CN106501553B - A kind of ultralow field nanometer magnetic probe and the preparation method and application thereof - Google Patents
A kind of ultralow field nanometer magnetic probe and the preparation method and application thereof Download PDFInfo
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- G—PHYSICS
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- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
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- G01N33/543—Immunoassay; Biospecific binding assay; Materials therefor with an insoluble carrier for immobilising immunochemicals
- G01N33/54313—Immunoassay; Biospecific binding assay; Materials therefor with an insoluble carrier for immobilising immunochemicals the carrier being characterised by its particulate form
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Abstract
The invention belongs to field of nano biotechnology, and in particular to a kind of ultralow field nanometer magnetic probe and the preparation method and application thereof.Ultralow field magnetic probe is the ligand modified magnetic nano-particle of surface hydrophilicity.Magnetic nano-particle is the ferrimagnetic nanoparticle of ferrimagnetic nanoparticle or doping, wherein the dopant in the ferrimagnetic nanoparticle adulterated is at least one of zinc, cobalt and manganese.The hydrophilic ligand are as follows: the PEG of 3,4- dihydroxyphenyl propionic acid, 2,3- dimercaptosuccinic acid and double carboxyl modifieds.Ultralow field magnetic probe is following 1) -3) at least one of in application also belong to protection scope of the present invention: 1) cell magnetic imaging；2) Bacteria Detection；3) the magnetic immune reagent kit based on optics atom magnetometer is prepared.The present invention provide it is a kind of be simple and efficient, low cost no longer needs to assemble, being prepared on a large scale, monodispersity is good, bio-compatibility is good, the ultralow field magnetic probe of Nano grade that has excellent magnetic characteristics.Ultralow field magnetic probe prepared by the present invention has multiple application.
Description
Technical field
The invention belongs to field of nano biotechnology, and in particular to a kind of ultralow field nanometer magnetic probe and preparation method thereof with
Using.
Background technique
Ultralow field optics atom magnetometer can detect low-intensity magnetic field.The application of optics atom magnetometer mainly includes inspection
Measure and monitor the growth of standing timber material ultralow field remanent magnetism performance and by marking cell, bacterium and large biological molecule using ultralow field magnetic probe, in turn
Application with biological fields such as magnetic sensing, magnetic imaging and Biological Strength spectrums.However, one of the key application of biological field is that
The preparation of ultralow field magnetic probe.Ultralow field magnetic probe be applied to ultralow field magnetic sensing, magnetic marker, magnetic imaging important medium,
It is played an important role for improving ultralow field Magnetic testi, magnetic marker, the sensitivity of magnetic imaging, scope of application etc..Make at present
Ultralow field magnetic probe is micron-sized, and ingredient is the assembly of magnetic nano-particle and polymer, is needed first
Then synthesizing magnetic nanoparticle carrys out synthesizing magnetic polymer microballoon again, time-consuming, laborious.Meanwhile these ultralow field magnetic probes exist
It can be precipitated in solution, these all leverage its application in ultralow field Magnetic testi, magnetic marker, magnetic imaging.
Summary of the invention
The object of the present invention is to provide a kind of ultralow field magnetic probes.
Ultralow field magnetic probe provided by the present invention, is magnetic nano particle.
The magnetic nano particle is the ligand modified magnetic nano-particle of surface hydrophilicity.
The partial size of the magnetic nano-particle can be 1-100nm, concretely 10-40nm.
The magnetic nano-particle are as follows: ferrimagnetic nanoparticle or the ferrimagnetic nanoparticle of doping, wherein adulterating
Ferrimagnetic nanoparticle in dopant can be at least one of for zinc, cobalt and manganese.
The hydrophilic ligand can be selected from following at least one: 3,4- dihydroxyphenyl propionic acid (DHCA), 2,3- dimercapto
The PEG of succinic acid and double carboxyl modifieds.
Above-mentioned ultralow field magnetic probe is prepared by the method comprising the following steps:
1) magnetic nano-particle is prepared；
2) hydrophilic ligand modification is carried out on the surface of the magnetic nano-particle, it is ligand modified obtains surface hydrophilicity
Magnetic nano-particle, i.e., ultralow field magnetic probe.
In above method step 1), the magnetic nano-particle can be prepared by high temperature organic liquid phase circumfluence method.
Specifically, the magnetic nano-particle can be prepared by following methods: under inert gas protection, with source of iron
For raw material, oleic acid, oleyl amine, octadecylene system in carry out back flow reaction, obtain magnetic nano-particle.
The source of iron concretely ferric acetyl acetonade and/or iron oleate.
The source of iron can also be the mixture of at least one of source of iron and zinc source, cobalt source and manganese source.
The oleic acid can also be at least one of capric acid, enuatrol, potassium oleate.
The octadecylene can also be at least one of octadecylene, benzyl ether, saualane, tri-n-octyl amine.
The source of iron and the mol ratio of oleic acid, oleyl amine and octadecylene are followed successively by 1:1-4:1-4:0.0625-0.25.
The time of the back flow reaction is 30min-2h.
In above method step 2), the operation for carrying out hydrophilic ligand modification are as follows: under inert gas protection, heating
Under the conditions of, the solution of magnetic nano-particle obtained in step 1) is added dropwise in the solution of hydrophilic ligand, is reacted, it will
Reaction system is cooled to room temperature, and alkaline solution is added, and centrifugation collects precipitating, obtains the ligand modified magnetism of surface hydrophilicity and receive
Rice corpuscles.
Hydrophily in the solution of the magnetic nano-particle in the solution of magnetic nano-particle and the hydrophilic ligand
The mass ratio of ligand is 1:2-5, concretely 20mg:50mg.
The temperature of the reaction is 5-80 DEG C, concretely 50 DEG C, time 3-12h, concretely 3h.
Above-mentioned ultralow field magnetic probe is following 1) -3) at least one of in application also belong to protection model of the invention
It encloses:
1) cell magnetic imaging；
2) Bacteria Detection；
3) the magnetic immune reagent kit based on optics atom magnetometer is prepared.
The present invention provide it is a kind of be simple and efficient, low cost no longer need to assemble, can be prepared on a large scale, monodispersity
It is good, bio-compatibility is good, the ultralow field magnetic probe of Nano grade that has excellent magnetic characteristics.Ultralow field magnetic spy prepared by the present invention
Needle has multiple application, optics atom magnetometer can be recycled to carry out non-contact scanning to cell sample by cell endocytic first
Imaging, that is to say, that ultralow field magnetic probe prepared by the present invention may have Cell magnetic imaging applications；Secondly, this invention is super
Low field magnetic probe is incubated for altogether with bacterium, equally can optics atom magnetometer detect magnetic signal, and then can be used for Bacteria Detection；Most
Afterwards, since ultralow field magnetic probe itself has also had both easily by antibody, the large biological molecules such as aptamers, DNA and RNA are modified, therefore
It is likely to be used for magnetic immunocapture, Magneto separate and carries out magnetic signal detection using optics atom magnetometer, ultralow field also just can be used
Magnetic probe prepares the magnetic immune reagent kit based on optics atom magnetometer.
Compared with existing probe and technology of preparing, the present invention is had the advantages that:
1. preparation method of the invention is not necessarily to carry out the preparation of high molecular material, it is simple and efficient, low cost.
2. ultralow field magnetic probe prepared by the present invention is Nano grade, monodispersity is good, does not precipitate.
3. ultralow field magnetic probe ingredient prepared by the present invention is single simple.
4. material involved in the present invention is commercially available, while method is novel, and simple process, equipment are common, handling good, function
Can be powerful, and can once prepare a large amount of ultralow field magnetic probe.
5. ultralow field magnetic probe size prepared by the present invention is small, there is superparamagnetism at room temperature.
Ultralow field magnetic probe prepared by 6 present invention shows preferable ultralow field remanent magnetism signal strength.
7. ultralow field magnetic probe prepared by the present invention can carry out cell marking, research in terms of biological magnetic imaging is carried out.
8. ultralow field magnetic probe prepared by the present invention can carry out Bacteria Detection, for biological magnetic sensing.
9. ultralow field magnetic probe prepared by the present invention has had both easily by big point of the biology such as antibody, aptamers, DNA and RNA
Son modification, it is thus possible to it is used for magnetic immunocapture, Magneto separate and using the progress magnetic signal detection of optics atom magnetometer, also
The magnetic immune reagent kit based on optics atom magnetometer can be prepared with ultralow field magnetic probe.
In consideration of it, the present invention design it is a kind of be simple and efficient, low cost synthetic method, can prepare high-volume synthesis, single point
Dissipating the ultralow field magnetic probe of Nano grade that property is good, has excellent magnetic characteristics has important scientific meaning and huge using valence
Value.
Detailed description of the invention
Fig. 1 is transmission electron microscope (TEM) figure of magnetic nano-particle prepared by step 1 in the embodiment of the present invention 1.
Fig. 2 a is the transmission electron microscope (TEM) of ultralow field magnetic probe prepared by step 2 in the embodiment of the present invention 1
Figure, Fig. 2 b be metal Ion-hydrophilic Ligand before modified after compatibility experiments contrast effect figure.
Fig. 3 is transmission electron microscope (TEM) photo of ultralow field magnetic probe prepared by the embodiment of the present invention 2.
Fig. 4 is that the dynamic light scattering (DLS) of magnetic nano-particle prepared by the embodiment of the present invention 3 surveys hydrodynamics partial size
Histogram.
Fig. 5 is transmission electron microscope (TEM) figure of ultralow field magnetic probe prepared by the embodiment of the present invention 4.
Fig. 6 is vibrating specimen magnetometer (VSM) map of magnetic nano-particle prepared by the embodiment of the present invention 5.
Fig. 7 is remanent magnetism signal-figure-of-merit curve of ultralow field magnetic probe prepared by the embodiment of the present invention 6.
Fig. 8 is the A549 cell toxicant rationality test of ultralow field magnetic probe in the embodiment of the present invention 7.
Fig. 9 is that ultralow field magnetic probe is by after A549 cell endocytic in the embodiment of the present invention 8, in the inspection of optics atom magnetometer
Remanent magnetism signal stabilization under surveying.
After Figure 10 is ultralow field magnetic probe in the embodiment of the present invention 9 and staphylococcus aureus co-cultivation, in optical microphotograph
The bacterium picture shot under mirror.
Figure 11 is that ultralow field magnetic probe is with after staphylococcus aureus co-cultivation in the embodiment of the present invention 9, and sample is in optics
The magnetic signal strength detected under atom magnetometer.
Specific embodiment
The present invention will be described below by way of specific embodiments, but the present invention is not limited thereto.
Experimental method used in following embodiments is conventional method unless otherwise specified；Institute in following embodiments
Reagent, material etc., are commercially available unless otherwise specified.
Iron oleate employed in following embodiments is prepared by following methods:
The mixed solvent of ethyl alcohol, distilled water and hexamethylene is prepared, wherein the volume ratio of three is ethyl alcohol: distilled water: hexamethylene
The mixed solvent of six chloride hydrate three-iron (purity 98%) of 40mmol, 120mmol oleic acid and 280mL are added alkane=8:6:14
To the there-necked flask of 250mL.1600rpm/min magnetic agitation is uniformly mixed, and nitrogen protection is warming up to 70 DEG C and reacts at 70 DEG C
4h.Heat source is removed, room temperature is cooled to, reaction mother liquor moves in separatory funnel, and 30mL distilled water is added, takes oily phase, then use liquid separation
Funnel is extracted twice, and takes oil phase part point in clean beaker, and normal-temperature vacuum makes solvent evaporation completely, obtains waxy solid, i.e.,
Product iron oleate.
Embodiment 1
1,2mmol ferric acetyl acetonade, 6mmol oleic acid, 6mmol oleyl amine and 20ml octadecylene are added to three mouthfuls of 150ml
Bottle, 1600rpm/min magnetic agitation are uniformly mixed, and 80 DEG C vacuumize 30min, are filled with nitrogen later, are then warming up to 200 DEG C,
30min is kept, then is warming up to 300 DEG C, flow back 30min, and heat source is removed, room temperature is cooled to, suitable ethyl alcohol is then added,
6000r/min be centrifugated 10min, take precipitating, suitable hexamethylene be then added, dissolves product, 6000r/min again from
The heart separates 10min, takes supernatant liquid, repeats ethanol precipitation/hexamethylene dispersion process 3 times, finally receives prepared magnetism
Rice corpuscles is directly used in tests in next step, or is dispersed in hexamethylene and is stored in sample bottle and is placed in 4 DEG C of refrigerator.
2,100mgDHCA (3,4- is added in the four-hole boiling flask (19*14 × 3) of a 100ml
Dihydroxyhydrocinnamic acid) and 12ml THF, four mouths of four-hole boiling flask be separately connected thermocouple, condensation
The THF of 40mg magnetic nano-particle and 2ml is added in separatory funnel, is filled with nitrogen in systems for pipe, Bent tube stopper and separatory funnel
Gas, flow velocity is slow as far as possible (flow velocity is too fast to take away solvent), and common heating set is heated to 50 DEG C, then opens the work of separatory funnel
Plug, is added dropwise to the THF solution of magnetic nanometer in four-hole boiling flask, reacts 3h under the conditions of 50 DEG C, be then cooled to room temperature,
The NaOH (0.5M) of 1000ul is added, then product is sub-packed in two centrifuge tubes, 3000rpm/min is centrifuged 10min, removal
Liquid takes precipitating, and the deionized water of 2ml is then respectively added into two centrifuge tubes, and product is finally poured into sample by ultrasonic 30min
In bottle, it is placed in 4 DEG C of refrigerator.Complete the preparation process of ultralow field magnetic probe.
Transmission electron microscope (TEM) picture such as Fig. 1 of the magnetic nano-particle as prepared by step 1 in the embodiment 1
It is shown, a in transmission electron microscope (TEM) picture such as Fig. 2 of ultralow field magnetic probe prepared by step 2) shown in, metal Ion-hydrophilic Ligand
Modified (the ultralow field magnetic probe of preparation, Fig. 2 b in left centrifuge tube) and metal Ion-hydrophilic Ligand before modified (magnetic nano-particle of preparation,
Right centrifuge tube in Fig. 2 b) Experimental comparison's effect picture such as Fig. 2 in b) shown in.
From Fig. 1 and Fig. 2: prepared ultralow field magnetic probe has good monodispersity and has good water-soluble
Property.
Embodiment 2
2mmol ferric acetyl acetonade, 6mmol oleic acid, 6mmol oleyl amine and 20ml octadecylene are added to the there-necked flask of 150ml,
1600rpm/min magnetic agitation is uniformly mixed, and 80 DEG C vacuumize 30min, are filled with nitrogen later, is then warming up to 200 DEG C, is kept
2h, then 300 DEG C are warming up to, flow back 1h, removes heat source, is cooled to room temperature, and suitable ethyl alcohol, 6000r/min centrifugation is then added
10min is separated, precipitating is taken, suitable hexamethylene is then added, dissolves product, 6000r/min is centrifugated 10min again,
Supernatant liquid is taken, ethanol precipitation/hexamethylene dispersion process 3 times is repeated, finally directly uses prepared magnetic nano-particle
It is tested in next step.
Then, 50mgDHCA (3,4- is added in the four-hole boiling flask (19*14 × 3) of a 50ml
Dihydroxyhydrocinnamic acid) and 6ml THF, four mouths of four-hole boiling flask be separately connected thermocouple, condenser pipe,
The THF of 20mg magnetic nanoparticle and 1ml is added in separatory funnel, pours nitrogen in systems for Bent tube stopper and separatory funnel, flows
Speed is slow as far as possible (flow velocity is too fast to take away solvent), and common heating set is heated to 50 DEG C, then opens the piston of separatory funnel, makes
MNPs is added dropwise in four-hole boiling flask, is reacted 3h under the conditions of 50 DEG C, is then cooled to room temperature, and the NaOH of 500ul is added
Then product is sub-packed in two centrifuge tubes by (0.5M), 3000rpm/min is centrifuged 10min, and removal liquid takes precipitating, then
The deionized water of 1ml is respectively added into two centrifuge tubes, ultrasonic 30min finally pours into product in sample bottle, is placed in 4 DEG C
In refrigerator.Complete the preparation process of ultralow field magnetic probe.
Transmission electron microscope (TEM) picture of the ultralow field magnetic probe prepared by the embodiment 2 is as shown in Figure 3.
As shown in Figure 3: under the experiment condition slightly changed to embodiment 1, prepared ultralow field magnetic probe still has
Uniform size and pattern.
Embodiment 3
2mmol ferric acetyl acetonade, 6mmol oleic acid, 6mmol oleyl amine and 20ml octadecylene are added to the there-necked flask of 150ml,
1600rpm/min magnetic agitation is uniformly mixed, and 80 DEG C vacuumize 30min, are filled with nitrogen later, is then warming up to 200 DEG C, is kept
15min, then be warming up to 300 DEG C, flow back 1h, removes heat source, is cooled to room temperature, is then added suitable ethyl alcohol, 6000r/min from
The heart separates 10min, takes precipitating, suitable hexamethylene is then added, dissolves product, 6000r/min is centrifugated again
10min takes supernatant liquid, ethanol precipitation/hexamethylene dispersion process 3 times is repeated, finally by prepared magnetic nano-particle
It is dispersed in the refrigerator that 4 DEG C are stored in sample bottle and be placed in hexamethylene.
The dynamic light scattering (DLS) of the magnetic nano-particle prepared by the embodiment surveys the histogram of hydrodynamics partial size such as
Shown in Fig. 4.
As shown in Figure 4: prepared magnetic nano-particle narrow size distribution, monodispersity are good.
Embodiment 4
1, the preparation of the ferrimagnetic nanoparticle of zinc-manganese element doping
By 1.33mmol ferric acetyl acetonade, 6mmol oleic acid, 6mmol oleyl amine, 0.27mmol zinc chloride, 0.4mmol manganese chloride
The there-necked flask of 50ml is added to 20ml octadecylene, 1600rpm/min magnetic agitation is uniformly mixed, and 80 DEG C vacuumize 30min, it
After be filled with nitrogen, be then warming up to 300 DEG C, flow back 60min, remove heat source, be cooled to room temperature, suitable ethyl alcohol is then added,
6000r/min be centrifugated 10min, take precipitating, suitable hexamethylene be then added, dissolves product, 6000r/min again from
The heart separates 10min, takes supernatant liquid, repeats ethanol precipitation/hexamethylene dispersion process 3 times, finally receives prepared magnetism
Rice corpuscles ((Zn0.4Mn0.6)Fe2O4) hexamethylene colloidal solution pour into the sample bottle of a 20ml, be placed in 4 DEG C of refrigerator
In.
2, the preparation of the ferrimagnetic nanoparticle of the zinc-manganese element doping of 2,3-dimercaptosuccinic acid modification
Take (the Zn of the above-mentioned preparation of 10mL0.4Mn0.6)Fe2O4The hexamethylene colloidal solution and 40mL ethyl alcohol of nanoparticle in from
In heart pipe, 6000rmp is centrifuged 10min, removes upper solution, must precipitate.Precipitating is dried in vacuo, the iron of zinc-manganese element doping is obtained
Oxygen magnetic nano-particle solid.The solid nanoparticles for weighing 10mg are dissolved in 1mL toluene, obtain solution A.In addition, by 10mg's
2,3-dimercaptosuccinic acid is dissolved in the dimethyl sulfoxide of 1mL, obtains solution B.Solution A and B are mixed, centrifuge separation takes black
Precipitating, it is dry, then black solid is dispersed in the deionized water of 1mL, 4 DEG C of preservations.
By the transmission electron microscope of ferrimagnetic nanoparticle prepared by zinc-manganese element doping prepared by the embodiment
(TEM) picture is as shown in Figure 5.
As shown in Figure 5: the ferrimagnetic nanoparticle of zinc-manganese element doping preparation, size uniformity, monodispersity are good.
Embodiment 5
2mmol ferric acetyl acetonade, 6mmol oleic acid, 6mmol oleyl amine and 20ml octadecylene are added to the there-necked flask of 150ml,
1600rpm/min magnetic agitation is uniformly mixed, and 80 DEG C vacuumize 30min, are filled with nitrogen later, is then warming up to 200 DEG C, is kept
15min, then be warming up to 300 DEG C, flow back 2h, removes heat source, is cooled to room temperature, is then added suitable ethyl alcohol, 6000r/min from
The heart separates 10min, takes precipitating, suitable hexamethylene is then added, dissolves product, 6000r/min is centrifugated again
10min takes supernatant liquid, ethanol precipitation/hexamethylene dispersion process 3 times is repeated, finally by prepared magnetic nano-particle
It is dispersed in the refrigerator that 4 DEG C are stored in sample bottle and be placed in hexamethylene.
The picture of the vibrating specimen magnetometer (VSM) of the magnetic nano-particle as prepared by the embodiment is as shown in Figure 6.
As shown in Figure 6: prepared magnetic nano-particle has preferable saturation magnetization.
Embodiment 6
The ultralow field magnetic probe prepared in embodiment 1 is weighed into different quality (between 0~10 microgram) in clean respectively
Glass slide on, it is forever ferromagnetic away from micro slide 2cm magnetization 2min at a distance, then take magnet away.The sample difference after magnetization
Magnetic signal is measured with optics atom magnetometer, obtains the quality of ultralow field magnetic probe and the relational graph of magnetic signal.
Relational graph such as Fig. 7 institute of the quality of the ultralow field magnetic probe and the magnetic signal measured in optics atom magnetometer
Show.
As shown in Figure 7: ultralow field magnetic probe prepared by embodiment 1 has good remanent magnetism-quality linear dependence.
Embodiment 7
First by A549 cell inoculation in 96 orifice plates (1 × 105) in, using complete medium (10% fetal calf serum, 1%
It is dual anti-) in 5% carbon dioxide environment cultivate 17h.Equal cells are adherent and in good condition, outwell complete medium, and nothing is added
Blood serum medium (200 μ L), while ultralow field magnetic probe prepared by a certain amount of embodiment 1 is added, so that probe final concentration
It is 0,5,20,50 μ g/mL.It cultivates under identical condition for 24 hours.Then the culture medium with probe is discarded, then cell uses
PBS is cleaned three times.The CCK-8 reagent of 20 μ L is added while complete medium (200 μ L) is added, in 5% titanium dioxide carbocyclic ring
2h is cultivated in border.Ultraviolet absorption value directly with microplate reader detection solution at 405nm.By with blank test (same volume
PBS) comparison, calculate the cytotoxicity of nano-probe.
The result of the A549 cell toxicant rationality test of ultralow field magnetic probe is as shown in Figure 8.
As shown in Figure 8: the ultralow field magnetic probe is under higher incubation concentration and longer incubation time, to cell without poison
Property.
Embodiment 8
By A549 cell inoculation in the dedicated miniature incubator (1 × 10 of magnetometer4), using complete medium (10% tire
Cow's serum, 1% is dual anti-) 17h is cultivated in 5% carbon dioxide environment.Equal cells are adherent and in good condition, outwell complete culture
Base is added serum free medium (200 μ L), while ultralow field magnetic probe (20 μ g/mL) prepared in embodiment 1 is added and continues
4h is cultivated under the same conditions.Then cell culture medium is discarded, is cleaned 3 times with PBS.After complete medium is added, use is forever ferromagnetic
Iron is in the cell 2min for having probe away from magnetization at micro slide 2cm.With the probe after the measurement magnetization of optics atom magnetometer thin
Remanent magnetism signal in born of the same parents, while recording the intensity value of the signal relative to time change.To judge that probe magnetizes in the cell
The stability of the remanent magnetism signal of 2h afterwards.
The stability of remanent magnetism signal is as shown in Figure 9 in ultralow field magnetic probe living cells.
As shown in Figure 9: prepared ultralow field magnetic probe has good signal stabilization.
Embodiment 9
Staphylococcus aureus (S.aureus) is cultivated into 4h in TBS culture medium, is cultivated to S.aureus to logarithmic phase,
It is inoculated in the dedicated miniature incubator (1 × 10 of magnetometer5) in, optical microphotograph microscopic observation bacterial growth situation will be thin
Bacterium ultralow field magnetic probe prepared in PBS buffer solution and in 5 μ g/mL embodiments 1 is incubated for 1h.With ferromagnetic iron forever away from loading
Magnetization has the bacterium 2min of probe at piece 2cm.With remanent magnetism of the probe after the measurement magnetization of optics atom magnetometer in cell
Signal.
The optical microscope picture of the bacterium obtained by the embodiment is as shown in Figure 10.
As shown in Figure 10: the bacterial growth of culture is in order.
After the ultralow field magnetic probe of bacterial incubations obtained by the embodiment, believed using the remanent magnetism that optics atom magnetometer measures
Number as shown in figure 11.
As shown in Figure 11: prepared ultralow field magnetic probe can be marked bacterium and under optics atom magnetometer
Detect higher remanent magnetism signal.
Claims (1)
1. application of the ligand modified magnetic nano-particle of surface hydrophilicity as ultralow field magnetic probe；
The application is ultralow field magnetic probe following 1) -2) at least one of in application:
1) cell magnetic imaging；
2) Bacteria Detection；
The ligand modified magnetic nano-particle of the surface hydrophilicity is prepared via a method which to obtain:
2mmol ferric acetyl acetonade, 6mmol oleic acid, 6mmol oleyl amine and 20ml octadecylene are added to the there-necked flask of 150ml,
1600rpm/min magnetic agitation is uniformly mixed, and 80 DEG C vacuumize 30min, are filled with nitrogen later, is then warming up to 200 DEG C, is kept
30min, then 300 DEG C are warming up to, flow back 30min, removes heat source, is cooled to room temperature, suitable ethyl alcohol, 6000r/ is then added
Min is centrifugated 10min, takes precipitating, suitable hexamethylene is then added, dissolves product, 6000r/min is centrifugated again
10min takes supernatant liquid, ethanol precipitation/hexamethylene dispersion process 3 times is repeated, finally by prepared magnetic nano-particle
It is directly used in and tests in next step, or be dispersed in hexamethylene and be stored in sample bottle and be placed in 4 DEG C of refrigerator；
The THF of 100mgDHCA and 12ml is added in the four-hole boiling flask of a 100ml, four mouths of four-hole boiling flask are separately connected
The THF of 40mg magnetic nano-particle and 2ml is added in separatory funnel, is being for thermocouple, condenser pipe, Bent tube stopper and separatory funnel
Nitrogen is filled in system, flow velocity is slow as far as possible, and common heating set is heated to 50 DEG C, then opens the piston of separatory funnel, makes magnetic nanometer
The THF solution of particle is added dropwise in four-hole boiling flask, is reacted 3h under the conditions of 50 DEG C, is then cooled to room temperature, and 1000ul is added
0.5M NaOH, then product is sub-packed in two centrifuge tubes, 3000rpm/min be centrifuged 10min, removal liquid take it is heavy
It forms sediment, the deionized water of 2ml is then respectively added into two centrifuge tubes, product is finally poured into sample bottle, set by ultrasonic 30min
In 4 DEG C of refrigerator, that is, complete the preparation process of ultralow field magnetic probe.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611120451.4A CN106501553B (en) | 2016-12-08 | 2016-12-08 | A kind of ultralow field nanometer magnetic probe and the preparation method and application thereof |
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