Preparation method and application of monodisperse magnetic bead material with controllable particle size
Synthesis and surface modification of large-particle ferromagnetic beads through hydrothermal method, solving the size and surface area limitations of existing magnetic beads in biological enrichment and clinical diagnosis, and achieving more efficient biological separation and detection capabilities.
Patent Information
- Application Number
- CN202311154881.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2023-09-03
- Publication Date
- 2025-03-04
AI Technical Summary
The existing magnetic beads are small in size during biological enrichment, difficult to separate quickly, and have a small surface area, which limits their application in clinical diagnosis and medical research.
The hydrothermal method synthesized ferromagnetic beads with controllable particle size, combined with silica shell and amino modification, to form a monodisperse magnetic bead material with large particle size and good surface modification.
Larger-sized magnetic beads are achieved, rapid separation ability of bioenrichment is improved, surface area is increased, and a broader application space is provided for detection and research in the field of biomedical science.
Smart Images
Figure CN119549116A_ABST
Abstract
Description
Technical Field
[0001] The magnetic beads synthesized by the hydrothermal method in this patent have a larger size compared to other similar products. They can be separated better and faster during the bio-enrichment process. Secondly, the large-size magnetic beads have a larger surface area, which provides the possibility of enriching their surface modification and increasing their detection limit in clinical diagnosis. In addition, in the field of medical research, they can better enrich some trace biomarkers, providing convenience for in-depth research in scientific research. Background Art
[0002] With the development of science and technology, in the field of biomedical research, the enrichment and purification of some specific target substances are becoming increasingly important, especially for some biomarkers that exist in trace amounts, such as proteins and nucleic acids. Purification through large-sized magnetic nanoparticles can provide research materials for subsequent research to a great extent, enriching researchers' research on their biological functions; in clinical diagnosis, the enrichment effect of large-sized magnetic beads can provide the possibility of minimally invasive diagnosis. While minimizing the damage to patients when extracting samples, it improves the detection limit of clinical diagnosis. Provide accurate guarantees for patients' diagnosis and strive for more living space for them. Summary of the invention
[0003] The purpose of this patent is to provide a method for preparing a monodisperse magnetic bead material with controllable particle size. The prepared iron-based magnetic nanomaterial controls the particle size between 100-1000 nanometers by adjusting the reaction conditions. On the one hand, the magnetic nanoparticles exhibit excellent magnetic characteristics. On the other hand, the surface modification of the nanoparticles shows a wide range of application space in the biomedical field. Therefore, the preparation of monodisperse magnetic bead materials with controllable particle size has important potential application value.
[0004] The monodisperse magnetic bead material with controllable particle size in this patent is formed by the reaction of ferric chloride hexahydrate, sodium acetate and PEG2000 in polyethylene glycol. The surfactant PEG2000 plays a very important role in the formation of monodisperse magnetic beads. Finally, high-quality monodisperse magnetic bead material is obtained by washing with ethanol and distilled water.
[0005] The method for preparing a monodisperse magnetic bead material with controllable particle size provided in this patent comprises the following steps:
[0006] 1) Preparing ferroferric oxide magnetic beads of different particle sizes;
[0007] 2) coating the surface of the prepared ferroferric oxide nanoparticles with a silicon dioxide shell layer;
[0008] 3) performing amino modification on the surface of the prepared ferroferric oxide nanoparticles;
[0009] Step 1) dissolving ferric chloride hexahydrate, sodium acetate and PEG2000 in polyethylene glycol at room temperature and stirring overnight;
[0010] Step 2) Place the prepared mixed solution in a muffle furnace and react at 150-240°C for 6-24 hours
[0011] Step 3) The prepared ferroferric oxide nanoparticles are dissolved in an ethanol / water mixed solvent, and a silica shell layer is formed on the surface of the magnetic beads by an emulsion method using ethyl orthosilicate and ammonia water.
[0012] Step 4) The prepared ferroferric oxide nanoparticles are dissolved in an ethanol / water mixed solvent, and the surfaces of the magnetic beads are amino-modified by an emulsion method using tetraethyl orthosilicate, 3-aminopropyltriethoxysilane and ammonia water.
[0013] This patent further provides structural identification and magnetic testing of the above-mentioned ferroferric oxide nanoparticles, further illustrating their potential applications in the biomedical field. BRIEF DESCRIPTION OF THE DRAWINGS
[0014] Figure 1 This is a scanning electron microscope image of the functionalized modified 900 nm ferrosoferric oxide nanoparticles prepared in Example 1.
[0015] Figure 2 This is a scanning electron microscope image of 400nm ferrosoferric oxide nanoparticles prepared in Example 2.
[0016] Figure 3 This is the hysteresis curve of the 900nm ferrosoferric oxide particles prepared in Example 1.
[0017] Figure 4 This is the particle size distribution diagram of 900nm ferrosoferric oxide particles prepared in Example 1.
[0018] Figure 5 This is the X-ray diffraction analysis diagram of the functionalized modified 900nm ferrosoferric oxide nanoparticles prepared in Example 1.
[0019] Figure 6 This is the X-ray photoelectron spectrum of the functionalized modified 900nm ferrosoferric oxide nanoparticles prepared in Example 1.
[0020] Figure 7 This is the infrared spectrum analysis diagram of the functionalized modified 900nm ferrosoferric oxide nanoparticles prepared in Example 1. DETAILED DESCRIPTION
[0021] The contents of this patent will be described clearly and completely below in conjunction with the embodiments, but the scope of this patent is not limited to the embodiments.
[0022] Example 1
[0023] (1) Preparation of 900 nm FeO4 nanoparticles
[0024] Ferroferric oxide nanoparticles were synthesized by hydrothermal method. 1.89g ferric chloride hexahydrate, 0.875g PEG2000 and 2.52g anhydrous sodium acetate were dissolved in 35ml ethylene glycol respectively and stirred magnetically overnight. The Teflon containing the mixed solution was placed in a high pressure reactor and reacted in a muffle furnace at 200℃ for 12h. Finally, ethanol and water were circulated and washed in a centrifuge (9000rpm; 2min) until clean.
[0025] (2) Preparation of FeO-coated SiO2 nanoparticles
[0026] Ferroferric oxide coated silica nanoparticles were synthesized by a simple emulsion method. 0.1 g of ferroferric oxide nanoparticles were pretreated with a 1M hydrochloric acid solution to remove the oxide layer on the surface. Added to a mixed solvent system of 80 ml ethanol, 20 ml distilled water and 1 ml ammonia water, stirred at 500 rpm for 30 min at room temperature. Then 1 ml of tetraethyl orthosilicate was added dropwise, and stirring was continued at 800 rpm for 12 h. After the reaction was completed, ethanol and water were circulated and washed in a centrifuge (9000 rpm; 2 min) until clean.
[0027] (3) Amino modification of FeO-coated silica nanoparticles
[0028] Ferroferric oxide coated silica nanoparticles were synthesized by a simple emulsion method. 0.1 g of ferroferric oxide nanoparticles were pretreated with a 1M hydrochloric acid solution to remove the oxide layer on the surface. Added to a mixed solvent system of 80 ml ethanol, 20 ml distilled water and 1 ml ammonia water, stirred at 500 rpm for 30 min at room temperature. Then 800 μl of tetraethyl orthosilicate and 200 μl of 3-aminopropyltriethoxysilane were added dropwise, and stirring was continued at 800 rpm for 12 h. After the reaction was completed, ethanol and water were used to circulate and wash in a centrifuge (9000 rpm; 2 min) until clean.
[0029] Example 2
[0030] (1) Preparation of 400 nm FeO4 nanoparticles
[0031] Ferroferric oxide nanoparticles were synthesized by hydrothermal method. 0.945g ferric chloride hexahydrate, 0.875g PEG2000 and 2.52g anhydrous sodium acetate were dissolved in 35ml ethylene glycol respectively and stirred magnetically overnight. The Teflon containing the mixed solution was placed in a high pressure reactor and reacted in a muffle furnace at 200℃ for 8h. Finally, ethanol and water were circulated and washed in a centrifuge (9000rpm; 2min) until clean.
Claims
1. A general synthesis method for preparing monodisperse magnetic beads with controllable particle size based on solvothermal method.
2. The monodisperse magnetic beads with controllable particle size as claimed in claim 1, characterized in that The particle size of the synthesized magnetic beads can be controlled between 100-1000nm.
3. The monodisperse magnetic beads with controllable particle size as claimed in claim 1, characterized in that The synthesized magnetic beads exhibit superparamagnetic properties.
4. The monodisperse silica-coated magnetic beads with controllable particle size as claimed in claim 1, characterized in that The surface of the magnetic beads is covered with a smooth silicon dioxide layer with a thickness greater than 50-200nm.
5. The monodisperse silica-coated magnetic beads with controllable particle size as claimed in claim 1, characterized in that The dispersibility in polar solvents (such as water, ethanol, etc.) is better, and the dispersibility in non-polar solvents (such as n-hexane, acetone, etc.) is poor.
6. The general synthesis method as claimed in claim 1, characterized in that The technical means adopted is solvent thermal synthesis, which is convenient for large-scale preparation.
7. The synthesis method according to claim 1, characterized in that The selection and control of the reactant concentration, reaction time and acid-base environment are very important for preparing monodisperse silica-coated magnetic beads with controllable particle size. The reactant concentration and reaction time are conducive to controlling the particle size of the magnetic beads. The alkaline reaction environment includes ammonia water, triethanolamine, triethylamine and sodium hydroxide, which is conducive to the coating of the silicon layer of the magnetic beads.
8. The synthesis method according to claim 1, characterized in that The parameters involved include a reaction temperature of 150-250 degrees Celsius for synthesizing magnetic beads with controllable particle size, and a reaction time of 6-24 hours for synthesizing magnetic beads with controllable particle size.
9. The monodisperse magnetic beads with controllable particle size according to claim 1, characterized in that The magnetic saturation intensity of the magnetic beads ranges from 30-100emu g -1 .