CN117624512A - Magnetic microsphere and preparation method thereof - Google Patents
Magnetic microsphere and preparation method thereof Download PDFInfo
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- CN117624512A CN117624512A CN202311521185.6A CN202311521185A CN117624512A CN 117624512 A CN117624512 A CN 117624512A CN 202311521185 A CN202311521185 A CN 202311521185A CN 117624512 A CN117624512 A CN 117624512A
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- 239000004005 microsphere Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000006249 magnetic particle Substances 0.000 claims abstract description 45
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 17
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 16
- 239000000839 emulsion Substances 0.000 claims abstract description 15
- 238000006772 olefination reaction Methods 0.000 claims abstract description 15
- -1 acrylic glycol ester compound Chemical class 0.000 claims abstract description 12
- 150000001875 compounds Chemical class 0.000 claims abstract description 10
- 239000006185 dispersion Substances 0.000 claims abstract description 10
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 239000003945 anionic surfactant Substances 0.000 claims abstract description 7
- 239000003999 initiator Substances 0.000 claims abstract description 7
- 238000001556 precipitation Methods 0.000 claims abstract description 5
- 150000001298 alcohols Chemical class 0.000 claims abstract description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 230000003647 oxidation Effects 0.000 claims abstract description 3
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 17
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 16
- 108020004707 nucleic acids Proteins 0.000 claims description 15
- 150000007523 nucleic acids Chemical class 0.000 claims description 15
- 102000039446 nucleic acids Human genes 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 238000000605 extraction Methods 0.000 claims description 9
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 9
- 235000010333 potassium nitrate Nutrition 0.000 claims description 8
- 239000004323 potassium nitrate Substances 0.000 claims description 8
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical group O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 6
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 229960002089 ferrous chloride Drugs 0.000 claims description 4
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 4
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 3
- 239000011790 ferrous sulphate Substances 0.000 claims description 3
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 3
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 2
- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical compound [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- XZTJQQLJJCXOLP-UHFFFAOYSA-M sodium;decyl sulfate Chemical compound [Na+].CCCCCCCCCCOS([O-])(=O)=O XZTJQQLJJCXOLP-UHFFFAOYSA-M 0.000 claims description 2
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims description 2
- PNGBYKXZVCIZRN-UHFFFAOYSA-M sodium;hexadecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCCCCCS([O-])(=O)=O PNGBYKXZVCIZRN-UHFFFAOYSA-M 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000010419 fine particle Substances 0.000 claims 1
- 229910000859 α-Fe Inorganic materials 0.000 claims 1
- 230000003749 cleanliness Effects 0.000 abstract description 2
- 230000004044 response Effects 0.000 abstract description 2
- 239000008367 deionised water Substances 0.000 description 11
- 229910021641 deionized water Inorganic materials 0.000 description 11
- 238000001514 detection method Methods 0.000 description 10
- 238000005406 washing Methods 0.000 description 10
- 238000001816 cooling Methods 0.000 description 8
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- KUDUQBURMYMBIJ-UHFFFAOYSA-N 2-prop-2-enoyloxyethyl prop-2-enoate Chemical compound C=CC(=O)OCCOC(=O)C=C KUDUQBURMYMBIJ-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 230000001804 emulsifying effect Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 241000700605 Viruses Species 0.000 description 3
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- 238000009210 therapy by ultrasound Methods 0.000 description 3
- LEJBBGNFPAFPKQ-UHFFFAOYSA-N 2-(2-prop-2-enoyloxyethoxy)ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOCCOC(=O)C=C LEJBBGNFPAFPKQ-UHFFFAOYSA-N 0.000 description 2
- 241000711549 Hepacivirus C Species 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- 241000700627 Monkeypox virus Species 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000007400 DNA extraction Methods 0.000 description 1
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 1
- 206010020843 Hyperthermia Diseases 0.000 description 1
- 238000010802 RNA extraction kit Methods 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
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- 238000005859 coupling reaction Methods 0.000 description 1
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- 241001493065 dsRNA viruses Species 0.000 description 1
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- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
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- 230000008676 import Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
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- 239000012266 salt solution Substances 0.000 description 1
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- 229910052710 silicon Inorganic materials 0.000 description 1
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Landscapes
- Soft Magnetic Materials (AREA)
Abstract
The invention discloses a magnetic microsphere and a preparation method thereof. The method comprises the following steps: preparing ferroferric oxide magnetic particles by an oxidation precipitation method; reacting the ferroferric oxide magnetic particles with methacryloxypropyl trimethoxysilane in a mixed solution of alcohols and water to obtain olefination ferroferric oxide magnetic particles; dispersing olefination ferroferric oxide magnetic particles in the emulsion to obtain a dispersion system; the components of the emulsion comprise methacrylic acid, acrylic monoester compound, acrylic glycol ester compound, water-soluble initiator, water-soluble anionic surfactant and water; and (3) carrying out polymerization reaction on the dispersion system to obtain the magnetic microsphere. The magnetic particles prepared by the method have the advantages of good cleanliness, high stability, strong magnetic response, uniform particle size and good dispersibility, and are suitable for large-scale operation.
Description
Technical Field
The invention relates to the technical field of magnetic materials, in particular to a magnetic microsphere and a preparation method thereof.
Background
Magnetic particles (e.g. Fe 3 O 4 Nanoparticles) have the characteristics of the nano material, such as small particle size, large specific surface, high coupling capacity and the like, have magnetic responsiveness and superparamagnetism, can be gathered and positioned under a constant magnetic field, and can absorb electromagnetic waves to generate heat under an alternating magnetic field. In addition, the magnetic particles can also be provided with a plurality of active functional groups (such as-OH, -COOH, -NH) by surface modification 2 Etc.). Therefore, the magnetic particles have wide application prospects in the biological medicine fields such as biological separation, drug release, hyperthermia treatment and the like.
In the prior art, the preparation process of the magnetic microsphere is complex, most of raw materials depend on import, and the price is high. How to simplify the preparation process of magnetic particles and ensure the stability, the dispersibility and the magnetic saturation of the magnetic particles is a problem to be solved at present.
Disclosure of Invention
The invention provides a magnetic microsphere and a preparation method thereof.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
in one aspect, the invention provides a method for preparing magnetic microspheres, comprising the following steps:
s1: preparing ferroferric oxide magnetic particles by an oxidation precipitation method;
s2: reacting the ferroferric oxide magnetic particles obtained in the step S1 with methacryloxypropyl trimethoxy silane in a mixed solution of alcohols and water to obtain olefination ferroferric oxide magnetic particles;
s3: dispersing the olefination ferroferric oxide magnetic particles prepared in the step S2 in emulsion to obtain a dispersion system; the components of the emulsion comprise methacrylic acid, acrylic monoester compounds, acrylic glycol ester compounds, water-soluble initiator, water-soluble anionic surfactant and water;
s4: and (3) carrying out polymerization reaction on the dispersion system obtained in the step (S3) to obtain the magnetic microsphere.
In a preferred embodiment, in step S1, the oxidative precipitation method comprises the steps of: ferrous salt, sodium hydroxide and potassium nitrate are heated in aqueous solution for reaction;
preferably, the ferrous salt is selected from at least one of ferrous sulfate, ferrous ammonium sulfate and ferrous chloride;
preferably, in the heating reaction, the ferrous salt is used in an amount of 10 to 60g based on 100g of water; the dosage of the sodium hydroxide is 5-8 g, and the dosage of the potassium nitrate is 30-80 g;
preferably, the reaction temperature of the heating reaction is 60-100 ℃ and the reaction time is 2-24 hours.
In certain specific embodiments, step S1 further comprises a post-treatment operation, said post-treatment comprising washing.
In certain embodiments, step S1 specifically comprises the steps of: dispersing sodium hydroxide and potassium nitrate in water, stirring and heating to 60-100 ℃ under nitrogen atmosphere, and rapidly adding ferrous salt solution and reacting for 2-24 hours; and (3) washing with deionized water and absolute ethyl alcohol after cooling to obtain the ferroferric oxide magnetic particles.
In a preferred embodiment, in the step S2, the mass of the methacryloxypropyl trimethoxysilane is 2 to 6 times that of the ferroferric oxide particles;
preferably, the mixed solution of the alcohol and the water is ethanol water solution with the mass fraction of 5-20%;
preferably, the temperature of the reaction is 50-80 ℃ and the reaction time is 8-24 hours.
In certain specific embodiments, step S2 further comprises a post-processing operation; the post-treatment includes washing and vacuum drying.
In certain embodiments, step S2 specifically comprises the steps of: dispersing ferroferric oxide magnetic particles in ethanol water solution containing methacryloxypropyl trimethoxy silane, heating to 50-80 ℃ for reaction for 8-24 hours, cooling, and washing with deionized water for 3-6 times; and then drying for 2-3 hours in a vacuum environment at 40-60 ℃ to obtain the olefination ferroferric oxide magnetic particles.
As a preferred embodiment, in step S3, the mass concentration of the methacrylic acid is 0.1 to 3wt%, the mass concentration of the acrylic acid monoester compound is 3 to 15wt%, the mass concentration of the acrylic acid diol ester compound is 0.1 to 3wt%, the mass of the water-soluble initiator is 0.3 to 3% of the total mass of the methacrylic acid, the acrylic acid monoester compound, the acrylic acid diol ester compound and the water, and the mass of the water-soluble anionic surfactant is 0.1 to 2% of the total mass of the methacrylic acid, the acrylic acid monoester compound, the acrylic acid diol ester compound and the water;
preferably, the water-soluble initiator is selected from at least one of sodium persulfate, potassium persulfate and amine persulfate;
preferably, the water-soluble anionic surfactant is selected from at least one of sodium dodecyl sulfate, sodium dodecyl sulfonate, sodium hexadecyl sulfonate, and sodium n-decyl sulfate;
in certain embodiments, the emulsion is emulsified with the mixed components using an emulsifying machine.
In a preferred embodiment, in step S3, the mass ratio of the olefinized ferroferric oxide magnetic particles to methacrylic acid is 1: (0.1 to 1);
preferably, the dispersing is performed under ultrasonic agitation; the ultrasonic stirring time is 1-3 hours.
In a preferred embodiment, in step S4, the temperature of the polymerization reaction is 65 to 75 ℃; the time of the polymerization reaction is 12-24 hours;
preferably, the polymerization is carried out under stirring.
In yet another aspect, the present invention provides the magnetic microsphere obtained by the above preparation method.
In yet another aspect, the present invention provides the use of the magnetic microsphere described above in the preparation of a nucleic acid extraction kit.
The technical scheme has the following advantages or beneficial effects:
according to the preparation method provided by the invention, the substrate of the magnetic microsphere is treated by a proper emulsion, and the surface modification of the substrate of the magnetic microsphere is realized by emulsion polymerization, so that the magnetic microsphere for biological separation is obtained. The magnetic microsphere prepared by the method has good dispersibility, is suitable for large-scale biological separation operation, and has simple and feasible separation process. In addition, the preparation method has the advantages of simple operation steps, no need of pre-coating a silicon layer in olefination modification, low-cost and easily obtained raw materials, mild conditions, short reaction time, high yield and great utilization value and economic significance.
According to the preparation method provided by the invention, the olefine ferroferric oxide magnetic particles are dispersed in the emulsion containing methacrylic acid, so that the olefine ferroferric oxide magnetic particles and the methacrylic acid are subjected to interface self-assembly, thereby forming composite particles, and the magnetic microsphere with high magnetic content is prepared. The method can realize the preparation of magnetic microspheres with various sizes, meet different application requirements and realize quick and efficient geomagnetic attraction separation.
The magnetic microsphere provided by the invention has the advantages of good cleanliness, high stability, uniform particle size, high crystallinity and excellent magnetic response, is beneficial to improving the batch-to-batch stability and high-efficiency magnetic enrichment of the magnetic microsphere, and has the excellent characteristics of high strength, high specific surface area, adjustable pore diameter and the like, so that the magnetic microsphere is widely applied to the fields of pretreatment of molecular detection samples and extraction and separation of organic matters.
Drawings
FIG. 1 is a transmission electron microscope image of the olefinic ferroferric oxide magnetic particles prepared in example II of the present invention;
FIG. 2 is a scanning electron microscope image of the magnetic microspheres prepared in the second embodiment of the present invention;
FIG. 3 is a particle size distribution diagram of magnetic microspheres prepared in example II of the present invention.
Detailed Description
The following examples are only some, but not all, of the examples of the invention. Accordingly, the detailed description of the embodiments of the invention provided below is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by a person skilled in the art without making any inventive effort, are intended to fall within the scope of the present invention.
In the present invention, all the equipment, raw materials and the like are commercially available or commonly used in the industry unless otherwise specified. The methods in the following examples are conventional in the art unless otherwise specified.
Example 1
The embodiment provides a magnetic microsphere, which is prepared by the following steps:
s1: synthesis of ferroferric oxide magnetic particles
6g of sodium hydroxide and 30.3g of potassium nitrate were dispersed in 80g of deionized water; stirring and heating to 80 ℃ under nitrogen atmosphere; 20mL of 0.5g/mL ferrous sulfate aqueous solution is added rapidly, and the reaction is carried out for 12 hours; after cooling, washing the obtained product with deionized water and absolute ethyl alcohol for 3 times respectively to obtain ferroferric oxide magnetic particles;
s2: olefination of magnetic particles;
dispersing 1.5g of the ferroferric oxide magnetic particles obtained in the step S1 in 100mL of ethanol water solution with the mass fraction of 10%, then adding 4.5g of methacryloxypropyl trimethoxysilane, uniformly mixing, and heating to 70 ℃ for reaction for 10 hours; washing with deionized water for 4 times after cooling, and then drying for 2 hours in a vacuum environment at 50 ℃ to obtain olefination ferroferric oxide magnetic particles;
s3: preparing emulsion;
0.29g of methacrylic acid, 4.3g of methyl acrylate, 0.34g of ethylene glycol diacrylate, 0.5g of sodium persulfate and 0.2g of sodium dodecyl sulfate are added into 95g of pure water, mixed and put into an emulsifying machine for emulsification;
s4: dispersing 1g of the olefination magnetic particles prepared in the step S2 in the emulsion prepared in the step S3, and carrying out ultrasonic treatment for 1 hour while stirring to obtain a dispersion system;
s5: and heating the mixed solution to 70 ℃, and stirring and reacting for 12 hours to obtain the magnetic microsphere with the particle size of 200nm, wherein the uniformity of the particle size is less than 5%.
Example two
The embodiment provides a magnetic microsphere, which is prepared by the following steps:
s1: synthesis of ferroferric oxide magnetic particles
6g of sodium hydroxide and 40.4g of potassium nitrate were dispersed in 80g of deionized water; stirring and heating to 80 ℃ under nitrogen atmosphere; 20mL of 1g/mL ferrous chloride aqueous solution is rapidly added for reaction for 18 hours; after cooling, washing 3 times by deionized water and absolute ethyl alcohol respectively to obtain ferroferric oxide magnetic particles;
s2: olefination of magnetic particles;
3g of ferroferric oxide magnetic particles obtained in the step S1 are dispersed in 150mL of ethanol water solution with the mass fraction of 10%, then 10.5g of methacryloxypropyl trimethoxysilane is added, and after uniform mixing, the temperature is raised to 70 ℃ for reaction for 12 hours; and (3) washing the mixture with deionized water for 4 times after cooling, and drying the mixture for 2 hours in a vacuum environment at 50 ℃ to obtain the olefination ferroferric oxide magnetic particles.
S3: preparing emulsion;
0.43g of methacrylic acid, 8.6g of ethyl methacrylate, 0.4g of ethylene glycol diacrylate, 0.75g of ammonium persulfate and 0.4g of sodium dodecyl sulfate are added into 90.5g of pure water, mixed and then put into an emulsifying machine for emulsification;
s4: dispersing 2g of the olefine magnetic particles prepared in the step S2 in the emulsion prepared in the step S3, and carrying out ultrasonic treatment for 1.5 hours while stirring to obtain a dispersion system;
s5: and heating the mixed solution to 70 ℃, and stirring and reacting for 16 hours to obtain the magnetic microsphere with the particle size of 500nm, wherein the uniformity of the particle size is less than 5%.
Example III
The embodiment provides a magnetic microsphere, which is prepared by the following steps:
s1: synthesis of ferroferric oxide magnetic particles
8g of sodium hydroxide and 75.8g of potassium nitrate were dispersed in 120g of deionized water; stirring and heating to 80 ℃ under nitrogen atmosphere; 30mL of 2g/mL ferrous chloride aqueous solution is added rapidly, and the reaction is carried out for 24 hours; after cooling, washing 3 times by deionized water and absolute ethyl alcohol respectively to obtain ferroferric oxide magnetic particles;
s2: olefination of magnetic particles;
dispersing 5g of ferroferric oxide magnetic particles obtained in the step S1 in 250mL of ethanol water solution with the mass fraction of 15%, then adding 20g of methacryloxypropyl trimethoxysilane, uniformly mixing, and heating to 70 ℃ for reaction for 16 hours; washing with deionized water for 4 times after cooling, and then drying for 2 hours in a vacuum environment at 50 ℃ to obtain olefination ferroferric oxide magnetic particles;
s3: preparing emulsion;
adding 0.86g of methacrylic acid, 10g of ethyl acrylate, 1.1g of diethylene glycol diacrylate, 1.5g of potassium persulfate and 1g of sodium dodecyl sulfate into 88g of pure water, mixing and then putting into an emulsifying machine for emulsification;
s4: dispersing 3g of the olefine magnetic particles prepared in the step S2 in the emulsion prepared in the step S3, and carrying out ultrasonic treatment for 2.5 hours while stirring to obtain a dispersion system;
s5: and heating the mixed solution to 70 ℃, and stirring and reacting for 24 hours to obtain the magnetic microsphere with the particle size of 800nm, wherein the uniformity of the particle size is less than 5%.
The morphology of the olefin-based ferroferric oxide magnetic particles prepared in the step S2 of the embodiment is characterized by a transmission electron microscope, wherein the transmission electron microscope diagram of the olefin-based ferroferric oxide magnetic particles prepared in the second embodiment is shown in the figure 1, and the morphology is regular, and the average grain diameter is 277.54 +/-13.87 nm.
The magnetic microsphere prepared in the embodiment is subjected to morphology characterization by a scanning electron microscope, wherein a scanning electron microscope image of the magnetic microsphere prepared in the embodiment II is shown in a figure 2, the surface of the magnetic microsphere is relatively smooth and is in a uniform sphere shape, and the average particle size of the magnetic microsphere is 503.06 +/-23.92 nm.
The magnetic microspheres prepared in the second embodiment are characterized in terms of hydrated particle size by a nano-particle size potentiometer, and as shown in fig. 3, the average hydrated particle size of the magnetic microspheres is 627.59nm, and the particle size distribution is relatively uniform.
The invention carries out relevant tests on the nucleic acid extraction detection performance of the magnetic microsphere prepared by the embodiment, and specifically comprises the following steps:
taking 1mg of the magnetic microsphere prepared in the embodiment, dispersing in 1mL of pure water solution to obtain 1mg/mL of magnetic bead dispersion; then, the equivalent magnetic microspheres are used for replacing the control magnetic microspheres in a commercial nucleic acid extraction kit (Bo-Japanese biological virus DNA/RNA extraction kit), target nucleic acid is extracted by a full-automatic nucleic acid extraction instrument, and finally, the nucleic acid extraction detection performance of the magnetic microspheres is evaluated on a fluorescent quantitative PCR instrument by using a commercial RNA virus (hepatitis C virus, HCV) nucleic acid detection kit (DAA gene hepatitis C virus nucleic acid quantitative detection kit) and a commercial DNA virus (monkey pox virus, MPXV) nucleic acid detection kit (DAA gene monkey pox virus nucleic acid detection kit), and the test results are shown in Table 1.
As can be seen from Table 1, the magnetic microspheres prepared in the invention all show smaller Ct values, i.e., have higher detection sensitivity and good nucleic acid universality, compared with the control magnetic microspheres in the commercial kit, wherein the magnetic microspheres prepared in the second embodiment have more excellent nucleic acid detection performance.
Comparative analysis of RNA/DNA Virus nucleic acid extraction detection Performance of magnetic microspheres prepared in Table 1 examples and control magnetic microspheres in commercial nucleic acid extraction kits
The foregoing is only a preferred embodiment of the invention, it being noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the invention.
Claims (10)
1. The preparation method of the magnetic microsphere is characterized by comprising the following steps:
s1: preparing ferroferric oxide magnetic particles by an oxidation precipitation method;
s2: reacting the ferroferric oxide magnetic particles obtained in the step S1 with methacryloxypropyl trimethoxy silane in a mixed solution of alcohols and water to obtain olefination ferroferric oxide magnetic particles;
s3: dispersing the olefination ferroferric oxide magnetic particles prepared in the step S2 in emulsion to obtain a dispersion system; the components of the emulsion comprise methacrylic acid, acrylic monoester compounds, acrylic glycol ester compounds, water-soluble initiator, water-soluble anionic surfactant and water;
s4: and (3) carrying out polymerization reaction on the dispersion system obtained in the step (S3) to obtain the magnetic microsphere.
2. The method according to claim 1, wherein in step S1, the oxidative precipitation method comprises the steps of: ferrous salt, sodium hydroxide and potassium nitrate are heated in aqueous solution for reaction;
preferably, the ferrous salt is selected from at least one of ferrous sulfate, ferrous ammonium sulfate and ferrous chloride.
3. The production method according to claim 2, wherein the amount of the ferrite is 10 to 60g based on 100g of water in the heating reaction; the dosage of the sodium hydroxide is 5-8 g, and the dosage of the potassium nitrate is 30-80 g.
4. The preparation method according to claim 2, wherein the reaction temperature of the heating reaction is 60 to 100 ℃ and the reaction time is 2 to 24 hours.
5. The method according to claim 1, wherein in step S2, the mass of the methacryloxypropyl trimethoxysilane is 2 to 6 times that of the ferroferric oxide particles;
preferably, the mixed solution of the alcohol and the water is ethanol water solution with the mass fraction of 5-20%;
preferably, the temperature of the reaction is 50-80 ℃ and the reaction time is 8-24 hours.
6. The production method according to claim 1, wherein in step S3, the mass concentration of the methacrylic acid is 0.1 to 3wt%, the mass concentration of the acrylic acid monoester compound is 3 to 15wt%, the mass concentration of the acrylic acid diol ester compound is 0.1 to 3wt%, the mass of the water-soluble initiator is 0.3 to 3% of the total mass of the methacrylic acid, the acrylic acid monoester compound, the acrylic acid diol ester compound and the water, and the mass of the water-soluble anionic surfactant is 0.1 to 2% of the total mass of the methacrylic acid, the acrylic acid monoester compound, the acrylic acid diol ester compound and the water, based on the total mass of the methacrylic acid, the acrylic acid monoester compound, the acrylic acid diol ester compound and the water;
preferably, the water-soluble initiator is selected from at least one of sodium persulfate, potassium persulfate and amine persulfate;
preferably, the water-soluble anionic surfactant is selected from at least one of sodium dodecyl sulfate, sodium dodecyl sulfonate, sodium hexadecyl sulfonate, and sodium n-decyl sulfate.
7. The method according to claim 1, wherein in step S3, the mass ratio of the olefinized ferroferric oxide fine particles to methacrylic acid is 1: (0.1 to 1);
preferably, the dispersing is performed under ultrasonic agitation; the ultrasonic stirring time is 1-3 hours.
8. The method according to claim 1, wherein in step S4, the polymerization reaction temperature is 65 to 75 ℃; the time of the polymerization reaction is 12-24 hours;
preferably, the polymerization is carried out under stirring.
9. A magnetic microsphere obtained by the method of any one of claims 1 to 8.
10. Use of the magnetic microsphere of claim 9 in the preparation of a nucleic acid extraction kit.
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