CN103013106A - Preparation method of gamma-polyglutamic acid/Pulullan composite hydrogel - Google Patents
Preparation method of gamma-polyglutamic acid/Pulullan composite hydrogel Download PDFInfo
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- CN103013106A CN103013106A CN2013100084892A CN201310008489A CN103013106A CN 103013106 A CN103013106 A CN 103013106A CN 2013100084892 A CN2013100084892 A CN 2013100084892A CN 201310008489 A CN201310008489 A CN 201310008489A CN 103013106 A CN103013106 A CN 103013106A
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Abstract
The invention provides a preparation method of a gamma-polyglutamic acid/Pulullan composite hydrogel. The hydrogel contains gamma-polyglutamic acid, Pulullan and water. The preparation method comprises the following steps: dissolving 8-20% of gamma-polyglutamic acid in distilled water to obtain a first reaction solution; adding Pulullan according to different gamma-polyglutamic acid/Pulullan ratios to obtain a second reaction solution; and adding a crosslinking agent into the second reaction solution, stirring uniformly, regulating the pH value of the system, and reacting at 50 DEG C for 24 hours. The gamma-polyglutamic acid/Pulullan composite hydrogel prepared by the method has favorable adsorbability for brine. The hydrogel is applicable to a brine environment, and is especially applicable to an environment of soil, sweat, blood or the like.
Description
Technical field
The present invention relates to the composite aquogel field, be specifically related to a kind of gamma-polyglutamic acid-/pulullan polysaccharide composite aquogel and preparation method thereof.
Background technology
Gamma-polyglutamic acid-is by the synthetic a kind of extracellular biopolymer aminoacid polymers of microorganism, through chemical cross-linking agent, gamma-radiation irradiation or the crosslinked water absorbent gel with three-dimensional net structure that forms of other modes, have the performances such as water-absorbent, water absorbability and water conservation, can absorb the water yield of hundreds of times to thousands of times of sole masses, expand after the suction, moisture can not sloughed after the pressurization, also has recyclability and biodegradable performance, is a kind of water-retentivity material to the physical environment close friend.Can be applicable to the fields such as agricultural, food, makeup, sanitary product, biomedicine.
But find generally that in use hydrogel can arrive thousands of times to the absorption of pure water, but when it come to arrives salt solution, its receptivity fast-descending.In actual application, in most cases all be in the certain density ionic environment, therefore improving hydrogel is a problem that needs to be resolved hurrily to the absorptive character of solion.
Composite is crosslinked to be to improve gamma-polyglutamic-acid hydrogel performance simple and efficient way, it also is the focus of gamma-polyglutamic-acid hydrogel research, wherein a kind of blend method is that 10% gamma-polyglutamic acid-reaction solution is joined polyacrylamide and N, N ' methylene-bisacrylamide proportioning is in 29: 1 the reaction soln, add promotor and initiator, vacuumize, radical polymerization obtains semi-interpenetrating network aqueous gel.Show the susceptibility to pH and temperature, but salt tolerance not mentioned (Materials Letters, 2006,60:1390-1393).Another kind of blend method is that carboxyl on chitosan amido and the gamma-polyglutamic acid-is by [NH
2]: [COOH]=75: 25,50: 50,25: 75 mol ratio preparation chitosan and gamma-polyglutamic acid-mixing solutions, the acetic acid solution of adding 1%, by-NH
2And-COOH between complicated deacetylation obtain the polyelectrolyte hydrogel, this gel to intestinal bacteria and streptococcus aureus show anti-microbial activity (Carbohydrate Research, 2010,345:1774-1780).Also having a kind of method is that gamma-polyglutamic acid-is mixed by 1: 1,2: 3,3: 7,1: 4,1: 9 proportioning respectively with polyvinyl alcohol, centrifugal 5min under the 3000rpm, form gel by the hydrogen bond action between the macromolecular chain, plural gel has better thermostability, mechanical property and blood compatibility (Colloids and Surfaces B:Biointerfaces than pure polyvinyl alcohol gel, 2006,47:43-49).
The reaction conditions of the needs complexity that these preparation methods have and preparation manipulation process, what have then exists defective aspect performance and the intensity, and the salt tolerance of gamma-polyglutamic acid-plural gel all is not significantly improved.
Summary of the invention
The invention provides a kind of gamma-polyglutamic acid-/pulullan polysaccharide composite aquogel.
The present invention also provides the preparation method of a kind of gamma-polyglutamic acid-/pulullan polysaccharide composite aquogel.The method of concrete preparation comprises: take by weighing a certain amount of gamma-polyglutamic acid-and be dissolved in the distilled water, obtain 8-20% gamma-polyglutamic acid-the first reaction soln; By gamma-polyglutamic acid-and pulullan polysaccharide mass ratio 0.5-4: 1 proportioning adds pulullan polysaccharide in the first reaction soln, obtains the second reaction soln; Add linking agent in the second reaction soln, dosage of crosslinking agent is the 40%-60% of gamma-polyglutamic acid-consumption, stirs, and conditioned reaction pH value of solution environment is 2-12, reacts 24h under 50 ℃ of constant temperatures; After reaction finishes the hydrogel that forms is taken out.
The present invention utilizes the non-ionic hydrophilic hydroxyl on the biopolymer pulullan polysaccharide molecular chain, improves the absorbency of gamma-polyglutamic-acid hydrogel in salt solution.Have simple to operately, reaction conditions is easy to control, and the material requested safety and environmental protection is the advantage of degraded easily.The hydrogel that is made by the present invention is applicable to the occasion that not only requires hydrogel to have certain water-absorbent and have salt tolerance, biocompatibility concurrently, is particularly useful for the fields such as pharmaceutical carrier, wound dressing, plant water keeping agent.
Specific implementation method
Embodiment 1: gamma-polyglutamic acid-1.6g, add water 18.4g, and fully stir, then add pulullan polysaccharide 3.2g, ethylene glycol diglycidylether 1.28g, fully stirring and dissolving conditioned reaction liquid pH is 4,50 ℃ of lower isothermal reaction 24h.Take out hydrogel and be dissolved in the physiological saline, swelling equilibrium, water absorbent rate are 53 times.
Embodiment 2: gamma-polyglutamic acid-3.2g, add water 16.8g, and fully stir, then add pulullan polysaccharide 1.6g, ethylene glycol diglycidylether 1.28g, fully stirring and dissolving conditioned reaction liquid pH is 6,50 ℃ of lower isothermal reaction 24h.Take out hydrogel and be dissolved in the distilled water, swelling equilibrium, water absorbent rate are 260 times.
Embodiment 3: gamma-polyglutamic acid-3.2g, add water 16.8g, and fully stir, then add pulullan polysaccharide 6.4g, ethylene glycol diglycidylether 1.92g, fully stirring and dissolving conditioned reaction liquid pH is 4,50 ℃ of lower isothermal reaction 24h.Take out hydrogel and be dissolved in the physiological saline, swelling equilibrium, water absorbent rate are 37 times.
Embodiment 4: gamma-polyglutamic acid-3.2g, add water 16.8g, and fully stir, then add pulullan polysaccharide 3.2g, ethylene glycol diglycidylether 1.28g, fully stirring and dissolving conditioned reaction liquid pH is 8,50 ℃ of lower isothermal reaction 24h.Take out hydrogel and be dissolved in the physiological saline, swelling equilibrium, water absorbent rate are 130 times.
Embodiment 5: gamma-polyglutamic acid-3.2g, add water 23.5g, and fully stir, then add pulullan polysaccharide 1.6g, ethylene glycol diglycidylether 1.6g, fully stirring and dissolving conditioned reaction liquid pH is 2,50 ℃ of lower isothermal reaction 24h.Take out hydrogel and be dissolved in the physiological saline, swelling equilibrium, water absorbent rate are 149 times.
Embodiment 6: gamma-polyglutamic acid-6.4g, add water 25.6g, and fully stir, then add pulullan polysaccharide 1.6g, ethylene glycol diglycidylether 1.28g, fully stirring and dissolving conditioned reaction liquid pH is 12,50 ℃ of lower isothermal reaction 24h.Take out hydrogel and be dissolved in the physiological saline, swelling equilibrium, water absorbent rate are 160 times.
Claims (8)
1. gamma-polyglutamic acid-/pulullan polysaccharide composite aquogel contains gamma-polyglutamic acid-, pulullan polysaccharide and water.
2. preparation of gels method according to claim 1 comprises the steps:
Get gamma-polyglutamic acid-and be dissolved in the distilled water, obtain gamma-polyglutamic acid-the first reaction soln; By gamma-polyglutamic acid-and pulullan polysaccharide mass ratio 0.5-4: 1 proportioning adds pulullan polysaccharide in the first reaction soln, obtains the second reaction soln; Add linking agent in the second reaction soln, stir, conditioned reaction pH value of solution environment is 2-12, reacts 24h under 50 ℃ of constant temperatures; After reaction finishes the hydrogel that forms is taken out.
3. preparation method according to claim 2 is characterized in that, described gamma-polyglutamic acid-concentration is 8-20%.
4. preparation method according to claim 2 is characterized in that, the mass ratio of described gamma-polyglutamic acid-and pulullan polysaccharide is 1: 2,1: 1,2: 1,3: 1 or 4: 1.
5. preparation method according to claim 2 is characterized in that, described linking agent is ethylene glycol diglycidylether.
According to claim 2 with 5 described preparation methods, it is characterized in that the consumption of described linking agent ethylene glycol diglycidylether is the 40%-60% of gamma-polyglutamic acid-consumption.
7. according to claim 2,5 and 6 described preparation methods, it is characterized in that described temperature of reaction is 50 ℃.
8. according to claim 2,5,6,7 described preparation methods, it is characterized in that the described reaction times is 24h.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103301504A (en) * | 2013-06-28 | 2013-09-18 | 天津工业大学 | Preparation method of gamma-polyglutamate/sericin hydrogel dressing |
| CN104606680A (en) * | 2014-12-29 | 2015-05-13 | 天津北洋百川生物技术有限公司 | Preparation method of drug-loaded gamma-polyglutamic acid hydrogel |
| CN104771780A (en) * | 2015-04-09 | 2015-07-15 | 中国工程物理研究院核物理与化学研究所 | Polymeric hydrogel for dressing and preparation method of polymeric hydrogel |
| CN104857560A (en) * | 2015-05-26 | 2015-08-26 | 西北大学 | Injectable hydrogel prepared from carboxylated pullulan and preparation method of injectable hydrogel |
| CN105199112A (en) * | 2014-06-10 | 2015-12-30 | 天津工业大学 | Preparation method of high-strength gamma-polyglutamic acid hydrogel |
| CN105544096A (en) * | 2015-12-07 | 2016-05-04 | 天津北洋百川生物技术有限公司 | Method improving water stability of polyglutamic acid-Pullulan nanometer fiber film |
| CN108478846A (en) * | 2018-04-20 | 2018-09-04 | 薛春玲 | A kind of medical hemostatic antiseptic dressing and preparation method thereof |
| CN108553681A (en) * | 2018-04-24 | 2018-09-21 | 江西省科学院应用化学研究所 | A kind of hemostasis medical dressing and preparation method thereof |
| CN110092922A (en) * | 2019-05-31 | 2019-08-06 | 成都金开生物工程有限公司 | A kind of preparation method of gamma-polyglutamic acid plural gel |
| CN110878145A (en) * | 2019-11-29 | 2020-03-13 | 浙江树人学院（浙江树人大学） | Preparation method of okra extract gamma-polyglutamic acid gel nanoparticles |
| CN110903501A (en) * | 2019-11-29 | 2020-03-24 | 浙江树人学院（浙江树人大学） | Preparation method and application of gamma-polyglutamic acid gel nanoparticles |
| CN111068627A (en) * | 2019-11-29 | 2020-04-28 | 温州医科大学 | Polydopamine/pullulan composite hydrogel as well as preparation method and application thereof |
| CN112430336A (en) * | 2018-06-07 | 2021-03-02 | 天津工业大学 | Application of superfine bacterial cellulose powder in preparation of hydrogel |
| CN112625265A (en) * | 2020-12-01 | 2021-04-09 | 扬州大学 | Preparation method of high-strength gamma-PGA modified PVA composite hydrogel |
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| CN101891954A (en) * | 2010-06-23 | 2010-11-24 | 南开大学 | Method for preparing polyglutamic acid hydrogel |
| CN102321256A (en) * | 2011-09-06 | 2012-01-18 | 南开大学 | Biocompatibility gamma-polyglutamic acid-hydrogel preparation method |
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2013
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Patent Citations (2)
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| CN101891954A (en) * | 2010-06-23 | 2010-11-24 | 南开大学 | Method for preparing polyglutamic acid hydrogel |
| CN102321256A (en) * | 2011-09-06 | 2012-01-18 | 南开大学 | Biocompatibility gamma-polyglutamic acid-hydrogel preparation method |
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103301504A (en) * | 2013-06-28 | 2013-09-18 | 天津工业大学 | Preparation method of gamma-polyglutamate/sericin hydrogel dressing |
| CN107325301B (en) * | 2014-06-10 | 2020-05-29 | 天津工业大学 | High-strength gamma-polyglutamic acid hydrogel |
| CN105199112A (en) * | 2014-06-10 | 2015-12-30 | 天津工业大学 | Preparation method of high-strength gamma-polyglutamic acid hydrogel |
| CN107325301A (en) * | 2014-06-10 | 2017-11-07 | 天津工业大学 | A kind of high intensity γ polyglutamic acid hydrogels |
| CN105199112B (en) * | 2014-06-10 | 2017-12-26 | 天津工业大学 | A kind of preparation method of high intensity γ polyglutamic acid hydrogels |
| CN104606680A (en) * | 2014-12-29 | 2015-05-13 | 天津北洋百川生物技术有限公司 | Preparation method of drug-loaded gamma-polyglutamic acid hydrogel |
| CN104771780A (en) * | 2015-04-09 | 2015-07-15 | 中国工程物理研究院核物理与化学研究所 | Polymeric hydrogel for dressing and preparation method of polymeric hydrogel |
| CN104771780B (en) * | 2015-04-09 | 2017-04-12 | 中国工程物理研究院核物理与化学研究所 | Preparation method for polymeric hydrogel for dressing |
| CN104857560A (en) * | 2015-05-26 | 2015-08-26 | 西北大学 | Injectable hydrogel prepared from carboxylated pullulan and preparation method of injectable hydrogel |
| CN105544096A (en) * | 2015-12-07 | 2016-05-04 | 天津北洋百川生物技术有限公司 | Method improving water stability of polyglutamic acid-Pullulan nanometer fiber film |
| CN108478846A (en) * | 2018-04-20 | 2018-09-04 | 薛春玲 | A kind of medical hemostatic antiseptic dressing and preparation method thereof |
| CN108553681A (en) * | 2018-04-24 | 2018-09-21 | 江西省科学院应用化学研究所 | A kind of hemostasis medical dressing and preparation method thereof |
| CN112430336A (en) * | 2018-06-07 | 2021-03-02 | 天津工业大学 | Application of superfine bacterial cellulose powder in preparation of hydrogel |
| CN112430336B (en) * | 2018-06-07 | 2021-10-08 | 天津工业大学 | Application of superfine bacterial cellulose powder in preparation of hydrogel |
| CN110092922A (en) * | 2019-05-31 | 2019-08-06 | 成都金开生物工程有限公司 | A kind of preparation method of gamma-polyglutamic acid plural gel |
| CN110878145A (en) * | 2019-11-29 | 2020-03-13 | 浙江树人学院（浙江树人大学） | Preparation method of okra extract gamma-polyglutamic acid gel nanoparticles |
| CN110903501A (en) * | 2019-11-29 | 2020-03-24 | 浙江树人学院（浙江树人大学） | Preparation method and application of gamma-polyglutamic acid gel nanoparticles |
| CN111068627A (en) * | 2019-11-29 | 2020-04-28 | 温州医科大学 | Polydopamine/pullulan composite hydrogel as well as preparation method and application thereof |
| CN110903501B (en) * | 2019-11-29 | 2022-04-15 | 浙江树人学院（浙江树人大学） | Preparation method and application of gamma-polyglutamic acid gel nanoparticles |
| CN112625265A (en) * | 2020-12-01 | 2021-04-09 | 扬州大学 | Preparation method of high-strength gamma-PGA modified PVA composite hydrogel |
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Application publication date: 20130403 |