CN109559888A - Fe3O4@SiO2The preparation method of composite Nano magnetic bead - Google Patents
Fe3O4@SiO2The preparation method of composite Nano magnetic bead Download PDFInfo
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- CN109559888A CN109559888A CN201811584527.8A CN201811584527A CN109559888A CN 109559888 A CN109559888 A CN 109559888A CN 201811584527 A CN201811584527 A CN 201811584527A CN 109559888 A CN109559888 A CN 109559888A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/32—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying conductive, insulating or magnetic material on a magnetic film, specially adapted for a thin magnetic film
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
- C12N15/00—Mutation or genetic engineering; DNA or RNA concerning genetic engineering, vectors, e.g. plasmids, or their isolation, preparation or purification; Use of hosts therefor
- C12N15/09—Recombinant DNA-technology
- C12N15/10—Processes for the isolation, preparation or purification of DNA or RNA
- C12N15/1003—Extracting or separating nucleic acids from biological samples, e.g. pure separation or isolation methods; Conditions, buffers or apparatuses therefor
- C12N15/1006—Extracting or separating nucleic acids from biological samples, e.g. pure separation or isolation methods; Conditions, buffers or apparatuses therefor by means of a solid support carrier, e.g. particles, polymers
- C12N15/1013—Extracting or separating nucleic acids from biological samples, e.g. pure separation or isolation methods; Conditions, buffers or apparatuses therefor by means of a solid support carrier, e.g. particles, polymers by using magnetic beads
Abstract
The invention discloses a kind of Fe for biological sample DNA separating-purifying3O4@SiO2The preparation method of composite Nano magnetic bead.Fe is prepared by solvent-thermal method3O4Nano particle usesMethod wraps up SiO2, prepare Fe3O4@SiO2Composite Nano magnetic bead, to be applied to the separating-purifying of DNA.The different-grain diameter ferromagnetism Fe being prepared with solvent-thermal method3O4Nano particle is core, is scattered in alkaline ethanol aqueous solution after purification, and ethyl polysilicate -40 (TEOS-40) then is added into solution, and by controlling the additional amount of TEOS-40, SiO is prepared2The adjustable composite magnetic nano particle of thickness can carry out the separating-purifying of the DNA of whole blood, saliva, rat-tail genome and virus using the NEW TYPE OF COMPOSITE magnetic bead of synthesis.
Description
Technical field
The invention belongs to field of nanocomposite materials, and in particular to be a kind of for biological sample DNA separating-purifying
Fe3O4@SiO2The preparation method of composite Nano magnetic bead.
Background technique
With gene diagnosis, GM food detection, the fast development of personalized medicine, the extraction of DNA is had become and is made a living
The basis of the fields clinical practice research such as object medicine and farming, forestry, husbandary and fishing.Paramagnetic particle method nucleic acid extraction has traditional DNA extraction method can not
The advantage of analogy, is mainly reflected in: 1. can be realized automation, high-volume operates;2. it is easy to operate, the used time is short, extract process
Step is few;3. it is safe and non-toxic, without using toxic reagents such as benzene, chloroforms in conventional method;4. the nucleic acid purity extracted is high, concentration
Greatly.The key factor of paramagnetic particle method nucleic acid extraction is nanometer magnetic bead, therefore develops nanometer magnetic bead of good performance with important reality
With value.Fe3O4The features such as because its biological safety is good, preparation method is simple, can be easily separated under external magnetic field is biology and doctor
Common magnetic material, and the common magnetic particle of nucleic acid extraction at present.The Fe that solvent structure goes out3O4Nanoparticle
Its performance is better than other prior synthesizing methods, has many advantages, such as that product particle size is distributed uniform, good dispersion, strong magnetic responsiveness
(H.Deng,X.L.Li,Q. Peng,et.al.,Angew.Chem.Int.Ed.2005,44,2782–2785).Magnetic nano particle
Son is inclined to due to specific surface energy with higher and dipolar magnetic interaction with strong aggregation, is difficult to keep stable state.
Therefore it needs to carry out particle surface modification and forms magnetic compound particles to improve the dispersibility of particle, protect exposed magnetic particles
Son.There is silica good physical and chemical stability and biocompatibility, surface easily to modify, and can apply to a variety of different
In environment, there is good adsorbing separation ability to DNA, be current ideal capsulating material.At present in Fe3O4Upper package
SiO2Prepare Fe3O4/SiO2The most common method of nanoscale magnetic bead isMethod (W.A.Fink,E.Bohn,
Et.al., J.Colloid Interface Sci., 1968,26,62-69), by Fe3O4Nanoparticle surface hydrolysis is organic
Siloxanes makes SiO2It is coated on magnetic particle, obtains the magnetic composite particle of functionalization.SiO is generated currently used for dissociation2's
Organosiloxane is ethyl orthosilicate (dioxide-containing silica 28%), and the magnetic microsphere of preparation often has dispersibility not enough reason
Think, partial size it is uneven, shape not enough rule, the problems such as reproducibility is bad.
Summary of the invention
In view of this, the invention is directed to a kind of new Fe3O4@SiO2The preparation method of composite Nano magnetic bead, with
The more efficient synthesis of lower cost can efficiently separate the nanometer magnetic bead of purification DNA.
In order to achieve the above objectives, the technical solution of the invention is achieved in that
A kind of Fe3O4@SiO2The preparation method of composite Nano magnetic bead, it is characterised in that: the preparation method is with solvent heat
The ferroferric oxide nano granules of method preparation are core, are passed throughMethod wraps up SiO2The Fe is made3O4@SiO2Composite Nano
Magnetic bead, wherein the SiO2Silicon source be ethyl polysilicate -40.
Further, the Fe3O4@SiO2The preparation method of composite Nano magnetic bead the following steps are included:
(1)Fe3O4The preparation of nano particle: ferric chloride hexahydrate is dissolved in ethylene glycol, and Sodium acetate trihydrate is then added
And Polyethylene glycol-2000, mixture stir 90min, are added in the stainless steel cauldron of polytetrafluoroethyllining lining and seal, 185
6~72h is reacted at~200 DEG C, reaction solution, products therefrom centrifuge separation is poured out after cooling, and wash 3 with ethyl alcohol and deionized water
~4 times, it is drying to obtain the Fe3O4Nano particle is spare;
(2)Fe3O4@SiO2The preparation of composite Nano magnetic bead: nano particle obtained in step (1) is added to ethyl alcohol, is gone
In the mixed-alkali solution of ionized water and ammonium hydroxide, citric acid is added, ethyl polysilicate -40 is added dropwise in mechanical stirring, stirs
12h is reacted, Magneto separate obtains the magnetic ball for being coated with silicon layer, washed to neutrality with deionized water and dehydrated alcohol to get described
Fe3O4@SiO2Composite Nano magnetic bead.
Further, the material compactedness in step (1) is 92-96%.
Further, the mass ratio of ferric chloride hexahydrate, Sodium acetate trihydrate and Polyethylene glycol-2000 is 1 in step (1):
(2~3): (0.5~1).
Further, ethyl alcohol in step (2): deionized water: the volume ratio of ammonium hydroxide is (3~4): 4:(1~1.2), every 1
It rises in mixed solution and Fe is added3O4The quality of nano particle is between 20-30 grams.
Further, ethyl polysilicate -40, citric acid and Fe in step (2)3O4The mass ratio of nano particle be (2.5~
3.2): 1:(7~10), the silicon dioxide layer thickness of the change adjustable magnetic ball surface of the additional amount of ethyl polysilicate -40.
Further, the nanometer Fe that the reaction time in step (1) and temperature can control3O4The partial size of particle, grain
Diameter range is 160-600nm.
Compared with the existing technology, Fe of the present invention3O4@SiO2The preparation method of composite Nano magnetic bead has following excellent
Gesture:
(1) preparation method of the present invention is preparing different-grain diameter Fe3O4The nanosphere stage increases by adjusting formula
Add the water content (using the inorganic salts containing the crystallization water) in system, improves compactedness, added with approaching the temperature of mixed system boiling point
Heat improves safety when yield reduces costs and improves production;In package SiO2Stage uses ethyl polysilicate-
40 be the new formulation of core material, nanometer magnetic bead separating-purifying DNA effect can be improved, and greatly reduce production cost;
(2) silicon source primary raw material of the present invention is ethyl polysilicate -40, is different from ethyl orthosilicate, in ethyl polysilicate -40
Dioxide-containing silica is higher than ethyl orthosilicate by 66.7%, and the dosage of corresponding various raw materials is all accordingly reduced, and can reduce the cost, and subtract
The discharge of few waste, environmental pollution is smaller, meets environmentally protective requirement;
(3) Fe is prepared using the present invention3O4@SiO2Composite Nano magnetic bead, batch internal difference of magnetic composite microsphere carrier and
Difference between batch is reproducible all within 5%, can averagely be extracted greater than 40 by automating every milliliter of new blood of purification system
The genomic DNA of μ g, DNA does not degrade in the uniform band that becomes clear in electrophoresis, and chemical stability is high, has better DNA
Separating-purifying effect.
Detailed description of the invention
Fig. 1 is Fe obtained by embodiment 13O4@SiO2Composite Nano magnetic bead grain size distribution;
Fig. 2 is Fe obtained by embodiment 23O4@SiO2Composite Nano magnetic bead grain size distribution;
Fig. 3 is Whole Blood Genomic DNA electrophoretogram;
The ultraviolet spectrogram that 1 gained nanometer magnetic bead of embodiment extracts DNA is added by saliva sample by Fig. 4;
The ultraviolet spectrogram that 2 gained nanometer magnetic bead of embodiment extracts DNA is added by whole blood sample by Fig. 5;
Fig. 6 is rat-tail genome dna electrophoresis figure;
Fig. 7 is 1 gained nanometer magnetic bead shape appearance figure of embodiment.
Specific embodiment
In addition to being defined, technical term used in following embodiment has and the invention one of ordinary skill in the art
The identical meanings being commonly understood by.Test reagent used in following embodiment is unless otherwise specified conventional biochemical reagent;
The experimental method is unless otherwise specified conventional method.
Below with reference to examples and drawings come the present invention will be described in detail create.
Embodiment 1
A kind of Fe3O4@SiO2The preparation method of composite Nano magnetic bead, comprising the following steps:
(1) ferric chloride hexahydrate 27g is dissolved in 800mL ethylene glycol, it is poly- that anhydrous sodium acetate 72g and 20g is then added
Ethylene glycol -2000, mixture stir 90min, are added in stainless steel cauldron and seal, react 9h in 200 DEG C;It is poured out after cooling
Reaction solution, products therefrom centrifuge separation, and washed 3-4 times with dehydrated alcohol and deionized water, it is drying to obtain the Fe3O4Nanometer
Particle is spare;
(2) Fe being prepared is taken3O4Nano particle 100g is added in the three-necked bottle of 10L, sequentially adds dehydrated alcohol, goes
Each 2L of ionized water, mechanical stirring;10g citric acid is added, -40 30mL of ethyl polysilicate, machine is slowly added dropwise in 500mL ammonium hydroxide
Tool stirs 12h;Magneto separate obtains the magnetic ball for being coated with silicon layer, is washed to neutrality with deionized water and dehydrated alcohol to get ruler is arrived
The very little Fe in 300nm or so3O4@SiO2Composite Nano magnetic bead obtains product 3.
Embodiment 2
A kind of Fe3O4@SiO2The preparation method of composite Nano magnetic bead, comprising the following steps:
(1) ferric chloride hexahydrate 36g is dissolved in 800mL ethylene glycol, it is poly- that anhydrous sodium acetate 100g and 20g is then added
Ethylene glycol -2000, mixture stir 90min, are added in polytetrafluoroethylcontainer container and seal, react 36h in 195 DEG C;After cooling
Reaction solution, products therefrom centrifuge separation are poured out, and is washed 3-4 times with dehydrated alcohol and deionized water, the Fe is drying to obtain3O4
Nano particle is spare;
(2) Fe being prepared is taken3O4Nano particle 100g is added in the three-necked bottle of 10L, sequentially adds dehydrated alcohol, goes
Each 2L of ionized water, mechanical stirring;8.3g citric acid is added, -40 25mL of ethyl polysilicate, machine is slowly added dropwise in 500mL ammonium hydroxide
Tool stirs 12h;Magneto separate obtains the magnetic ball for being coated with silicon layer, is washed to neutrality with deionized water and dehydrated alcohol to get ruler is arrived
The very little Fe in 500nm or so3O4@SiO2Composite Nano magnetic bead obtains product 4.
Comparative example 1
A kind of Fe3O4@SiO2The preparation method of composite Nano magnetic bead, comprising the following steps:
(1) ferric chloride hexahydrate 27g is dissolved in 800mL ethylene glycol, it is poly- that anhydrous sodium acetate 72g and 20g is then added
Ethylene glycol -2000, mixture stir 90min, are added in stainless steel cauldron and seal, react 9h in 200 DEG C;It is poured out after cooling
Reaction solution, products therefrom centrifuge separation, and washed 3-4 times with dehydrated alcohol and deionized water, it is drying to obtain the Fe3O4Nanometer
Particle is spare;
(2) Fe being prepared is taken3O4Nano particle 100g is added in the three-necked bottle of 10L, sequentially adds dehydrated alcohol, goes
Each 2L of ionized water, mechanical stirring;10g citric acid is added, ethyl orthosilicate 30mL is slowly added dropwise in 500mL ammonium hydroxide, and machinery stirs
Mix 12h;Magneto separate obtains the magnetic ball for being coated with silicon layer, is washed with deionized water and dehydrated alcohol to neutrality and is existed to get to size
The Fe of 300nm or so3O4@SiO2Composite Nano magnetic bead obtains product 1.
Comparative example 2
A kind of Fe3O4@SiO2The preparation method of composite Nano magnetic bead, comprising the following steps:
(1) ferric chloride hexahydrate 27g is dissolved in 800mL ethylene glycol, it is poly- that anhydrous sodium acetate 72g and 20g is then added
Ethylene glycol -2000, mixture stir 90min, are added in stainless steel cauldron and seal, react 9h in 200 DEG C;It is poured out after cooling
Reaction solution, products therefrom centrifuge separation, and washed 3-4 times with dehydrated alcohol and deionized water, it is drying to obtain the Fe3O4Nanometer
Particle is spare;
(2) Fe being prepared is taken3O4Nano particle 100g is added in the three-necked bottle of 10L, sequentially adds dehydrated alcohol, goes
Each 2L of ionized water, mechanical stirring;500mL ammonium hydroxide is added, -40 30mL of ethyl polysilicate, mechanical stirring 12h is slowly added dropwise;Magnetic
The isolated magnetic ball for being coated with silicon layer is washed to neutrality with deionized water and dehydrated alcohol to get size is arrived in 300nm or so
Fe3O4@SiO2Composite Nano magnetic bead obtains product 2.
Experiment: WG is the best product of presently commercially available effect (for degree biology, MA0309C magnetic microsphere).
Partial size test:
For product 3 and product 4,1mg Fe is taken respectively3O4@SiO2It is scattered in the distilled water of 2mL, ultrasonic disperse, then
Particle diameter distribution is measured with Nano ZS90 partial size tester.Test result shows uniform particle sizes, and it is compound that Fig. 1 shows that product 3 obtains
Nanoscale magnetic bead particle diameter distribution is 250-400nm;The composite Nano magnetic spherolite diameter that Fig. 2 shows that product 4 obtains is distributed as 400-
600nm。
Electrophoresis experiment:
The Ago-Gel for preparing 1% carries out electrophoresis experiment.
Embodiment 1, embodiment 2, comparative example 1, the product of comparative example 2 and WG is selected to carry out electrophoresis experiment.
(1) it weighs 0.7g agarose to be put in conical flask, then measures 1 × TAE solution mixing of 70mL, be put in micro-wave oven
It boils, until solution is transparent.
(2) gel maker is assembled, and is adjusted to level.Glue is fallen in gel maker, comb is plugged.It is cooling to 40 minutes glue
After solidification, so that it may be put in the electrophoresis tank of electrophoretic buffer and carry out point sample.
(3) the 5 μ L of sample solution with bromophenol blue is taken to carry out point sample.The Marker of every one 5 μ L of row's loading wells main points.
(4) after having put, each parameter of electrophoresis apparatus is adjusted to carry out electrophoresis.
(5) after electrophoresis, gel is taken out, dyeing 20min is carried out with the buffer dye liquor containing EB, in buffer solution for cleaning.
(6) it finally observes in the UV lamp.Using the DNA of this patent product purification in the uniform band that becomes clear, show
Good DNA separating-purifying effect.And change the DNA that this patent is formulated synthesized product purification, band brightness obviously weakens,
Its DNA separating-purifying effect illustrates that changing formula has very big shadow to the DNA refining effect of composite Nano magnetic ball much worse than the former
It rings.
As shown in figure 3, its purity of DNA and yield purified using this patent product 3 and product 4 is omited for whole blood sample
Better than the best product of presently commercially available effect.
As shown in fig. 6, for rat-tail sample, DNA its purity purified using this patent product 3 and product 4 is substantially better than
The presently commercially available best product of effect (compare set product 1 and product 2 have obvious trailing phenomenon).
Ultraviolet spectroscopy
Select the product of embodiment 1
100 μ L of purification gained DNA solution sample sweeps ultra-violet (UV) band wavelength, and OD260/280 ratio illustrates purity 1.8 or so
Up to standard, absorption peak strength is directly proportional to DNA concentration.According to formula: DNA concentration (ng/ μ L)=OD260 × 50ng/ μ L can be counted
DNA product design is calculated, 200 μ L saliva samples can purify 64.7ng/ μ L DNA sample (Fig. 4);
Select the product of embodiment 2
100 μ L of purification gained DNA solution sample sweeps ultra-violet (UV) band wavelength, and OD260/280 ratio illustrates purity 1.8 or so
Up to standard, absorption peak strength is directly proportional to DNA concentration.According to formula: DNA concentration (ng/ μ L)=OD260 × 50ng/ μ L can be counted
DNA product design is calculated, 120 μ L whole blood samples can purify 172.0ng/ μ L DNA sample (Fig. 5).
Fig. 7 is nanometer magnetic bead shape appearance figure obtained by the product of embodiment 1.The nanometer magnetic bead prepared using this patent formula,
With good stability and dispersed, ultrasound or (can be greater than 2 minutes) whithin a period of time after shaking up suspends in the solution, point
Cloth is uniform, and sinking speed is slow.Magnetic responsiveness is strong, under externally-applied magnetic field can rapid aggregation, convenient for the separating-purifying to DNA.
The foregoing is merely the preferred embodiments of the invention, are not intended to limit the invention creation, all at this
Within the spirit and principle of innovation and creation, any modification, equivalent replacement, improvement and so on should be included in the invention
Protection scope within.
Claims (7)
1. a kind of Fe3O4@SiO2The preparation method of composite Nano magnetic bead, it is characterised in that: the preparation method is with solvent-thermal method
The ferroferric oxide nano granules of preparation are core, are passed throughMethod wraps up SiO2The Fe is made3O4@SiO2Composite Nano magnetic
Pearl, wherein the SiO2Silicon source be ethyl polysilicate -40.
2. Fe according to claim 13O4@SiO2The preparation method of composite Nano magnetic bead, it is characterised in that: including following
Step:
(1)Fe3O4The preparation of nano particle: ferric chloride hexahydrate is dissolved in ethylene glycol, and Sodium acetate trihydrate is then added and gathers
Ethylene glycol -2000, mixture stir 90min, are added in the stainless steel cauldron of polytetrafluoroethyllining lining and seal, 185~200
6~72h is reacted at DEG C, reaction solution, products therefrom centrifuge separation is poured out after cooling, and wash 3~4 with ethyl alcohol and deionized water
It is secondary, it is drying to obtain the Fe3O4Nano particle is spare;
(2)Fe3O4@SiO2The preparation of composite Nano magnetic bead: nano particle obtained in step (1) is added to ethyl alcohol, deionization
In the mixed-alkali solution of water and ammonium hydroxide, citric acid is added, ethyl polysilicate -40 is added dropwise in mechanical stirring, is stirred to react
12h, Magneto separate obtain the magnetic ball for being coated with silicon layer, are washed to neutrality with deionized water and dehydrated alcohol to get the Fe3O4@
SiO2Composite Nano magnetic bead.
3. Fe according to claim 23O4@SiO2The preparation method of composite Nano magnetic bead, it is characterised in that: in step (1)
Material compactedness be 92-96%.
4. Fe according to claim 23O4@SiO2The preparation method of composite Nano magnetic bead, it is characterised in that: in step (1)
The mass ratio of ferric chloride hexahydrate, Sodium acetate trihydrate and Polyethylene glycol-2000 is 1:(2~3): (0.5~1).
5. Fe as claimed in claim 23O4@SiO2The preparation method of composite Nano magnetic bead, it is characterised in that: second in step (2)
Alcohol: deionized water: the volume ratio of ammonium hydroxide is (3~4): 4:(1~1.2), Fe is added in every 1 liter of mixed solution3O4Nano particle
Quality is between 20-30 grams.
6. Fe according to claim 23O4@SiO2The preparation method of composite Nano magnetic bead, it is characterised in that: in step (2)
Ethyl polysilicate -40, citric acid and Fe3O4The mass ratio of nano particle is (2.5~3.2): 1:(7~10).
7. Fe according to claim 23O4@SiO2The preparation method of composite Nano magnetic bead, it is characterised in that: in step (1)
Reaction time and the nanometer Fe that can control of temperature3O4The partial size of particle, particle size range are 160-600nm.
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Cited By (3)
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CN112007605A (en) * | 2019-05-30 | 2020-12-01 | 苏州海狸生物医学工程有限公司 | Hydroxyl nano magnetic bead for nucleic acid extraction and preparation method thereof |
CN115254067A (en) * | 2022-09-29 | 2022-11-01 | 山东博科科学仪器有限公司 | Silicon hydroxyl magnetic bead and synthetic method and application thereof |
CN117550650A (en) * | 2023-11-21 | 2024-02-13 | 无锡国盛生物工程股份有限公司 | SiO (silicon dioxide) 2 Wrapping magnetic Fe 3 O 4 Method for preparing nano particles |
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