CN115245498A - Method for preparing near infrared absorption magnetic nano particles - Google Patents
Method for preparing near infrared absorption magnetic nano particles Download PDFInfo
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- CN115245498A CN115245498A CN202111626103.5A CN202111626103A CN115245498A CN 115245498 A CN115245498 A CN 115245498A CN 202111626103 A CN202111626103 A CN 202111626103A CN 115245498 A CN115245498 A CN 115245498A
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- mxene
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- infrared absorption
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/51—Nanocapsules; Nanoparticles
- A61K9/5107—Excipients; Inactive ingredients
- A61K9/5115—Inorganic compounds
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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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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P37/00—Drugs for immunological or allergic disorders
- A61P37/02—Immunomodulators
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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
Abstract
A process for preparing the magnetic nanoparticles able to absorb near infrared ray includes dissolving single-layer MXene in water, ultrasonic treating in ice bath, centrifugal removing deposit by 5,000rmp, centrifugal resuspending the deposit by 10,000rmp, baking and preparing MXene solution (1.0 mg/mL). FeCl is added 3 .6H 2 O was dissolved in ethylene glycol and stirred to form a yellow-brown solution, naOH and MXene were added first. Then, the mixture solution is transferred into an autoclave after being stirred, is kept at 180 ℃ for 10 hours, and is cooled to room temperature to obtain a black product; finally, washing the magnetic nanoparticles with water and ethanol respectively and drying the magnetic nanoparticlesFe 3 O 4 @ MXene. The magnetic nano particles Fe prepared by the invention 3 O 4 @ MXene, can also label cells, utilize the external magnetic field to control cells or target tissues under the effect, exert infrared effect again, reach treatment purpose, for example: activate immune response, and kill cancer cells.
Description
Technical Field
The invention relates to a magnetic composite material, in particular to a nano particle formed by coating a polymer outside a magnetic particle and a preparation method thereof.
Background
Magnetic Nanoparticles/Magnetic Nanoparticles (MNPs) are novel materials that have been developed rapidly and have great application value in recent years, and are increasingly widely used in many fields of modern science, such as biomedicine, magnetofluid, catalysis, nuclear Magnetic resonance imaging, data storage, environmental protection, and the like.
The magnetic composite nano particles are nano-sized particles and generally comprise a magnetic inner core consisting of metal oxides such as iron, cobalt, nickel and the like and a high polymer/silicon/hydroxyapatite shell layer wrapping the magnetic inner core. The most common core layer is made of Fe with superparamagnetic or ferromagnetic properties 3 O 4 Or gamma-Fe 2 O 3 The magnetic guide type magnetic separation device has magnetic guidance (targeting), can realize directional movement under the action of an external magnetic field, and is convenient to position and separate from a medium. The magnetic composite nano particles have the characteristics of superparamagnetism and macromolecules, and have magnetic guidance, biocompatibility, small-size effect, surface effect, active groups and certain biomedical functions.
MXene materials are a class of metal carbide and metal nitride materials with a two-dimensional layered structure, are used as a new generation of energy materials, and are known as next generation energy storage materials with the best development prospect. Among them, titanium carbide MXene nanosheets are more common.
CN110160646A discloses a method for preparing a flexible near infrared detector containing MXene, which comprises the steps of packaging an ink solution containing MXene, writing or spraying on a substrate, and bonding double-sided copper foil adhesive on two ends of the substrate to obtain the flexible near infrared detector containing MXene.
CN113060734A discloses an infrared low-emissivity MXene film and a preparation method thereof, wherein MXene solution is poured into a filter flask with a filter membrane, MXene is uniformly loaded on the surface of the filter membrane through vacuum filtration, and an MXene thin layer is formed on the surface of the filter membrane; and then separating the dried MXene thin layer from the filter membrane to obtain the MXene film which is used for infrared stealth and thermal camouflage of the MXene film with low infrared emissivity.
Disclosure of Invention
The invention aims to provide a method for preparing near-infrared absorption magnetic nano particles, which wraps Fe on a near-infrared absorption MXene nano sheet layer 3 O 4 To prepare magnetic nano-particle Fe 3 O 4 @MXene。
Another object of the present invention is to provide a method for preparing near-infrared absorbing magnetic nanoparticles for the purpose of post-exposure treatment of target cells or tissues.
A method for preparing near-infrared absorbing magnetic nanoparticles, comprising the steps of:
dissolving MXene in water, carrying out ice bath ultrasonic treatment for more than 5 hours, centrifuging at 5000rpm to remove precipitates, and cleaning for three times;
then, the mixture is centrifuged at 10,000rmp for 20 minutes, and the precipitate is resuspended to prepare 1.0mg/mL MXene solution;
0.6g FeCl 3 .6H 2 Dissolving O in Ethylene Glycol (EG), stirring at room temperature to form a yellowish brown solution, adding 1mL NaOH (10 mM) and then 5mL MXene (1.0 mg/mL) while stirring;
then, the mixture solution was vigorously stirred for 10 minutes, and then transferred to an autoclave and kept at 180 ℃ for 10 hours, and then cooled to room temperature to obtain a black product;
finally, washing the magnetic nano particle by water and ethanol for three times respectively, and drying the magnetic nano particle in an oven at 60 ℃ to obtain the magnetic nano particle Fe 3 O 4 @MXene。
The resulting particle size may be from 5nm to 10 μm, for example: 1-10 μm. Magnetic particles of 5nm to 50nm are preferred.
The method of the invention, centrifugation at 5000rpm for 10 minutes.
In the method, the ultrasonic treatment is carried out for 8 hours.
The method of the invention is carried out at room temperature with stirring at 2500 rpm.
The magnetic nano particle Fe prepared by the invention 3 O 4 @ MXene co-cultured with cells (such as but not limited to fibroblasts, mesenchymal stem cells and adipose stem cells, etc.) and endocytosed into cellsIs intracellular and can be maintained in the cell for a long time without being excreted out of the cell by exocytosis, thereby facilitating the operation of the cell.
The magnetic nano particles Fe prepared by the invention 3 O 4 @ MXene, can also utilize external magnetic field to control cells or target tissues, and then apply infrared action to achieve the therapeutic purposes, such as: activate immune response, and kill cancer cells.
Drawings
FIG. 1 shows the magnetic nanoparticles of the present invention Fe 3 O 4 @ MXene Transmission Electron microscopy;
FIG. 2 is a magnetic hysteresis loop of magnetic nanoparticles Fe3O4@ MXene of the present invention;
FIG. 3 is an XRD pattern of the magnetic nanoparticle Fe3O4@ MXene of the present invention;
FIG. 4 is a diagram of the ultraviolet absorption spectrum of the magnetic nanoparticle Fe3O4@ MXene of the present invention;
FIG. 5 is the field view of confocal microscope after co-culture of magnetic nanoparticles Fe3O4@ MXene and cells.
Detailed Description
The technical scheme of the invention is described in detail in the following with reference to the accompanying drawings. Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.
Preparing Fe by a hydrothermal method 3 O 4 @ MXene nano-magnetic particles: weighing 1g MXene dissolved in 20mLdH 2 Placing the mixture in a 200W ultrasonic instrument, performing ice bath ultrasonic treatment for 8 hours, centrifuging at 5000rpm for 10 minutes, removing precipitates, and cleaning for three times; after centrifugation at 10000rmp for 20 min, the pellet was resuspended and made into 1.0mg/mL MXene solution for further use. 0.6g FeCl 3 .6H 2 O was dissolved in 25mL Ethylene Glycol (EG), stirred vigorously at room temperature for 30 minutes to form a clean yellow-brown solution, and then 1mL NaOH (10 mM) was added with stirring. Subsequently, the solution was added while stirringTo this was added 5mL of MXene (1.0 mg/mL). Finally, the mixture solution was vigorously stirred for 10 minutes, and then transferred to a 40mL polytetrafluoroethylene-lined stainless steel autoclave and maintained at 180 ℃ for 10 hours. The autoclave was then cooled to room temperature. Washing the obtained black product with deionized water and ethanol for three times respectively, and drying in a drying oven at 60 ℃ to obtain the magnetic nano particle Fe 3 O 4 @ MXene, as shown in FIG. 1, the particle size was about 10 nm.
As shown in FIG. 3, the nanoparticles Fe obtained in this example 3 O 4 @ MXene containing Fe 3 O 4 . FIG. 2 shows that Fe was obtained 3 O 4 The @ MXene particles are superparamagnetic and have good response capability to a magnetic field. The infrared spectrum shows that the nano particle Fe obtained in the example 3 O 4 @ MXene has a UV absorption peak as shown in FIG. 4.
Mixing Fe 3 O 4 @ MXene was used to label MGC-803 cells. And observing the imaging condition. The experimental procedure was as follows:
fe to be dissolved in the culture medium 3 O 4 @ MXene was co-incubated for 3h with MGC-803 cells in a cell culture plate with a final concentration of 500. Mu.g/ml for 3h. Fe that did not enter cells and did not bind to cells was washed 3 times with 0.01M PBS using a magnet to provide a magnetic field 3 O 4 @ MXene was washed well and stained for nuclei with DAPI. After 5 minutes, washing with 0.01M PBS solution for 3 times, fixing the cells with 2% paraformaldehyde, making cell slide, placing under TCS SP5-II Leica laser confocal microscope with excitation light source of 530nm and emission light receiving of 650nm, and observing Fe 3 O 4 Interaction of @ MXene with MGC-803 cells and imaging of nanoparticles in gastric cancer cells, as shown in FIG. 5.Fe 3 O 4 @ MXene is endocytosed into cells and can be maintained inside cells for a long period of time without being excreted outside cells by exocytosis.
Claims (6)
1. A method for preparing near-infrared absorption magnetic nano particles is characterized by comprising the following steps:
dissolving MXene in water, carrying out ice bath ultrasonic treatment for more than 5 hours, centrifuging at 5000rpm to remove precipitates, and cleaning for three times;
then, the mixture is centrifuged at 10,000rmp for 20 minutes, and the precipitate is resuspended to prepare 1.0mg/mL MXene solution;
0.6g FeCl 3 .6H 2 Dissolving O in ethylene glycol, stirring at room temperature to form a yellowish-brown solution, and adding 1mL of NaOH and MXene while stirring;
then, the mixture solution was vigorously stirred for 10 minutes, and then transferred to an autoclave and kept at 180 ℃ for 10 hours, and then cooled to room temperature to obtain a black product;
finally, washing the magnetic nano particle by water and ethanol for three times respectively, and drying the magnetic nano particle in an oven at 60 ℃ to obtain the magnetic nano particle Fe 3 O 4 @MXene。
2. The method for preparing magnetic nanoparticles with near infrared absorption as claimed in claim 1, wherein the NaOH is 10mM.
3. The method of claim 1 wherein the amount of MXene used is 5mL.
4. The method for preparing magnetic nanoparticles with near infrared absorption according to claim 1, wherein the sonication is carried out for 8 hours.
5. The method for preparing magnetic nanoparticles with near infrared absorption according to claim 1, wherein the magnetic nanoparticles are centrifuged at 5000rpm for 10 minutes.
6. The method for preparing magnetic nanoparticles with near infrared absorption according to claim 1, wherein the stirring is vigorously carried out at room temperature for 30 minutes.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108251054A (en) * | 2018-03-23 | 2018-07-06 | 中国工程物理研究院材料研究所 | A kind of composite wave-suction material and preparation method thereof |
| CN108342036A (en) * | 2018-03-26 | 2018-07-31 | 南昌航空大学 | A kind of magnetism Mxenes polymer composite wave-suction materials and preparation method thereof |
| CN112047386A (en) * | 2020-08-27 | 2020-12-08 | 西北工业大学 | Heating modified MXene/ferroferric oxide composite wave-absorbing material and preparation method thereof |
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- 2021-12-28 CN CN202111626103.5A patent/CN115245498A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108251054A (en) * | 2018-03-23 | 2018-07-06 | 中国工程物理研究院材料研究所 | A kind of composite wave-suction material and preparation method thereof |
| CN108342036A (en) * | 2018-03-26 | 2018-07-31 | 南昌航空大学 | A kind of magnetism Mxenes polymer composite wave-suction materials and preparation method thereof |
| CN112047386A (en) * | 2020-08-27 | 2020-12-08 | 西北工业大学 | Heating modified MXene/ferroferric oxide composite wave-absorbing material and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| GUOLIANG ZHAO ET AL.: "Self-Assembled Sandwich-like MXene-Derived Nanocomposites for Enhanced Electromagnetic Wave Absorption" * |
| PEIJIANG LIU ET AL.: "Facile synthesis of ultrasmall Fe3O4 nanoparticles on MXenes for high microwave absorption performance" * |
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