CN102766267A - Preparation method of chitosan hydrogel containing magnetic nanoparticle - Google Patents
Preparation method of chitosan hydrogel containing magnetic nanoparticle Download PDFInfo
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- CN102766267A CN102766267A CN2012102553537A CN201210255353A CN102766267A CN 102766267 A CN102766267 A CN 102766267A CN 2012102553537 A CN2012102553537 A CN 2012102553537A CN 201210255353 A CN201210255353 A CN 201210255353A CN 102766267 A CN102766267 A CN 102766267A
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Abstract
The invention relates to a preparation method of chitosan hydrogel containing magnetic nanoparticle, which comprises the following steps of: (1) dissolving the chitosan powder in 0.5%-5% of acetic acid solution, mechanically stirring until clarification; taking 5-10ml of the mixture obtained in the step (1), adding 200ul-1000ul of magnetic nanoparticle dispersion with the iron content of 1.2g/ml-1.4g/ml, then adding 200ul-1000ul of crosslinking agent, reacting at room temperature for 2h-36h, and conducting Schiff reaction to produce the chitosan hydrogel containing magnetic nanoparticle. The magnetic nanoparticle is polyacrylic acid coated iron oxide nanoparticle. The crosslinking agent is glutaraldehyde or a mixture of polyethylene glycol and formaldehyde. The chitosan hydrogel containing magnetic nanoparticle is brown, transparent and has no significant precipitation and reunion internal, can be used as an auxiliary pressure material for masks used in the burn treatment, so as to enable the mask better fit the face of people and further strengthen the effect of pressure treatment.
Description
Technical field
The present invention relates to the preparing gel technology of chitosan and verivate thereof, and the technology of preparing of plural gel that contains chitosan and the verivate thereof of magnetic nano-particle.
Background technology
Chitosan (chitosan) is to be obtained through deacetylation by the Regitex FA (chitin) that nature extensively exists, and chemical name is poly-dextrose amine (1-4)-2-amino-B-D glucose, and molecular formula is following:
It is tasteless, odorless, nontoxicity.Active hydroxyl and amino are arranged in the chitosan macromole; They have stronger chemical reaction ability; Under given conditions; Chemical reactions such as hydrolysis, alkylation, acylations, carboxymethylation, sulfonation, nitrated, halogenation, oxidation, reduction, condensation and complexing can take place in chitosan, can generate various chitosan derivatives with different performance, and have good water-retentivity and chemicalstability.Through the anti-microbial activity of research chitosan and verivate thereof, oxidation-resistance, the ionogen adsorptive power is applied to fields such as life and medical science.Especially at medical field, chitosan and verivate thereof are widely used as the microcosmic medical material, as being used as medicament sustained-release matrix, hemostatic agent, base mateiral of artificial tissue and organ or the like.
LUTARALDEHYDE (GA); Molecular formula has 2 aldehyde radicals on
monomer whose; Act on thin base, hydroxyl, carboxyl and the amino of tropina; Can make it alkylation, cause that protein coagulating causes bacterial death to play the killing action to mikrobe.Therefore, LUTARALDEHYDE is as high effect disinfectants, is widely used in sterilization and sterilization, has the characteristics of wide spectrum, efficient, low toxicity.Though it has certain pungency to organism, under working concentration, pungency is little, corrodibility is low, can think safety and low toxicity.It also is the good linking agent of chemical crosslink reaction.But, little to metal protection, receive characteristics such as organic substance influence is little, good stability.
Polyoxyethylene glycol has another name called polymkeric substance, the polyoxyethylene (PEO-LS) of α-hydrogen-ω-hydroxyl (oxygen-1,2-second two bases).Be molecular-weight average in the general name of about 200 at least 6000 terepthaloyl moietie superpolymer.Along with the difference of molecular-weight average, character is also variant.The no color or smell thick liquid is to waxy solid.Water-soluble, ethanol and many other organic solvents.Steam forces down.To thermally-stabilised.Inoperative with many chemical, not hydrolysis is never degenerated.Nontoxic, eyes and skin there are not obvious stimulation.
Formaldehyde is a kind of colourless, and the gas of intense stimulus type smell is arranged.Soluble in water, pure and mild ether.Formaldehyde is gaseous state at normal temperatures, occurs with aqueous solution form usually.Soluble in water and ethanol, 35～40% formalin is called Superlysoform.Formaldehyde is a kind of important organic raw material, is mainly used in plastics industry, synthon, leather industry, medicine, dyestuff etc.
Magnetic nano-particle is that nanoparticle is by number atom or molecular former subgroup or molecular group seldom; Its particulate size is between 1-100nm; The characteristics that nanoparticle is different from body construction are: nanoparticle has shell structure; Because the upper layer of particle accounts for significant proportion, and surface atom is both not had long-range order, does not have the noncrystalline layer of SRO again; Can think that the virtual condition of particle surface layer is more near gaseous state; And, have the atom that the complete crystallization cycle arranges, but its structure is slightly different with the body sample in the heart portion of particle; The structure of this specific type of nanoparticle has caused it to have the effect of four aspects: surface effects, volume effect, quantum size effect and macro quanta tunnel effect, and produce many special propertys thus: unusual mechanics, electricity, magnetics, calorifics, optics and chemically reactive etc.Because magnetic nano-particle has its special paramagnetic characteristic, thereby has broad application prospects at aspects such as giant magnetoresistance, magnetic liquid and magnetic recording, soft magnetism, permanent magnetism, magnetic cooling, giant magnetic impedance material and magnetic-optic devices, magnetic detectors.
Hydrogel is to be dispersion medium with water, contains the crosslink polymer network structure of hydrophilic radical and hydrophobic group.As the high water-keeping material of a kind of high suction, hydrogel is widely used in the facial mask in the makeup of multiple field, defervescence plaster used, analgesia is pasted, and the preservation agent in the foodstuffs industry, thickening material, pharmaceutical carrier in the medical treatment or the like.
In burn treatment, the rehabilitation problem of patient's shaping and postoperative is the key in the therapeutic process.In the process of rehabilitation and scar treatment, be widely used stretch fabric and plastic mask are treated with pressure therapy.Because people's shape of face looks are complicated, height differs, even take pressure therapy can not obtain ideal results.
Summary of the invention
In order to overcome the deficiency of prior art, the object of the present invention is to provide a kind of chitosan derivatives hydrogel that contains magnetic nano-particle.
Another object of the present invention is to provide a kind of preparation method who contains the chitosan derivatives hydrogel of magnetic nano-particle.
To achieve these goals, technical scheme provided by the invention is following:
A kind of preparation method who contains the aquagel of magnetic nano-particle may further comprise the steps:
(1), the chitosan powder is dissolved in the acetic acid soln of 0.5%-5%, mechanical stirring is mixed with the chitosan solution of 0.002%-1% (being that the 0.002-1g chitosan is dissolved in the chitosan solution that 100m l acetum forms) until clarification, and is subsequent use.
(2), get the mixed solution 5-10mL of step (1), adding iron level is 1.2g/ml-1.4g/ml magnetic nano-particle dispersion liquid 200 μ L-1500 μ L;
(3), add linking agent 200uL-1000uL, react 2h-36h under the room temperature, schiff reaction takes place, generate the aquagel that contains magnetic nano-particle;
Described magnetic nano-particle is the ferriferrous oxide nano-particle that ROHM coats, and median size is 10nm-20nm;
Described linking agent is the LUTARALDEHYDE of 1wt%-25wt% or the mixed solution of polyoxyethylene glycol 0.05g-0.6g and formaldehyde (36wt%-40wt% stoste).Molecular weight polyethylene glycol Mw is respectively 10K and 20K.
Principle explanation: the amino that contains positively charged on the molecular chain of chitosan; And a large amount of electronegative carboxyls are contained on the ferriferrous oxide nano-particle surface that ROHM coats; Electrostatic adhesion takes place in both; Add linking agent LUTARALDEHYDE and chitosan then and schiff reaction takes place, crosslinked direct acquisition contains the hydrogel of nanoparticle; Perhaps add formaldehyde and chitosan generation schiff reaction earlier, form two keys of C=N, and then add polyoxyethylene glycol and gained Schiff's base generation addition reaction, obtain to contain the aquagel of nanoparticle, be brown, transparent, inner no obvious sediment and reunion.
Chitosan can be directly and the reaction of the mixed solution of linking agent LUTARALDEHYDE or formaldehyde and polyoxyethylene glycol make hydrogel, but owing to adopt acetate to make solvent, product has certain yellow, character is similar with silica gel, degree of crosslinking is bigger, its shearing modulus is high more, but frangible.
Description of drawings
The Electronic Speculum figure of the aquagel that contains magnetic nano-particle that Fig. 1 embodiment 1 obtains.Chitosan gel rubber after the freeze-drying is vesicular.
The Electronic Speculum figure of the aquagel that contains magnetic nano-particle that Fig. 2 embodiment 3 obtains.Same observation under the scale of 100 μ m is compared with embodiment 1, and along with the increase of LUTARALDEHYDE usage quantity, degree of crosslinking increases, and the freeze-drying structure porosity of chitosan gel rubber increases.
Embodiment
The ferriferrous oxide nano-particle that ROHM coats is available from Deco island gold Science and Technology Ltd.'s (median size is 10nm-20nm) in Beijing; Chitosan available from traditional Chinese medicines group (1, deacetylation is 80%-95%, molecular weight 590K-600K; 2, deacetylation>95%, molecular weight 280K-310K).
Embodiment 1
A kind of preparation method who contains the aquagel of magnetic nano-particle:
(1), 0.29g chitosan powder is dissolved in the acetic acid soln of 30mL 1%, to clarification, leave standstill 3h afterwards and remove bubble after the mechanical stirring 3h.And filter;
(2), in the resulting mixed solution of step (1), add 500 μ L and contain Fe
3O
4The dispersion liquid of nanoparticle (median size is 10nm-14nm) (iron level is 1.285mg/mL) shakes 1h again;
(3), the resulting mixed solution of step (2) is placed 40 ℃ of water-baths, to wherein dropwise dripping 1% glutaraldehyde solution totally 500 μ L, and impose mechanical stirring or concussion 3h, can obtain brown transparent aquagel.
Embodiment 2
The deacetylation of the chitosan powder that is to use in the step 1 with embodiment 1 difference>95%.
Embodiment 3
Be that with embodiment 1 difference step 3 drips 25% glutaraldehyde solution totally 200 μ L, and impose machinery concussion 10min, can obtain the transparent aquagel of brownish black.
The aquagel that adopts the embodiment of the invention 3 preparations is as the aux. pressure material in the burn treatment mask; According to the requirement of rehabilitation, generally need keep the 18mm mercury column at least, i.e. the stress of 2400Pa to the scar place; The chitosan gel rubber that embodiment 3 obtains glutaraldehyde cross-linking provides material as stress; The pressure that the 2500Pa that can load is above, if further improve degree of crosslinking, load still can continue to rise.Can make the mask people's face of more fitting, play the effect of further reinforcement pressure therapy.The adding of magnetic nano-particle can be played the effect of strengthening the gel mechanical property, simultaneously also can the initiation of outside magnetic field under, take place partially to gather partially, play controlled local enhanced effect.At last, according to the pressurized deformed state of hydrogel, feed back manufacturing in facial mould.
Embodiment 4
Be that with embodiment 1 difference step 2 adds 1000 μ L and contains Fe
3O
4Magnetic nano-particle; Obtain the transparent aquagel of brownish black.
Embodiment 5
Be that with embodiment 1 difference step 2 adds the 1500L adding and contains Fe
3O
4The aqueous solution of magnetic nano-particle, the transparent aquagel of acquisition brownish black, compare and embodiment 3 this moment, brown darker, reunites or deposition but have.
Embodiment 6
Be with embodiment 4 differences; In step 3, adding molecular-weight average is polyoxyethylene glycol (PEG) 0.2g of 10k; Machinery concussion 1h is above to add the formaldehyde reference liquid (36wt%-40wt%) of 0.3mL again to there not being deposition, can obtain brown, transparent chitosan composite aquogel.
Embodiment 7
Be in the step 3 with embodiment 6 differences, add the polyoxyethylene glycol M of 0.4g
n=20K, the transparent aquagel of acquisition brownish black.
Embodiment material that 8-10 adopts is as shown in table 1:
Table 1
Claims (4)
1. preparation method who contains the aquagel of magnetic nano-particle may further comprise the steps:
(1), the chitosan powder is dissolved in the acetic acid soln of 0.5%-5%, mechanical stirring is until clarification;
(2), get the mixed solution 5-10mL of step (1), adding iron level is 1.2g/ml-1.4g/ml magnetic nano-particle dispersion liquid 200uL-1500uL;
(3), add linking agent 200uL-1000uL, react 2h-36h under the room temperature, schiff reaction takes place, generate the aquagel that contains magnetic nano-particle.
2. the preparation method who contains the aquagel of magnetic nano-particle according to claim 1, the magnetic nano-particle that it is characterized in that described step (2) is the ferriferrous oxide nano-particle that ROHM coats.
3. the preparation method who contains the aquagel of magnetic nano-particle according to claim 1, the linking agent that it is characterized in that said step (3) is the LUTARALDEHYDE of 1wt%-25wt%.
4. the preparation method who contains the aquagel of magnetic nano-particle according to claim 1, the linking agent that it is characterized in that said step (3) is the mixed solution of polyoxyethylene glycol 0.05g-0.6g and formaldehyde.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105646902A (en) * | 2016-04-01 | 2016-06-08 | 江苏大学 | Preparation method of iron-chitosan metal supermolecular gel |
| CN108060158A (en) * | 2018-02-10 | 2018-05-22 | 成都理工大学 | A kind of chitosan magnetic carries the preparation method of denitrifying bacteria bead |
| CN108992702A (en) * | 2018-06-26 | 2018-12-14 | 东莞市联洲知识产权运营管理有限公司 | A kind of preparation method of porous nano oxide modifying chitosan medical aerogel dressing |
| CN109895131A (en) * | 2019-03-27 | 2019-06-18 | 江苏大学 | A kind of magnetic control software crawl robot based on magnetic programming temperature-sensitive hydrogel |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050064045A1 (en) * | 2003-09-18 | 2005-03-24 | Sheng-Ping Zhong | Injectable therapeutic formulations |
| CN1803275A (en) * | 2005-12-06 | 2006-07-19 | 青岛科技大学 | Novel silica gel loaded cross-linked chitosan adsorbent for heavy metal |
| CN101882496A (en) * | 2009-05-04 | 2010-11-10 | 杨琥 | Chitosan-polyacrylamide magnetic composite microsphere material, preparation method and application thereof |
| CN101892217A (en) * | 2010-06-02 | 2010-11-24 | 中国水产科学研究院黄海水产研究所 | Preparation method of magnetic chitosan compound microsphere immobilized marine alkaline proteinase |
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2012
- 2012-07-23 CN CN201210255353.7A patent/CN102766267B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050064045A1 (en) * | 2003-09-18 | 2005-03-24 | Sheng-Ping Zhong | Injectable therapeutic formulations |
| CN1803275A (en) * | 2005-12-06 | 2006-07-19 | 青岛科技大学 | Novel silica gel loaded cross-linked chitosan adsorbent for heavy metal |
| CN101882496A (en) * | 2009-05-04 | 2010-11-10 | 杨琥 | Chitosan-polyacrylamide magnetic composite microsphere material, preparation method and application thereof |
| CN101892217A (en) * | 2010-06-02 | 2010-11-24 | 中国水产科学研究院黄海水产研究所 | Preparation method of magnetic chitosan compound microsphere immobilized marine alkaline proteinase |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105646902A (en) * | 2016-04-01 | 2016-06-08 | 江苏大学 | Preparation method of iron-chitosan metal supermolecular gel |
| CN105646902B (en) * | 2016-04-01 | 2018-11-09 | 江苏大学 | A kind of preparation method of iron-chitosan-metal supermolecular gel |
| CN108060158A (en) * | 2018-02-10 | 2018-05-22 | 成都理工大学 | A kind of chitosan magnetic carries the preparation method of denitrifying bacteria bead |
| CN108992702A (en) * | 2018-06-26 | 2018-12-14 | 东莞市联洲知识产权运营管理有限公司 | A kind of preparation method of porous nano oxide modifying chitosan medical aerogel dressing |
| CN109895131A (en) * | 2019-03-27 | 2019-06-18 | 江苏大学 | A kind of magnetic control software crawl robot based on magnetic programming temperature-sensitive hydrogel |
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