CN103937009A - Preparing method of chitosan hydrogel - Google Patents
Preparing method of chitosan hydrogel Download PDFInfo
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- CN103937009A CN103937009A CN201310023246.6A CN201310023246A CN103937009A CN 103937009 A CN103937009 A CN 103937009A CN 201310023246 A CN201310023246 A CN 201310023246A CN 103937009 A CN103937009 A CN 103937009A
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- chitosan
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- glutaraldehyde
- chitosan hydrogel
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- 229920001661 Chitosan Polymers 0.000 title claims abstract description 55
- 239000000017 hydrogel Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title abstract 4
- 230000008961 swelling Effects 0.000 claims abstract description 27
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000002360 preparation method Methods 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 3
- 239000002977 biomimetic material Substances 0.000 abstract description 2
- 239000003814 drug Substances 0.000 abstract description 2
- 238000001879 gelation Methods 0.000 abstract 2
- 239000003431 cross linking reagent Substances 0.000 abstract 1
- 229940079593 drug Drugs 0.000 abstract 1
- 239000000499 gel Substances 0.000 description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 238000004132 cross linking Methods 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- KIUKXJAPPMFGSW-DNGZLQJQSA-N (2S,3S,4S,5R,6R)-6-[(2S,3R,4R,5S,6R)-3-Acetamido-2-[(2S,3S,4R,5R,6R)-6-[(2R,3R,4R,5S,6R)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylic acid Chemical compound CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 KIUKXJAPPMFGSW-DNGZLQJQSA-N 0.000 description 1
- SQDAZGGFXASXDW-UHFFFAOYSA-N 5-bromo-2-(trifluoromethoxy)pyridine Chemical compound FC(F)(F)OC1=CC=C(Br)C=N1 SQDAZGGFXASXDW-UHFFFAOYSA-N 0.000 description 1
- 229920001817 Agar Polymers 0.000 description 1
- 229920002101 Chitin Polymers 0.000 description 1
- 229920001287 Chondroitin sulfate Polymers 0.000 description 1
- 239000004971 Cross linker Substances 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 244000061456 Solanum tuberosum Species 0.000 description 1
- 235000002595 Solanum tuberosum Nutrition 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 239000008272 agar Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229940059329 chondroitin sulfate Drugs 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229920006037 cross link polymer Polymers 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 230000006196 deacetylation Effects 0.000 description 1
- 238000003381 deacetylation reaction Methods 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 229920002674 hyaluronan Polymers 0.000 description 1
- 229960003160 hyaluronic acid Drugs 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a preparing method of chitosan hydrogel. According to the method, chitosan is used as a raw material, glutaraldehyde is used as a crosslinking agent, and the chitosan hydrogel is synthesized in an acetic acid solution. Process conditions for preparing the chitosan hydrogel are optimized through orthogonal experiments. Experiment results show that: when the concentration of the chitosan is 3%, the concentration of the glutaraldehyde is 3% and the gelation temperature is 55 DEG C, the hardness of the prepared chitosan hydrogel is the maximum; and when the concentration of the chitosan is 2%, the concentration of the glutaraldehyde is 1% and the gelation temperature is 45 DEG C, the swelling degree of the prepared chitosan hydrogel is the maximum. The chitosan hydrogel has good biological compatibility, and therefore the chitosan hydrogel has broad application prospects in the fields of drug release systems, biomimetic materials, chemical mechanical systems, and the like.
Description
1, technical field
The present invention belongs to chemistry by International Patent Classification (IPC) (IPC); Ministry of Metallurgical Industry, chemical branch, organic high molecular compound; Its preparation or chemical process; The large class of composition taking it as base-material, polyose; Its derivative group, chitin; Chondroitin sulfate; Hyaluronic acid; The technical field of their derivative group.
2, background technology
Hydrogel is a kind of high molecular polymer with three-dimensional structure, forms by hydrophilic macromolecular compound is crosslinked, can be in water swelling and keep large quantity of moisture and don't dissolving.Meanwhile, there is good biocompatibility, thereby have broad application prospects in fields such as drug delivery system, biomimetic material, chemical machinery systems.
Chitosan wide material sources, cheap and easy to get, and there is good biocompatibility, security and biological degradability, be the ideal material of preparing hydrogel.In the time thering is the cross-linked polymer of tridimensional network and solvent phase mutual effect, occur swellingly, owing to thering is crosslinking structure, its swelling behavior is restricted.Swelling degree is decided by cross-linking density, and cross-linking density is higher, and swelling capacity is less.Chitosan, because of its characteristic that has softness intensity difference, is unable to undergo weight.In addition, it also has the shortcomings such as character volatile, gel is very unstable compared with the mechanically resistant materials such as metal.Therefore, hardness and the swelling capacity of research chitosan, be the widespread use of chitosan gel, and synthesized high-performance chitosan based aquagel is laid a good foundation.
3, summary of the invention
3.1 experimental section
3.1.1 instrument and medicine
HHS type electric-heated thermostatic water bath, JA5003 type electronic balance, 10222A type digital display electric drying oven with forced convection, QTS225Texture Aualyser (Britain), FUHUA HZ22C constant incubator, microscope, blood counting chamber; Chitosan (biochemical reagents), glutaraldehyde (AR), Glacial acetic acid (AR), potato, glucose, agar, candiyeast.
3.1.2 the preparation of chitosan hydrogel
Accurately take 1.0g chitosan in clean beaker, add 40mL2% acetum, stirring and dissolving; Add 16mL2% glutaraldehyde, stir, 50 DEG C of constant temperature 1h obtain yellow transparent chitosan hydrogel; Room temperature is placed 48h and is obtained yellow transparent chitosan hydrogel.
3.1.3 the mensuration of sewlling ration
Accurately take 2g left and right gel, be dipped to swelling equilibrium in distilled water, elimination excessive moisture, blots its surface-moisture with filter paper, weighs, with following formula calculation sample sewlling ration.
In formula: the sewlling ration (%) that SR is hydrogel; Ws is the quality (g) of gel reach swelling equilibrium in distilled water time; Wd is gel quality (g) while not soaking.
3.1.4 gel hardness test
Cylindrical probe (diameter is 10mm) on QTS225TextureAualyser declines with the speed of 15cm/s, when from gel surface when pressing down 6mm, record gel hardness (g).Sample test 3 times, gets its mean value.
3.1.5 the mensuration of gel biological compatibility
In chitosan solution, add 1.0mL7.68 × 10
8individual yeast/mL candiyeast bacteria suspension, add glutaraldehyde solution again, gel under room temperature, with sterilized water soaks after placing 24h in 28 DEG C of constant incubators, shakes 1h in constant-temperature table; Get supernatant liquor 1mL and be inoculated on yeast solid substratum, in 28 DEG C of constant incubators, carry out microorganism culturing, observe its colony growth situation.
4, brief description of the drawings
Accompanying drawing has mainly been narrated the concentration of chitosan, concentration and the impact of temperature on hydrogel hardness and swelling capacity of glutaraldehyde, with and biocompatibility:
Fig. 1: the impact of chitosan concentration on gel hardness and swelling capacity;
Fig. 2: the impact of glutaraldehyde concentration on gel hardness and swelling capacity;
Fig. 3: the impact of gelling temp on hardness and swelling capacity;
Fig. 4: candiyeast colony growth situation.
5, Analysis of conclusion
Below in conjunction with above-mentioned accompanying drawing, chitosan hydrogel preparation method of the present invention is described further:
5.1 chitosan concentration
The concentration of glutaraldehyde is 2%, gelling temp is 50 DEG C, and preparation chitosan concentration is respectively 1%, 2%, 3%, 4%, 5%, 6% chitosan solution 40mL, adds 2% glutaraldehyde 16mL, 1h in 50 DEG C of constant temperature water baths, measures gel hardness after placing 24h under room temperature; Take the each 2g of the chitosan hydrogel of preparing under similarity condition left and right simultaneously, be soaked in distilled water to swelling equilibrium, measure its equilibrium swelling degree, chitosan concentration on the impact of gel hardness and swelling capacity as shown in Figure 1.
As shown in Figure 1, hydrogel hardness increases maximum in the time that chitosan concentration is 6% along with the increase of chitosan concentration; And swelling capacity is to reduce along with the increase of chitosan concentration.Reason is the increase along with chitosan concentration, and chitosan interchain has formed cohesion tangled structure, and this tangled structure causes by the hydrogen bond association structure forming between the light side group of chitosan interchain, and its effect is similar to the cross-linking set in cross-linked network structure.In the time that chitosan concentration increases, the interior chitosan molecule number of unit volume increases, and form interchain hydrogen bond and condense the increase of counting out of tangling, that is degree of crosslinking increase, therefore swelling capacity reduces.
5.2 glutaraldehyde concentration
Prepare 3% chitosan solution 40mL, add respectively concentration to be respectively 0.5%, 1.0%, 1.5%, 2%, 2.5%, 3% glutaraldehyde solution 16mL, 1h in 50 DEG C of constant temperature water baths, measures gel hardness after placing 24h under room temperature; Take the each 2g of the chitosan hydrogel of preparing under similarity condition left and right simultaneously, be soaked in distilled water to swelling equilibrium, measure its equilibrium swelling degree, glutaraldehyde concentration on the impact of gel hardness and swelling capacity as shown in Figure 2.
As shown in Figure 2, the hardness of hydrogel is along with crosslinker concentration increases and increases.Reason is that this deacetylation of testing raw material chitosan used is 92.67%, therefore there is a large amount of amino on chitosan molecular chain, increase linking agent glutaraldehyde concentration, make the crosslinked aggravation between chitosan molecular chain, it is finer and close that network structure becomes, thereby gel hardness is along with linking agent glutaraldehyde concentration increases and increases; And network structure becomes the more fine and close resistance increasing that also can make water molecules enter gel structure, hydrophilic radical on chitosan molecular chain is difficult to contact with water molecules, the stretching, extension of gel macromolecule network is restricted, thereby causes swelling capacity to reduce along with the increase of glutaraldehyde concentration.
5.3 gelling temp
Prepare 3% chitosan solution 40mL, adding concentration is 2% glutaraldehyde solution 16mL, stirs and is placed in 30 DEG C, 35 DEG C, 40.℃、45℃、50。DEG C and the constant temperature water bath of 55 DEG C in 1h, under room temperature, place 24h, measure gel hardness and swelling capacity, to study the impact of gelling temp on hardness and swelling capacity, experimental result is as shown in Figure 3.
As seen from Figure 3, hydrogel hardness is first to reduce along with the rising of gelling temp, then increases, hardness maximum 55 DEG C time; And swelling capacity first increases along with the rising of gelling temp, then reduce, 40 DEG C time, swelling behavior degree is the highest; But gelling temp is little to hardness, swelling capacity influence degree.
5.4 biocompatibility
The chitosan hydrogel of embedding candiyeast is immersed in sterilized water, gets 1mL supernatant liquor and be inoculated in yeast culture base, cultivate 2～3d in 28 DEG C of constant incubators, media surface grows shallow milk yellow candiyeast bacterium colony, and experimental result as shown in Figure 4.This result shows, chitosan hydrogel has good biocompatibility, and microorganism cells is not had to toxic action.
Claims (2)
1. the preparation method of chitosan hydrogel of the present invention, is taking chitosan as raw material, as linking agent, synthesizes chitosan hydrogel by glutaraldehyde in acetum.
2. according to claim 1, the processing condition of chitosan hydrogel of preparation highest hardness are: chitosan concentration is 3%, glutaraldehyde concentration is 3%, gelling temp is 55 DEG C; The processing condition of preparing the chitosan hydrogel of maximum swelling degree are: chitosan concentration is 2%, glutaraldehyde concentration is 1%, gelling temp is 45 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310023246.6A CN103937009A (en) | 2013-01-18 | 2013-01-18 | Preparing method of chitosan hydrogel |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310023246.6A CN103937009A (en) | 2013-01-18 | 2013-01-18 | Preparing method of chitosan hydrogel |
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| Publication Number | Publication Date |
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| CN103937009A true CN103937009A (en) | 2014-07-23 |
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| CN201310023246.6A Pending CN103937009A (en) | 2013-01-18 | 2013-01-18 | Preparing method of chitosan hydrogel |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018000486A1 (en) * | 2016-06-28 | 2018-01-04 | 深圳市阳光之路生物材料科技有限公司 | Joint lubricant and manufacturing method thereof |
| 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 |
-
2013
- 2013-01-18 CN CN201310023246.6A patent/CN103937009A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018000486A1 (en) * | 2016-06-28 | 2018-01-04 | 深圳市阳光之路生物材料科技有限公司 | Joint lubricant and manufacturing method thereof |
| 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 |
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Application publication date: 20140723 |