolframite powder into caustic soda to obtain sodium tungstate, and adding calcium chloride into the sodium tungstate to synthesize calcium tungstate;
s2, placing calcium tungstate and ultrapure water into a reaction kettle, stirring and dissolving at a rotating speed of 600-800r/min for 60-100min to obtain an aqueous solution A;
s3, adding gadolinium salt water solution into the reaction kettle, and stirring and reacting at the rotating speed of 600-800r/min for 60-100min to obtain gadolinium tungstate solution;
s4, cooling the gadolinium tungstate solution to room temperature, crystallizing, recrystallizing and filtering to obtain gadolinium tungstate crystals;
s5, adding glycerol, divalent manganese and silicon oxide into gadolinium tungstate crystal, heating to 200-300 ℃, and stirring at a rotating speed of 100-200r/min for reacting for 100-150min to obtain a reactant B;
s6, placing the reactant B in an ultrasonic dispersing instrument, treating for 100-120min under the condition that the ultrasonic frequency is 55-60kHz, dispersing the liquid, and then irradiating the dispersing liquid with ultraviolet light for 3-4d to obtain the inorganic nanocluster containing gadolinium tungstate.
2. The method for synthesizing a tumor radiotherapy material according to claim 1, wherein: the concentration of the caustic soda is 30-35%.
3. The method for synthesizing a tumor radiotherapy material according to claim 1, wherein: the ratio of the calcium tungstate to the ultrapure water is 3:10.
4. the method for synthesizing a tumor radiotherapy material according to claim 1, wherein: before gadolinium salt water solution is added, glacial acetic acid is firstly added into the reaction kettle in a dropwise manner to adjust the pH to 7.5-7.9.
5. The method for synthesizing a tumor radiotherapy material according to claim 1, wherein: the gadolinium tungstate, the glycerol, the divalent manganese and the silicon oxide are screened by a screen mesh with 200-250 meshes before being mixed.
6. The method for synthesizing a tumor radiotherapy material according to claim 1, wherein: the gadolinium tungstate, the glycerol, the divalent manganese and the silicon oxide are prepared from the following components in parts by weight:
50-90 parts of gadolinium tungstate, 30-40 parts of glycerol, 10-15 parts of divalent manganese and 7-13 parts of silicon oxide.
7. The method for synthesizing a tumor radiotherapy material according to claim 1, wherein: the wavelength of the ultraviolet rays is 200-280nm.
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| JP2006016427A (en) * | 2004-06-30 | 2006-01-19 | Mitsubishi Chemicals Corp | Method for producing polyester |
| WO2009088250A2 (en) * | 2008-01-10 | 2009-07-16 | Industry-Academic Cooperation Foundation, Yonsei University | Porous hollow silica n anop articles, preparation method of the silica nanoparticles, and drug carriers and pharmaceutical composition comprising the silica nanoparticles |
| CN106975078A (en) * | 2017-03-31 | 2017-07-25 | 国家纳米科学中心 | A kind of nano material comprising many Gadolinium Tungstates as sensitizer purposes |
| CN110204563A (en) * | 2019-06-13 | 2019-09-06 | 郑州大学 | A kind of nanogold clustered materials radiotherapeutic sensitizer |
| CN110327463A (en) * | 2019-06-10 | 2019-10-15 | 西南民族大学 | A kind of nano material and its preparation method and application comprising more Gadolinium Tungstates |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP2370362B1 (en) * | 2008-10-15 | 2013-11-27 | 3M Innovative Properties Company | Fillers and composite materials with zirconia and silica nanoparticles |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006016427A (en) * | 2004-06-30 | 2006-01-19 | Mitsubishi Chemicals Corp | Method for producing polyester |
| WO2009088250A2 (en) * | 2008-01-10 | 2009-07-16 | Industry-Academic Cooperation Foundation, Yonsei University | Porous hollow silica n anop articles, preparation method of the silica nanoparticles, and drug carriers and pharmaceutical composition comprising the silica nanoparticles |
| CN106975078A (en) * | 2017-03-31 | 2017-07-25 | 国家纳米科学中心 | A kind of nano material comprising many Gadolinium Tungstates as sensitizer purposes |
| CN110327463A (en) * | 2019-06-10 | 2019-10-15 | 西南民族大学 | A kind of nano material and its preparation method and application comprising more Gadolinium Tungstates |
| CN110204563A (en) * | 2019-06-13 | 2019-09-06 | 郑州大学 | A kind of nanogold clustered materials radiotherapeutic sensitizer |
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