CN109908172A - A kind of magnetic iron oxide and elemental selenium Nano Composite Particles and its preparation method and application - Google Patents
A kind of magnetic iron oxide and elemental selenium Nano Composite Particles and its preparation method and application Download PDFInfo
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 120
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 239000002245 particle Substances 0.000 title claims abstract description 32
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000011246 composite particle Substances 0.000 claims abstract description 25
- 239000002105 nanoparticle Substances 0.000 claims abstract description 25
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000012043 crude product Substances 0.000 claims abstract description 15
- BVTBRVFYZUCAKH-UHFFFAOYSA-L disodium selenite Chemical compound [Na+].[Na+].[O-][Se]([O-])=O BVTBRVFYZUCAKH-UHFFFAOYSA-L 0.000 claims abstract description 15
- 239000011669 selenium Substances 0.000 claims abstract description 15
- 229960001471 sodium selenite Drugs 0.000 claims abstract description 15
- 239000011781 sodium selenite Substances 0.000 claims abstract description 15
- 235000015921 sodium selenite Nutrition 0.000 claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 238000002955 isolation Methods 0.000 claims abstract description 13
- 230000001580 bacterial effect Effects 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 229920001661 Chitosan Polymers 0.000 claims abstract description 6
- 235000009508 confectionery Nutrition 0.000 claims abstract description 6
- 108090000765 processed proteins & peptides Proteins 0.000 claims abstract description 6
- 238000012545 processing Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 42
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- 238000004108 freeze drying Methods 0.000 claims description 14
- 230000010355 oscillation Effects 0.000 claims description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- 230000002085 persistent effect Effects 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 6
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 238000000975 co-precipitation Methods 0.000 claims description 3
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 3
- 239000003381 stabilizer Substances 0.000 claims description 3
- 230000001954 sterilising effect Effects 0.000 claims description 3
- 229910000828 alnico Inorganic materials 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 239000003431 cross linking reagent Substances 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 238000004659 sterilization and disinfection Methods 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 10
- 239000003814 drug Substances 0.000 abstract description 4
- 230000003115 biocidal effect Effects 0.000 abstract description 3
- 239000012620 biological material Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 14
- 235000011649 selenium Nutrition 0.000 description 11
- 239000000523 sample Substances 0.000 description 10
- 229910052711 selenium Inorganic materials 0.000 description 10
- 229940091258 selenium supplement Drugs 0.000 description 10
- 230000000844 anti-bacterial effect Effects 0.000 description 8
- 241000894006 Bacteria Species 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- -1 Selenite radical ion Chemical class 0.000 description 3
- 235000013339 cereals Nutrition 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- FXIJXJFYAWKLMQ-PRKWKTPOSA-N [Se].OC(=O)[C@@H](N)CCC(=O)N[C@@H](CS)C(=O)NCC(O)=O.OC(=O)[C@@H](N)CCC(=O)N[C@@H](CS)C(=O)NCC(O)=O Chemical compound [Se].OC(=O)[C@@H](N)CCC(=O)N[C@@H](CS)C(=O)NCC(O)=O.OC(=O)[C@@H](N)CCC(=O)N[C@@H](CS)C(=O)NCC(O)=O FXIJXJFYAWKLMQ-PRKWKTPOSA-N 0.000 description 2
- 239000000908 ammonium hydroxide Substances 0.000 description 2
- 230000001093 anti-cancer Effects 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 230000006196 deacetylation Effects 0.000 description 2
- 238000003381 deacetylation reaction Methods 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 238000006392 deoxygenation reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 208000015181 infectious disease Diseases 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- 238000007885 magnetic separation Methods 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 229940082569 selenite Drugs 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- 206010059866 Drug resistance Diseases 0.000 description 1
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- 229910021577 Iron(II) chloride Inorganic materials 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 208000026935 allergic disease Diseases 0.000 description 1
- 230000007815 allergy Effects 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 238000013196 antibiotherapy Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 230000003013 cytotoxicity Effects 0.000 description 1
- 231100000135 cytotoxicity Toxicity 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 231100000734 genotoxic potential Toxicity 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- 210000004379 membrane Anatomy 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 125000003748 selenium group Chemical group *[Se]* 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012549 training Methods 0.000 description 1
Abstract
The invention belongs to technical field of biological material, specifically provide a kind of magnetic iron oxide and elemental selenium Nano Composite Particles and its preparation method and application, the stable magnetic ferric oxide nano particle of chitosan is added into sodium selenite and the sweet peptide mixed solution of ancient Guang, solid composite particles crude product is obtained under basic catalyst effect, is centrifuged and is freeze-dried obtained magnetic iron oxide and elemental selenium Nano Composite Particles after Magnetic Isolation again.Preparation method of the present invention is simple, it is easy to operate, the composite particles contain element Se nanoparticles and magnetic ferric oxide nano particle simultaneously, two kinds of materials all have antibiotic property and biocompatibility, under the action of an external magnetic field, elemental selenium in composite particles can be penetrated into together bacterial biof iotalm by magnetic iron oxide, so that the obvious processing effect to biomembrane enhances, and can be widely used in a variety of field of medicaments.
Description
Technical field
The invention belongs to technical field of biological material, and in particular to a kind of magnetic iron oxide and elemental selenium Nano Composite Particles and its
Preparation method and application.
Background technique
Now, bacterium infection is considered as influencing a significant problem of World Medical Healthy System.Outside patient carries out
When section's operation or orthopaedics are implanted into, bacterium can enter wound from the skin or mucous membrane of patient, cause bacterium infection or implantation failure.More
The serious is one layer of biomembranes easy to form after bacterium contact surface.Bacterial biof iotalm once being formed, may be prevented from antibiotic etc.
Drug penetrates into inside biomembrane, keeps antibiotherapy effect poor or entirely ineffective.
For this problem, bio-nanotechnology is developed rapidly, and antibacterial nano particle just gradually replaces antibiosis
Element is to eliminate bacterial drug resistance, wherein silver and selenium nano particle are concerned.But silver can generate active oxygen former (ROS) and to the food in one's mouth
Newborn zooblast generates genotoxic potential, and part human body is to silver-colored allergy.On the contrary, selenium is a kind of necessity that can be found in human body
Microelement, selenium can control the presence of ROS, be a kind of natural anti-oxidation protein.Selenium has drawn in biomedical applications field
Broad interest has been played, there is antibacterial, anticancer and biocompatibility.Selenium is effective to many bacteriums, including staphylococcus aureus
(S.aureus) and Escherichia coli (E.coli) etc..But because of infiltration problem, selenium imitates the antibacterial of the bacterial biof iotalm of 10 μ m-thicks
Fruit is very limited.
Summary of the invention
For technical problem present in background technique, the object of the present invention is to provide a kind of magnetic iron oxide and elemental seleniums
Nano Composite Particles and its preparation method and application, which contains element Se nanoparticles simultaneously and magnetic iron oxide is received
Rice particle, under the action of an external magnetic field, magnetic ferric oxide nano particle can seep the Se nanoparticles in composite particles together
Enter bacterial biof iotalm, so that the obvious processing effect to biomembrane enhances.
The technical solution that the present invention uses is: magnetic is added into sodium selenite and ancient Guang sweet peptide (GSH) mixed solution
Property ferric oxide nano particle, solid crude product composite particles are obtained under the action of basic catalyst, are centrifuged and magnetic point
It is freeze-dried magnetic iron oxide and elemental selenium Nano Composite Particles obtained again from after.
Steps are as follows for the specific preparation method of magnetic iron oxide and elemental selenium Nano Composite Particles:
(1) by volume by the GSH solution of the sodium selenite solution of 0.01~0.07mol/L and 0.01~0.07mol/L
1:4 mixing, vibrates 15min, hunting speed 300rpm obtains mixed solution on platform shaker after mixing；
During oscillation obtains mixed solution, sodium selenite and the concentration of GSH need to be controlled, and makes the two concentration phase
Together, available selenium diglutathione intermediate after mixing, to obtain elemental selenium after subsequent step plus alkali.
(2) 50~300mg magnetic iron oxide is added in the mixed solution of step (1), after persistent oscillation 15min；Finally, plus
Enter basic catalyst (1.0mol/L NaOH) solution, the pH value of mixed solution is made to be adjusted to 10~13, after persistent oscillation 3h, oscillation speed
Degree is 250rpm, obtains crude product composite particles；
Alternatively, it is preferred that are as follows: first 50~300mg magnetic iron oxide is dispersed in aqueous phase solution, then with sodium selenite and GSH
Mixed solution mixing, the dispersion effect of such magnetic iron oxide are more preferable.
Magnetic iron oxide dosage is too high to be not easy to disperse, and can generate free iron oxide, and dosage influences magnetism very little, cannot
Obtain satisfactory magnetic composite particle.
(3) the crude product composite particles that step (2) obtains wash 3 times through deionized water, are centrifugated 10min through 6000rpm,
Then it is freeze-dried after Magnetic Isolation again, obtains magnetic iron oxide and elemental selenium Nano Composite Particles.
Centrifuge separation can remove water-soluble substances, and such as alkali, the extra sweet peptide of ancient Guang, Magnetic Isolation is that have in order to obtain
Magnetic joint product excludes not compound successful elemental selenium.
The magnetic iron oxide is magnetic ferroferric oxide nanometer particle, is prepared using coprecipitation, preparation method are as follows:
0.15g low-molecular weight chitoglycan (deacetylation 75%-85%) is dissolved in the acetum of 30mL 1%, is used
PH value is adjusted to 4.8 by 1.0mol/L NaOH.1.34g FeCl is added2·4H2O and 3.40g FeCl3·6H2O is poly- in above-mentioned shell
Sugar juice obtains mixed solution.By this mixed solution strong stirring, the ammonium hydroxide and 10mL 0.75% of 30mL 25% is successively added
TPP solution.50 DEG C of the reaction was continued 1h, entire reaction carry out under the conditions of nitrogen is led in deoxygenation.Crude product deionization after reaction
It water washing 3 times, is centrifuged and Magnetic Isolation, freeze-drying, obtains solid magnetic oxidation iron sample.
The partial size of magnetic ferric oxide nano particle obtained is 1-20nm；Wherein, low-molecular weight chitoglycan is used as to stablize
Agent, sodium tripolyphosphate (TPP) are crosslinking agent.
The basic catalyst is the NaOH solution of 1.0mol/L.
The Magnetic Isolation is using alnico magnets such as iron, cobalt, nickel.
Composite particles made from the method for the present invention can be used for the processing of bacterial biof iotalm, the biological medicines neck such as drug transmission
Domain, concrete application method are as follows: the composite particles after freeze-drying are made into water using high-temperature sterilization water after ultraviolet lamp sterilizes
Solution, solution concentration 0.025-0.25mg/mL remove precipitating, act directly on biomembrane.
The magnetic ferric oxide nano particle that the present invention uses coprecipitation to prepare partial size as 1-20nm first, stabilizer are
Chitosan with positive electricity after sodium selenite and GSH solution is added, forms selenium diglutathione intermediate, under alkaline condition,
Selenite radical ion is reduced to elemental selenium, is attached to chitosan surface, obtains compound micro- containing magnetic iron oxide and elemental selenium
Grain.Wherein, alkaline power will affect the formation shape of elemental selenium.Alkalinity is weak, obtains subsphaeroidal element Se nanoparticles；It is alkaline strong,
Obtain rodlike elemental selenium.Gained composite particles have antibacterial anti-cancer properties and magnetism, good biocompatibility, to bacterium living beings simultaneously
The treatment effect of film is obvious, and can be widely used in a variety of biomedicine fields.
The beneficial effects of the present invention are:
(1) by magnetic iron oxide in conjunction with elemental selenium, under the action of externally-applied magnetic field, magnetic iron oxide can be by elemental selenium one
With penetrating into inside biomembrane, the penetrating power of elemental selenium is greatly enhanced, while also more effectively having played elemental selenium to bacterium living beings
The antibacterial effect of film.
(2) partial size of used magnetic iron oxide is 1-20nm, itself has certain anti-microbial property, with elemental selenium knot
It closes, its coordinative role can be played, further increase the antibacterial effect of the composite particles.
(3) use chitosan of the surface with positive electricity as stabilizer, the negative electrical charge in adsorbable solution, such as selenite radical
Ion, selenium anion, itself has biocompatibility, will not cause apparent cytotoxicity.
(4) preparation process is simple, easy to operate.
This experiment is further illustrated with reference to the accompanying drawing.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture of magnetic ferric oxide nano particle in embodiment 1.
Fig. 2 is the XRD diagram of magnetic ferric oxide nano particle in embodiment 1.
Fig. 3 is the transmission electron microscope picture of magnetic iron oxide and elemental selenium Nano Composite Particles in embodiment 1.
Fig. 4 is the transmission electron microscope picture of magnetic iron oxide and elemental selenium Nano Composite Particles in embodiment 2.
Fig. 5 is the antibiont film activity figure of different samples in embodiment 1 and comparative example 1.Wherein, a is control group
(PBS) (blank assay), b are elemental selenium (SeNPs), and c is magnetic iron oxide (IONPs), and d is composite particles (SeIONPs)；It is green
Color table shows living cells, and red indicates dead cell.
Specific embodiment
Presently in connection with specific embodiment, the invention will be further described, following embodiment be intended to illustrate invention rather than
Limitation of the invention further.
Embodiment 1
(1) preparation of magnetic ferric oxide nano particle: by 0.15g low-molecular weight chitoglycan (deacetylation 75%-
85%) it is dissolved in the acetum of 30mL 1%, pH value is adjusted to 4.8 with 1.0mol/L NaOH.1.34g is added
FeCl2·4H2O and 3.40g FeCl3·6H2O is in above-mentioned chitosan solution.By this mixture strong stirring, 30mL is successively added
25% ammonium hydroxide and the TPP solution of 10mL 0.75%.50 DEG C of the reaction was continued 1h, entire reaction carry out under the conditions of nitrogen is led in deoxygenation.
Crude product is washed with deionized 3 times after reaction, is centrifuged and Magnetic Isolation, freeze-drying, obtains solid magnetic oxidation
Iron sample turns out to be magnetic ferroferric oxide, partial size 7.0-12.3nm through XRD.
(2) preparation of magnetic iron oxide and elemental selenium Nano Composite Particles；By the sodium selenite solution of 8mL 0.07mol/L
It is mixed with the GSH solution of 32mL 0.07mol/L, shaken at room temperature 15min is formed among the sweet peptide of the ancient Guang of selenium two on platform rocker
Body, and reaction is made to reach balance, hunting speed 300rpm.Then, the magnetic ferric oxide nano that 150mg freeze-drying is added is micro-
Grain, after persistent oscillation 15min.The NaOH solution of 3.0mL 1.0mol/L is added, solution ph 11.08, the reaction was continued by 250rpm
3h.Crude product is washed with deionized 3 times, is centrifuged and Magnetic Isolation, freeze-drying obtain solid composite particles sample.
Fig. 1 and Fig. 2 is respectively the transmission electron microscope picture and XRD diagram of magnetic iron oxide；Fig. 3 is that magnetic iron oxide is received with elemental selenium
The transmission electron microscope picture of rice composite particles, the subsphaeroidal particle of black are elemental selenium, and the shallower fine grained of color is magnetic iron oxide,
The two is adhered to each other.
Fig. 5 is the distribution map of dead cell and living cells in bacterial biof iotalm after different sample treatments, and test equipment is Germany
The laser confocal microscope of Cai Si LSM700.Wherein, red point indicates that dead cell, green point indicate living cells, blue dotted line
For magnetic field line of demarcation.Bacterial membrane used is the bacterial biof iotalm that S.aureus film forming strain culturing generates two days later, biomembrane training
After supporting well, a fritter circular magnet (size is close with disme), right side non-magnet are placed in the left side of square container bottom
Effect is added sample solution and is handled.Fig. 5 a and Fig. 5 b are respectively the biomembrane controlled after sample and elemental selenium effect.Fig. 5 a is left
The living cells of right two sides is distributed close, no significant change；The distribution of the living cells and dead cell of the two sides Fig. 5 b is close, becomes without obvious
Change.Fig. 5 c and Fig. 5 d are respectively magnetic iron oxide and magnetic iron oxide and the processed biomembrane of elemental selenium composite sample.Figure
The dead cell of 5c left side of dotted line is obviously more than right side, illustrates that magnetic fields can enhance the antibacterial effect of magnetic iron oxide；Fig. 5 d is empty
Dead cell distribution on the left of line is obvious more than right side, and is higher than Fig. 5 b and Fig. 5 c, and it is compound micro- to illustrate that magnetic fields significantly enhance
The antibacterial effect of grain, hence it is evident that be better than the effect of magnetic iron oxide and elemental selenium independent role.
Embodiment 2
(1) preparation of magnetic ferric oxide nano particle: with embodiment 1.
(2) preparation of magnetic iron oxide and elemental selenium Nano Composite Particles；By the sodium selenite solution of 8mL 0.05mol/L
It is mixed with the GSH solution of 32mL 0.05mol/L, the shaken at room temperature 15min on platform rocker, hunting speed 300rpm.So
Afterwards, the magnetic ferric oxide nano particles of 100mg freeze-drying are added, after persistent oscillation 15min.The NaOH of 3.5mL mol/L is added
Solution, solution ph 11.73,250rpm the reaction was continued 3h.Crude product is washed with deionized 3 times, is centrifuged and magnetic
Separation, freeze-drying, obtains solid composite particles sample.
Fig. 4 is the transmission electron microscope picture of magnetic iron oxide and elemental selenium Nano Composite Particles, and for elemental selenium at rodlike, color is shallower
Fine grained be magnetic iron oxide, the two is adhered to each other.
Embodiment 3
(1) preparation of magnetic ferric oxide nano particle: with embodiment 1.
(2) preparation of magnetic iron oxide and elemental selenium Nano Composite Particles；By the sodium selenite solution of 8mL 0.01mol/L
It is mixed with the GSH solution of 32mL 0.01mol/L, 15min, hunting speed 300rpm is vibrated on platform rocker.Then,
The magnetic ferric oxide nano particles of 50mg freeze-drying are added, after persistent oscillation 15min.The NaOH solution of 3.5mL mol/L is added,
Solution ph is 11.73,250rpm the reaction was continued 3h.Crude product is washed with deionized 3 times, is centrifuged and Magnetic Isolation,
Freeze-drying, obtains solid composite particles sample.
Embodiment 4
(1) preparation of magnetic ferric oxide nano particle: with embodiment 1.
(2) preparation of magnetic iron oxide and elemental selenium Nano Composite Particles；By the sodium selenite solution of 8mL 0.05mol/L
It is mixed with the GSH solution of 32mL 0.05mol/L, the shaken at room temperature 15min on platform rocker, hunting speed 300rpm.So
Afterwards, first 100mg magnetic iron oxide is dispersed in aqueous phase solution, then is mixed with sodium selenite and GSH mixed solution, after persistent oscillation
15min.The NaOH solution of 3.5mL mol/L, solution ph 11.73,250rpm the reaction was continued 3h is added.Crude product deionization
It water washing 3 times, is centrifuged and Magnetic Isolation, freeze-drying obtains solid composite particles sample.
Comparative example 1
The sodium selenite solution of 8mL 0.07mol/L is mixed with the GSH solution of 32mL 0.07mol/L, is vibrated in platform
Shaken at room temperature 15min forms the sweet peptide intermediate of the ancient Guang of selenium two on device, and reaction is made to reach balance, hunting speed 300rpm.So
Afterwards, the NaOH solution of 3.0mL 1.0mol/L, solution ph 11.08,250rpm the reaction was continued 30min is added.Crude product is spent
It ion water washing 3 times, is centrifuged and Magnetic Isolation, freeze-drying obtains selenium element particulate samples.
Comparative example 2
(1) preparation of magnetic ferric oxide nano particle: with embodiment 1.
(2) preparation of magnetic iron oxide and elemental selenium Nano Composite Particles；By the sodium selenite solution of 8mL 1.0mol/L
It is mixed with the GSH solution of 32mL 1.0mol/L, the shaken at room temperature 15min on platform rocker, hunting speed 300rpm.So
Afterwards, the magnetic ferric oxide nano particles of 100mg freeze-drying are added, after persistent oscillation 15min.The NaOH of 3.5mL mol/L is added
Solution, solution ph 11.73,250rpm the reaction was continued 3h.Crude product is washed with deionized 3 times, is centrifuged and magnetic
Separation, freeze-drying, is unable to get solid composite particles sample.
Claims (8)
1. a kind of magnetic iron oxide and elemental selenium Nano Composite Particles, it is characterised in that: the composite particles contain element simultaneously
Se nanoparticles and magnetic ferric oxide nano particle.
2. a kind of preparation method of magnetic iron oxide as described in claim 1 and elemental selenium Nano Composite Particles, feature exist
In: the preparation method is that: stable magnetic oxygenated of chitosan is added into sodium selenite and ancient Guang sweet peptide (GSH) mixed solution
Iron nanoparticle obtains solid crude product composite particles under the action of basic catalyst, be centrifuged with after Magnetic Isolation again
It is freeze-dried and magnetic iron oxide and elemental selenium Nano Composite Particles is made.
3. the preparation method of magnetic iron oxide as claimed in claim 2 and elemental selenium Nano Composite Particles, it is characterised in that: institute
Stating preparation method, steps are as follows:
(1) the GSH solution of the sodium selenite solution of 0.01~0.07mol/L and 0.01~0.07mol/L are pressed to the volume ratio of 1:4
Mixing, vibrates 15min, hunting speed 300rpm obtains mixed solution on platform shaker after mixing；
(2) 50~300mg magnetic iron oxide is added in the mixed solution of step (1), after persistent oscillation 15min；Finally, alkali is added
Property catalyst solution, makes the pH value of mixed solution be adjusted to 10~13, after persistent oscillation 3h, hunting speed 250rpm, obtains crude product
Composite particles；
(3) the crude product composite particles that step (2) obtains wash 3 times through deionized water, are centrifugated 10min through 6000rpm, then pass through
It is freeze-dried after Magnetic Isolation, obtains magnetic iron oxide and elemental selenium Nano Composite Particles.
4. the preparation method of magnetic iron oxide as claimed in claim 2 or claim 3 and elemental selenium Nano Composite Particles, feature exist
In: the magnetic iron oxide is the magnetic ferroferric oxide nanometer particle that partial size is 1-20nm, using coprecipitation, with deacetylated
The low-molecular weight chitoglycan that degree is 75%-85% is stabilizer, and sodium tripolyphosphate (TPP) is prepared for crosslinking agent.
5. the preparation method of magnetic iron oxide as claimed in claim 3 and elemental selenium Nano Composite Particles, it is characterised in that: step
Suddenly the NaOH solution that the basic catalyst that (2) are added is 1.0mol/L.
6. the preparation method of magnetic iron oxide as claimed in claim 3 and elemental selenium Nano Composite Particles, it is characterised in that: step
Suddenly Magnetic Isolation described in (3) uses iron, cobalt, nickel alnico magnets.
7. a kind of application of magnetic iron oxide as described in claim 1 and elemental selenium Nano Composite Particles, it is characterised in that: institute
State processing of the composite particles for bacterial biof iotalm.
8. the application of magnetic iron oxide as claimed in claim 7 and elemental selenium Nano Composite Particles, it is characterised in that: described multiple
Close the application method of particle are as follows: after the composite particles ultraviolet lamp sterilizing after freeze-drying, use high-temperature sterilization water wiring solution-forming
Concentration is the aqueous solution of 0.025-0.25mg/mL, removes precipitating, acts directly on biomembrane.
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