CN112402604A - Composite nano material of calcium peroxide wrapped by silicon dioxide, preparation method and application thereof - Google Patents

Composite nano material of calcium peroxide wrapped by silicon dioxide, preparation method and application thereof Download PDF

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CN112402604A
CN112402604A CN202011201233.XA CN202011201233A CN112402604A CN 112402604 A CN112402604 A CN 112402604A CN 202011201233 A CN202011201233 A CN 202011201233A CN 112402604 A CN112402604 A CN 112402604A
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nano material
calcium peroxide
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sio
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王春梅
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Shanghai East Hospital Tongji University Affiliated East Hospital
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K41/00—Medicinal preparations obtained by treating materials with wave energy or particle radiation ; Therapies using these preparations
    • A61K41/0028—Disruption, e.g. by heat or ultrasounds, sonophysical or sonochemical activation, e.g. thermosensitive or heat-sensitive liposomes, disruption of calculi with a medicinal preparation and ultrasounds
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    • 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
    • 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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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
    • C01B15/04—Metal peroxides or peroxyhydrates thereof; Metal superoxides; Metal ozonides; Peroxyhydrates thereof
    • C01B15/043—Metal peroxides or peroxyhydrates thereof; Metal superoxides; Metal ozonides; Peroxyhydrates thereof of alkali metals, alkaline earth metals or magnesium or beryllium or aluminium
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    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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Abstract

A composite nanometer material of calcium peroxide wrapped by silicon dioxide comprises a calcium peroxide nanometer material, wherein the surface of the calcium peroxide nanometer material is coated with the silicon dioxide to form SiO2@CaO2Composite nanoRice material, then in said SiO2@CaO2The surface of the composite nano material is modified by 3-aminopropyl triethoxysilane to obtain amino modified SiO2@CaO2Namely a composite nano material of calcium peroxide wrapped by silicon dioxide. The invention also provides a preparation method of the composite nano material. The invention also provides application of the composite nano material in preparing a medicine for enhancing high-intensity focused ultrasound treatment of tumors. The invention can make SiO reaching the tumor area2@CaO2‑NH2The nano material is decomposed in the tumor environment to generate oxygen, so that the cavitation effect in the HIFU treatment process is enhanced, and the aim of enhancing the curative effect of the HIFU treatment is fulfilled.

Description

Composite nano material of calcium peroxide wrapped by silicon dioxide, preparation method and application thereof
The technical field is as follows:
the invention belongs to the field of biomedicine and nano materials, and relates to a calcium peroxide nano material, in particular to a composite nano material of calcium peroxide wrapped by silicon dioxide and capable of enhancing the treatment effect of High Intensity Focused Ultrasound (HIFU), and a preparation method and application thereof.
Background art:
high-intensity focused ultrasound therapy is a novel method of tumor therapy. When the method is used for treating the tumor, the ultrasonic positioning can be utilized, and the characteristics of a specific target area are focused to generate instant high temperature and cavitation effect, so that the tumor is coagulatively necrotic, and the minimally invasive treatment of the tumor tissue is realized. However, high-intensity focused ultrasound requires higher ultrasound power during the treatment process, and inevitably damages surrounding normal tissues while killing tumor cells. Therefore, it is of great clinical significance to further enhance the treatment efficiency during the HIFU treatment while reducing the ultrasound power.
The invention content is as follows:
the invention aims to provide a composite nano material of calcium peroxide wrapped by silicon dioxide, a preparation method and application thereof, and aims to solve the technical problem that in the prior art, high-intensity focused ultrasound is adopted in the treatment process to kill tumor cells and damage surrounding normal tissues at the same time.
The invention provides a composite nano material of calcium peroxide coated by silicon dioxide, which comprises a calcium peroxide nano material, wherein the surface of the calcium peroxide nano material is coated by silicon dioxide to form SiO2@CaO2Compounding the nano material, then preparing the SiO2@CaO2The surface of the composite nano material is modified by 3-aminopropyl triethoxysilane to obtain amino modified SiO2@CaO2Namely a composite nano material of calcium peroxide wrapped by silicon dioxide.
Furthermore, the particle size range of the calcium peroxide nano material is 5-50 nm.
The invention also provides a preparation method of the composite nano material of calcium peroxide coated by silicon dioxide, which comprises the following steps:
1) adding CaCl2Dissolving in water, adding an ammonia water solution into the solution, wherein the concentration of the ammonia water solution is 0.5-1.5 mol/L, stirring, and adding H2O2Said H2O2The mass percentage concentration of the CaCl is 25-35%, the mixed solution is stirred at room temperature, and the CaCl is added2、Aqueous ammonia solution, H2O2The material ratio of (A) is 200 mg: 0.5-2 mL: 0.5-2 mL; adding a NaOH solution until the clarified solution becomes a white suspension, wherein the concentration of the NaOH solution is 0.5-2 mol/L, and finally centrifuging and collecting to obtain the calcium peroxide nano material;
2) dissolving the calcium peroxide nano material obtained in the step 1) into an ethanol solution, adding an ammonia water solution, stirring at room temperature, then adding an ethyl orthosilicate ethanol solution, wherein the volume percentage concentration of the ethyl orthosilicate ethanol solution is 0.5-1.5%, and the material ratio of the calcium peroxide nano material to the ammonia water solution to the ethyl orthosilicate solution is 2 mg: 0.05-0.2 mL: 0.05-2 mL; after stirring, centrifugally collecting and washing to obtain SiO2@CaO2A composite nanomaterial;
3) SiO obtained in step 2)2@CaO2Dispersing the composite nano material in ethanol solution, and then adding 3-aminopropyl triethoxysilane, wherein SiO is2@CaO2The material ratio of the composite nano material to the 3-aminopropyltriethoxysilane is 100 mg: 0.5-5 mL; refluxing for 8-16 hours at 70-95 ℃ to obtain amino modified SiO2@CaO2 (SiO2@CaO2-NH2) Namely the composite nano material of the calcium peroxide wrapped by the silicon dioxide.
Specifically, the mass percentage concentration of the ethanol solution is more than 98%.
The invention also provides application of the composite nano material of calcium peroxide coated by silicon dioxide in preparing a medicament for enhancing high-intensity focused ultrasound to treat tumors.
Calcium peroxide may react with water to produce oxygen, which may be used to enhance the cavitation effect during HIFU therapy. The cavitation effect is, in particular, the dynamic process of growth and collapse that occurs when microbubbles present in a liquid vibrate under the action of sound waves and when the sound pressure reaches a certain value. At the moment of bubble collapse, a huge instantaneous pressure is generated, generally up to tens of megapascals to hundreds of megapascals, generating high temperature accompanied by strong shock waves and microjets with a speed of 400 km per hour. The huge instantaneous pressure can effectively kill tumor tissues. The pure calcium peroxide is easy to agglomerate, so that the silicon dioxide layer is coated on the surface of the calcium peroxide, the dispersity of the calcium peroxide is improved, the contact of the calcium peroxide and water molecules is reduced, and the leakage of medicines is reduced. Finally, the surface of the silicon dioxide layer is further subjected to amino modification, so that the stability and the dispersibility of the silicon dioxide layer in a physiological environment can be further improved.
The innovation points of the invention are as follows:
1) the invention innovatively uses silicon dioxide to stabilize the oxygen-producing material calcium peroxide, and finally the calcium peroxide is prevented from agglomerating and is monodisperse.
2) The material has high biological safety performance, and in vivo mouse animal experiments show that the blood routine and liver and kidney functions of a mouse are observed after one month under the condition that the tail vein injection of a Kunming mouse reaches 20mg/kg, and no obvious abnormal change is found to the experimental mouse.
3) The oxygen generating efficiency is high, a large amount of oxygen can be generated in a tumor area, the cavitation effect of HIFU treatment is greatly improved, tumor cells are effectively killed, and the method has important significance for synergistic HIFU treatment.
Compared with the prior art, the invention has remarkable technical progress. The invention can make SiO reaching the tumor area2@CaO2-NH2The nano material is decomposed in a tumor microenvironment to generate oxygen, so that the cavitation effect in the HIFU treatment process is enhanced, and the aim of enhancing the curative effect of the HIFU treatment is fulfilled. The method adopted by the invention is simple, convenient, rapid, economical, applicable and high in repeatability.
Description of the drawings:
FIG. 1 shows CaO2Electron micrograph of TEM.
FIG. 2 is SiO2@CaO2Electron micrograph of TEM.
FIG. 3 shows the observation of SiO under ultrasound2@CaO2Oxygen production.
FIG. 4 shows SiO in vitro gels2@CaO2Sea richness and synergistic effect.
FIG. 5 shows SiO in 4T1 mammary gland tumor-bearing mice2@CaO2And (4) an ultrasonic effect chart of HIFU treatment.
FIG. 6 shows SiO in 4T1 mammary gland tumor-bearing mouse2@CaO2Pathological section picture of animal experiment.
FIG. 7 shows tail vein injection of SiO2@CaO2Blood routine and liver and kidney function indices of Kunming mice one month later.
The specific implementation mode is as follows:
example 1
200mg of CaCl2Dissolving in 2mL of water solution, adding 1 mL of ammonia solution (1M) into the solution, rapidly stirring for 30 minutes, and adding 1 mL of H with the mass percent concentration of 30% dropwise2O2. And stirring the mixed solution at room temperature for 1 hour, then slowly adding 1 mol/L NaOH solution until the clarified solution becomes a white suspension, finally centrifuging and collecting, washing for a plurality of times by using absolute ethyl alcohol (the mass percentage concentration is 98%), and storing the absolute ethyl alcohol (the mass percentage concentration is 98%) at 4 ℃ for later use to obtain the calcium peroxide nano material (the particle size range data is 5-50 nm).
Example 2
2mg of the calcium peroxide nanomaterial obtained above was added to 25 ml of an anhydrous ethanol solution (mass percentage concentration: 98%), 0.1 ml of concentrated ammonia water (concentration: 1 mol/L) was added, and the mixture was gently stirred at room temperature for 1 hour, and then 0.1 ml of ethyl orthosilicate was dissolved in 10 ml of ethanol, and the solution was added to the above solution and stirred for 6 hours. Then, the product collected by centrifugation was washed three times with anhydrous ethanol (mass percentage concentration: 98%) to remove impurities, to obtain SiO2@CaO2A composite nanomaterial. Finally, the collected product was stored in absolute ethanol (mass percent) at 4 ℃Specific concentration of 98%) for standby.
As can be seen from FIG. 1, SiO is clearly seen from the high resolution electron microscope2Successfully wrap the CaO2The surface of the nanoparticles (20 nm for A and 50nm for B).
Finally, 100mg SiO2@CaO2Is dispersed in 40 ml of absolute ethyl alcohol (the mass percentage concentration is 98 percent). Adding 1 mL of 3-aminopropyltriethoxysilane, refluxing at 80 ℃ for 12 hours to obtain amino-modified SiO2@CaO2 (SiO2@CaO2-NH2). The obtained SiO2@ CaO2-NH2Centrifuged and washed with ethanol three times. Finally, it was stored in ethanol for later use.
As a result: the synthesized nano particles have good dispersibility and the particle size is about 5-50 nm.
Example 3
Observation of SiO under ultrasound2@CaO2Oxygen production, divided into two groups, a pure water control group, and a control group containing SiO2@CaO2And (4) an aqueous solution group. Mixing 8 mg of SiO2@CaO2100 microliters of the aqueous solution was dispersed in 4 milliliters of water, and then observed under ultrasound, and a large amount of bubbles were observed to be generated (fig. 2).
Example 4
Simulating human tissue with in vitro gel, observing SiO under ultrasound2@CaO2The synergistic therapeutic effect of HIFU treatment is divided into two groups, one HIFU irradiation group and the other SiO2@CaO2+ HIFU group. SiO22@CaO2The injection dosage is 1 milligram per milliliter, and the HIFU ultrasonic power is 340W. And then ultrasonically observing the HIFU synergistic effect. It can be seen that the range of HIFU treatment is significantly larger than the HIFU treatment group alone (fig. 4). FIG. 4 shows SiO in vitro gels2@CaO2Sea-rich synergistic effect sonogram (left) and gel photograph (right).
Example 5
4T1 mammary gland tumor-bearing mouse tail vein injection SiO2@CaO2After the PBS solution is added, the injection dose is 20mg/kg, the injection amount is 100 microliters, then HIFU irradiation is carried out, the treatment power is 340W, and the synergistic treatment effect of the HIFU is observed under ultrasoundAnd (5) fruit. As can be seen, SiO was injected2@CaO2The extent of HIFU treatment after nanoparticles is greater (fig. 5).
Example 6
4T1 mammary gland tumor-bearing mouse HIFU treatment experiment, divided into four groups (5 mice with 4T1 mammary gland tumor-bearing each group), control group, SiO2@CaO2Group, simple HIFU treatment group and SiO2@CaO2+ HIFU treatment group, SiO2@CaO2The injection dose is 20mg/kg, the injection amount is 100 microliters, the HIFU irradiation treatment power is 340W, the tumor of the mouse is dissected after the treatment is finished, the tumor is sent to the pathology to be sliced and stained, and the treatment effect is confirmed.
The results show that SiO2@CaO2The + HIFU treatment group has the best treatment effect and better effect than the single HIFU treatment group (figure 6).
Example 7
Kunming mouse safety evaluation test, four groups (5 Kunming mice in each group), a control group, a 5mg/kg dose group, a 10mg/kg dose group and a 20mg/kg dose group are divided. Tail vein injection of SiO2@CaO2The dosages were 0, 5mg/kg, 10mg/kg and 20mg/kg, respectively. The injection volume was 100 microliters. One month later, blood of each group of experimental mice was taken and blood routine and liver and kidney function examination was performed, including blood routine hematocrit level (HCT), Hemoglobin (HGB), lymphocyte ratio (LYM), mean hemoglobin (MCH), mean hemoglobin concentration (MCHC), Mean Corpuscular Volume (MCV), median cell count (MID), Mean Platelet Volume (MPV), Neutrophil (NEUT), platelet-Pressure (PCT), Platelet (PLT), Red Blood Cell (RBC), White Blood Cell (WBC), creatinine (klebsia), urea (CREA), alanine Aminotransferase (ALT), aspartate Aminotransferase (AST), alkaline phosphatase (ALP).
The results show that SiO2@CaO2At the injection dose of 20mg/kg, there was no significant abnormality in the blood routine and liver kidney function of the mice as compared with the control group (FIG. 7).

Claims (4)

1. A composite nano material of calcium peroxide wrapped by silicon dioxide is characterized in that: comprises a calcium peroxide nano-material and a calcium oxide nano-material,coating silicon dioxide on the surface of the calcium peroxide nano material to form SiO2@CaO2Compounding the nano material, then preparing the SiO2@CaO2The surface of the composite nano material is modified by 3-aminopropyl triethoxysilane to obtain amino modified SiO2@CaO2Namely a composite nano material of calcium peroxide wrapped by silicon dioxide.
2. The silica-coated calcium peroxide composite nanomaterial according to claim 1, wherein: the particle size range of the calcium peroxide nano material is 5-50 nm.
3. The method for preparing the composite nano material of calcium peroxide coated by silicon dioxide as claimed in claim 1, which is characterized by comprising the following steps:
1) adding CaCl2Dissolving in water, adding an ammonia water solution into the solution, wherein the concentration of the ammonia water solution is 0.5-1.5 mol/L, stirring, and adding H2O2Said H2O2The mass percentage concentration of the CaCl is 25-35%, the mixed solution is stirred at room temperature, and the CaCl is added2、Aqueous ammonia solution, H2O2The material ratio of (A) is 200 mg: 0.5-2 mL: 0.5-2 mL; adding a NaOH solution until the clarified solution becomes a white suspension, wherein the concentration of the NaOH solution is 0.5-2 mol/L, and finally centrifuging and collecting to obtain the calcium peroxide nano material;
2) dissolving the calcium peroxide nano material obtained in the step 1) into an ethanol solution, adding an ammonia water solution, stirring at room temperature, then adding an ethyl orthosilicate ethanol solution, wherein the volume percentage concentration of the ethyl orthosilicate ethanol solution is 0.5-1.5%, and the material ratio of the calcium peroxide nano material to the ammonia water solution to the ethyl orthosilicate solution is 2 mg: 0.05-0.2 mL: 0.05-2 mL; after stirring, centrifugally collecting and washing to obtain SiO2@CaO2A composite nanomaterial;
3) SiO obtained in step 2)2@CaO2Dispersing the composite nano material in ethanol solution, and then adding 3-aminopropyl triethoxysilane, wherein SiO is2@CaO2The material ratio of the composite nano material to the 3-aminopropyltriethoxysilane is 100 mg: 0.5-5 mL; refluxing for 8-16 hours at 70-95 ℃ to obtain amino modified SiO2@CaO2Namely the composite nano material of the calcium peroxide wrapped by the silicon dioxide.
4. Use of the silica-coated calcium peroxide composite nanomaterial of claim 1 in the preparation of a medicament for enhancing tumor treatment by high intensity focused ultrasound.
CN202011201233.XA 2020-11-02 2020-11-02 Composite nano material of calcium peroxide wrapped by silicon dioxide, preparation method and application thereof Pending CN112402604A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113694247A (en) * 2021-08-09 2021-11-26 北京化工大学 Preparation method of multifunctional composite hemostatic sponge
CN115025052A (en) * 2022-06-27 2022-09-09 天津大学 Calcium peroxide and manganese dioxide based nano particle with oxygen production and oxidation resistance and preparation method thereof

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113694247A (en) * 2021-08-09 2021-11-26 北京化工大学 Preparation method of multifunctional composite hemostatic sponge
CN113694247B (en) * 2021-08-09 2022-08-23 北京化工大学 Preparation method of multifunctional composite hemostatic sponge
CN115025052A (en) * 2022-06-27 2022-09-09 天津大学 Calcium peroxide and manganese dioxide based nano particle with oxygen production and oxidation resistance and preparation method thereof
CN115025052B (en) * 2022-06-27 2023-04-18 天津大学 Calcium peroxide and manganese dioxide based nano particle with oxygen production and oxidation resistance and preparation method thereof

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Application publication date: 20210226