CN114751461A - Novel ferrite and synthesis method and application thereof - Google Patents
Novel ferrite and synthesis method and application thereof Download PDFInfo
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- CN114751461A CN114751461A CN202210384243.4A CN202210384243A CN114751461A CN 114751461 A CN114751461 A CN 114751461A CN 202210384243 A CN202210384243 A CN 202210384243A CN 114751461 A CN114751461 A CN 114751461A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/0018—Mixed oxides or hydroxides
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/24—Heavy metals; Compounds thereof
- A61K33/26—Iron; Compounds thereof
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y5/00—Nanobiotechnology or nanomedicine, e.g. protein engineering or drug delivery
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- 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
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a novel ferrite and a synthesis method and application thereof, belonging to the field of biological materials. The ferrite is prepared by carrying out hydrothermal reaction on ferric oxychloride with the particle size of 10-100 nm. The invention prepares the nanometer chlorine-oxygen-iron and nanometer ferrite particles with special shapes and smaller particle sizes by using the raw materials with low price and the simple and clear preparation method, and the nanometer particles can realize the effects of sensitizing tumor radiotherapy and increasing tumor chemical dynamic therapy.
Description
Technical Field
The invention relates to the field of biological materials, in particular to a novel ferrite and a synthesis method and application thereof.
Background
Cancer is the second most common cause of death worldwide, and therefore, effective and timely diagnosis and treatment means are crucial for cancers with high morbidity and mortality. In the conventional tumor treatment, a doctor generally adopts a surgical scheme to remove visible solid tumor tissue, however, the problem of metastatic lesions in the late stage of the tumor and some tiny invisible tumor tissue cannot be completely solved by the surgical scheme temporarily, and only conservative treatment can be performed by radiotherapy and chemical drug treatment.
Traditional radiotherapy or chemotherapy has more or less side effects on human body, for example, radiotherapy has the risk of canceration of normal tissue cells in human body, and excessive high-energy radiation dose also has certain influence on human immune system, so that the resistance of human body is reduced, and the capability of resisting external pathogens is weakened. Chemotherapy has obvious side effects, and can cause great damage to normal body cells of people, especially white blood cells responsible for human body immunity while killing tumor cells, and common side effects include vomiting, alopecia, immunity reduction and the like. Therefore, there are great disadvantages and inefficiencies in solving the tumor problem through a single treatment mode, and the best tumor treatment effect with the least damage to the body needs to be found, and the reasonable synergistic treatment by using a plurality of treatment means is needed.
The iron death is a programmed death mode which is discovered in recent years and is different from apoptosis, necrosis and autophagy, the main action mechanism of the iron death is that the cells are subjected to lipid peroxidation under the action of Fenton reaction participated by iron element and derivatives thereof so as to induce cell death, and the emerging cell death mechanism is expected to be applied to the aspect of tumor treatment.
The nano ferrite has good application prospect as an inorganic nano material with good biological affinity, the particle size of the nano chlorine oxygen iron synthesized by Jianan Zhang et al (New J.chem.,2017,41, 10339-10346) is 300-400nm, and the excessive particle size weakens the penetration of the tumor, so the nano ferrite cannot be well applied to the tumor treatment. The nano-grade chlorine-oxygen-iron synthesized by Meng Sun et al (environ.Sci. Techniol.Lett.2018, 5,186-191) has smooth and flat surface, is difficult to generate secondary reflection to high-energy rays, and cannot achieve the effect of sensitizing tumor radiotherapy. Zhi Min-Cui et al (RSC adv.,2016,6, 74545-74549) synthesized a layered flower-like ferrite which has a good Fenton reaction effect, but cannot be well applied to tumor treatment due to too large particle size (900-1000 nm).
Disclosure of Invention
The invention provides petal-shaped nano-ferric oxychloride and regular nano-ferrite with small particle size and shape, a synthetic method thereof and application thereof in tumor radiotherapy and chemotherapy, aiming at the technical problems in the prior art.
The purpose of the invention can be realized by the following technical scheme:
a novel ferrite is prepared by carrying out hydrothermal reaction on ferric oxychloride with the particle size of 10-100 nm to prepare the ferrite with the particle size of 20-50 nm.
In the technical scheme of the invention: the preparation method of the nano iron oxychloride comprises the following steps: dissolving ferric nitrate nonahydrate in deionized water, heating the mixed solution to 92-98 ℃ under the reflux condition, then adding a sodium chloride solution, reacting for 5-10 minutes, cooling, centrifuging, washing with water, and freeze-drying to obtain 20-50 nm ferric oxychloride particles.
The preparation method of the nano iron oxychloride comprises the following steps: the mass ratio of the ferric nitrate nonahydrate to the sodium chloride solution to the deionized water is 0.4-0.48: 4-10: 20-60, wherein: the mass concentration of the sodium chloride solution is 93-99%.
The ferrite described above: the grain size of the nano iron oxychloride particles is between 20 and 40nm, and the nano iron oxychloride particles are in petal-shaped sheet structures.
A preparation method of a novel ferrite comprises the following steps: and uniformly mixing the prepared ferric oxychloride particles with water, and then carrying out hydrothermal reaction to obtain the nano ferrite with the particle size of 20-50 nm.
The preparation method of the ferrite comprises the following steps: the temperature of the hydrothermal reaction is 200-400 ℃, and the reaction time is 24-48 h.
The preparation method of the ferrite comprises the following steps: the temperature in the hydrothermal reaction process is adjusted by adopting a temperature programming mode, and the temperature rising rate is 5-10 ℃/min.
The preparation method of the ferrite comprises the following steps: the mass ratio of the iron oxychloride particles to the water is 0.2-0.39: 5 to 10.
In the technical scheme of the invention: the novel ferrite is applied to the preparation of penetrating agents for radiotherapy and chemotherapy for treating tumors.
The invention has the beneficial effects that:
(1) the nano-particle synthesis preparation method is simple, the preparation process is simple and efficient, a plurality of complicated synthesis steps are reduced, the preparation method is simple and clear, and the used raw materials are simple, environment-friendly and free of biotoxicity.
(2) The nano-grade iron oxychloride prepared by the invention has good biocompatibility, small particle size and petal-shaped special structure, the small particle size can increase the tumor permeability, and the petal-shaped special structure can realize secondary reflection of high-energy rays and the effect of radiotherapy sensitization.
(3) The nano ferrite prepared by the invention has good biocompatibility, regular shape and smaller particle size, can increase the uptake of tumors to the nano ferrite, can generate hydroxyl free radicals through Fenton reaction under the action of a special tumor microenvironment to cause the death of tumor cells, and improves the treatment effect of tumor chemodynamic treatment
In a word, the invention prepares the nano iron oxychloride and nano ferrite particles with special shapes and small particle size by using the cheap raw materials and the simple and clear preparation method, and the nano particles can realize the sensitivity enhancement on tumor radiotherapy and the effect of increasing the tumor chemodynamic therapy.
Drawings
FIG. 1 is a TEM image of the nano-sized iron oxychloride of example 1.
FIG. 2 is a TEM image of the nano-ferrite of example 1.
FIG. 3 is a TEM image of the nano-sized iron oxychloride of example 2.
FIG. 4 is a TEM image of the nano-ferrite of example 2.
FIG. 5 is a TEM image of the nano-sized iron oxychloride of example 3.
FIG. 6 is a TEM image of the nano-ferrite of example 3.
FIG. 7 is a chart of cytotoxicity of nano-iron oxychloride to HUVEC normal cells
FIG. 8 is a graph showing the cytotoxicity of nano-ferric oxychloride on 4T1 mouse breast cancer cells
FIG. 9 is a cytotoxicity diagram of nano ferrite on HUVEC normal cells
FIG. 10 is a cytotoxicity diagram of nano ferrite on 4T1 mouse breast cancer cells
FIG. 11 is a graph showing cytotoxicity of radiotherapy on mouse breast cancer cells after adding nano-grade iron oxychloride and nano-grade ferrite
Detailed Description
The invention is further illustrated by the following examples, without limiting the scope of the invention:
example 1
Synthesis of nano-ferric oxychloride
Weighing 420mg of ferric nitrate, dissolving in 40mL of deionized water, transferring to a three-neck flask, heating the mixed solution to 98 ℃ under the condition of reflux heating, then adding 7.65g of 98% sodium chloride solution, reacting for 8 minutes, cooling and centrifuging the reactant, washing with water for three times, and freeze-drying to obtain the nano iron oxychloride particles.
Synthesis of nano ferrite
Weighing 280mg of the prepared nano iron oxychloride particles, putting the nano iron oxychloride particles into a reaction kettle, adding 6mL of deionized water, putting the mixture into a muffle furnace, heating to 300 ℃ per minute at the temperature of 5 ℃, reacting for 36 hours, cooling after the reaction is finished, and centrifuging, washing and freeze-drying the product to obtain the nano ferrite particles.
The transmission electron microscope image of the nano iron oxychloride in the above embodiment is shown in fig. 1, and it can be obviously observed that the nanoparticles are petal-shaped and have uniform size, and the particle size is distributed between 20 nm and 40 nm.
The transmission electron microscope image of the nano ferrite in the above embodiment is shown in fig. 2, and it can be obviously observed that the nano particles are in a regular polyhedral structure, the size is uniform, and the particle size is distributed between 25 nm and 45 nm.
Example 2
Synthesis of nano iron oxychloride
Weighing 430mg of ferric nitrate, dissolving the ferric nitrate in 60mL of deionized water, transferring the solution into a three-neck flask, heating the mixed solution to 97 ℃ under the condition of reflux heating, then adding 8.38g of 95% sodium chloride solution, reacting for 7 minutes, cooling and centrifuging the reactant, washing with water for three times, and freeze-drying to obtain the nano iron oxychloride particles.
Synthesis of nano ferrite
And weighing 310mg of the prepared nano iron oxychloride particles, putting the nano iron oxychloride particles into a reaction kettle, adding 7mL of deionized water, putting the nano iron oxychloride particles into a muffle furnace, heating to 250 ℃ at 5 ℃ per minute, reacting for 32 hours, cooling after the reaction is finished, and centrifugally washing, freezing and drying the product to obtain the nano ferrite particles.
The transmission electron microscope image of the nano iron oxychloride in the above embodiment is shown in fig. 3, it can be obviously observed that the nanoparticles are petal-shaped and have uniform size, and the particle size is distributed between 20 nm and 45 nm.
The transmission electron microscope image of the nano ferrite in the above embodiment is shown in fig. 4, and it can be obviously observed that the nano particles are in a regular polyhedral structure, the size is uniform, and the particle size is distributed between 35 nm and 45 nm.
Example 3
Weighing 450mg of ferric nitrate, dissolving the ferric nitrate in 55mL of deionized water, transferring the solution into a three-neck flask, heating the mixed solution to 96 ℃ under the condition of reflux heating, then adding 6.56g of 93% sodium chloride solution, reacting for 8 minutes, cooling and centrifuging the reactant, washing for three times, and freeze-drying to obtain the nano iron oxychloride particles.
Synthesis of nano ferrite
Weighing 360mg of the prepared nano iron oxychloride particles, putting the nano iron oxychloride particles into a reaction kettle, adding 5mL of deionized water, putting the nano iron oxychloride particles into a muffle furnace, heating to 400 ℃ per minute at 5 ℃, reacting for 48 hours, cooling after the reaction is finished, and centrifugally washing, freezing and drying the product to obtain the nano ferrite particles.
The transmission electron microscope image of the nano ferric oxychloride in the above example is shown in fig. 5, and it can be obviously observed that the nano particles are petal-shaped sheet structures, have uniform size, and have particle size distribution between 20 nm and 50 nm.
The transmission electron microscope image of the nano ferrite in the above embodiment is shown in fig. 6, and it can be obviously observed that the nano particles are in a regular polyhedral structure, the size is uniform, and the particle size is distributed between 35 nm and 50 nm.
The cytotoxicity of the nano iron oxychloride on normal cells in the above embodiment is shown in fig. 7, and it can be observed that the nano particles have less toxicity on normal cells, which indicates that the biocompatibility of the particles is good.
The cytotoxicity of the nano-iron oxychloride on the mouse breast cancer cells in the example 3 is shown in fig. 8, and it can be observed that the nano-particles generate toxicity on the tumor cells when the concentration is over 100ug/mL, and kill more than 50% of the tumor cells when the concentration is 2000ug/mL, which indicates that the particles have a certain killing effect on the tumor cells.
Cytotoxicity of the nano-ferrite in example 3 to normal cells is shown in fig. 9, and it can be observed that the nano-ferrite has less toxicity to normal cells, indicating that the biocompatibility of the nano-ferrite is good.
The cytotoxicity of the nano ferrite in the embodiment 3 on the mouse breast cancer cells is shown in fig. 10, and it can be observed that the nano ferrite generates toxicity on the tumor cells when the concentration of the nano ferrite is over 100ug/mL, and kills more than 40% of the tumor cells when the concentration of the nano ferrite is 2000ug/mL, which indicates that the particles have a certain killing effect on the tumor cells
In example 3, the effect of radiotherapy treatment on breast cancer cells of mice after radiotherapy treatment and addition of nano-iron oxychloride and nano-ferrite is shown in fig. 11, and we can see that radiotherapy has a good killing effect on tumor cells, and after the nano-iron oxychloride and the nano-ferrite are added, the death rate of cells is increased after the radiotherapy treatment with the same dose of rays, which indicates that the nano-iron oxychloride and the nano-ferrite have a radiotherapy sensitization effect, and this can be attributed to the secondary reflection enhancement effect (compton scattering, auger effect) of the two kinds of nanoparticles on radiotherapy rays.
The toxicity of the nanoparticles to cells in the above examples is tested by using a CCK8 kit, and the specific operation process is as follows: HUVEC and 4T1 cells were seeded in 96-well plates (5X 10)3Cells/well), adding nanoparticles of different concentrations for co-culture, adding 10 μ L CCK8 after 24 hours, and continuing incubation for two hours, then placing the 96-well plate in a microplate reader (SPARK TECAN) to detect and analyze absorbance of each well at 450nm, and the cell viability is calculated as: [ A (Add medicine) -A (blank)]/[ A (control) -A (blank)]X 100%, where A is the absorbance at 450nm for each group, blank is a group to which medium alone was added without culturing cells, control is a group to which medium was added and cells were inoculated, and dosed is a group to which various concentrations of nanoparticles were co-cultured with cells.
The radiosensitization effect of the nanoparticles on cells in the embodiment is tested by using a CCK8 kit, and the specific operation process is as follows: 4T1 cells are inoculated in 96 holes, 1ug/mL of nano-ferric chloride and nano-ferrite are added for co-culture, 10uL of CCK8 reagent is added after 2Gy dose radiotherapy, after incubation for 2h, the absorbance of each hole at 450nm is detected by a microplate reader, and the cell activity is calculated according to the method.
Claims (9)
1. A novel ferrite is characterized in that: the ferrite is prepared by carrying out hydrothermal reaction on ferric oxychloride particles with the particle size of 10-100 nm to prepare the ferrite with the particle size of 20-50 nm.
2. The novel ferrite of claim 1, wherein: the preparation method of the nano iron oxychloride particles comprises the following steps: dissolving ferric nitrate nonahydrate in deionized water, heating the mixed solution to 92-98 ℃ under the reflux condition, then adding a sodium chloride solution, reacting for 5-10 minutes, cooling, centrifuging, washing with water, and freeze-drying to obtain 20-50 nm ferric oxychloride particles.
3. The novel ferrite of claim 2, wherein: the mass ratio of ferric nitrate nonahydrate to sodium chloride solution to deionized water is (0.4-0.48): 4-10: 40-60, wherein: the mass concentration of the sodium chloride solution is 93-99%.
4. The novel ferrite as claimed in claim 1 or 2, wherein: the particle size of the nano ferric oxychloride particles is between 20 and 40nm, and the nano ferric oxychloride particles are in a petal-shaped sheet structure.
5. A novel preparation method of ferrite is characterized by comprising the following steps: the preparation method comprises the following steps: the iron oxychloride particles prepared in claim 2 are uniformly mixed with water, and then subjected to hydrothermal reaction to prepare the nano ferrite with the particle size of 20 nm-50 nm.
6. The method of claim 5, wherein: the temperature of the hydrothermal reaction is 200-400 ℃, and the reaction time is 24-48 h.
7. The method of claim 6, wherein: the temperature in the hydrothermal reaction process is adjusted by adopting a temperature programming mode, and the temperature rising rate is 5-10 ℃/min.
8. The method of claim 5, wherein: the mass ratio of the iron oxychloride particles to the water is 0.2-0.39: 5 to 10.
9. Use of the novel ferrite of claim 1 for the preparation of a penetrating agent for radiotherapy and chemotherapy for the treatment of tumors.
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