CN103739856B - A kind of can from the preparation method of the hydrogel lyophilized powder of gelling - Google Patents
A kind of can from the preparation method of the hydrogel lyophilized powder of gelling Download PDFInfo
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Abstract
The invention discloses a kind of can from the preparation method of the hydrogel lyophilized powder of gelling, after the aqueous solution of the aqueous solution of chitosan and polyvinylpyrrolidone or its multipolymer is directly mixed, leave standstill 10 ~ 20 days, or under vacuum, leave standstill 3 ~ 5 days, then by lyophilize process, grinding obtains freeze-drying powder.Lyophilized powder prepared by the inventive method has good water-absorbent, and after absorbing moisture, rapid swelling condensation forms the hydrogel of monoblock.This lyophilized powder is used for the surface of a wound, can play the effect of hemostasis, and because the hydrogel formed has adaptivity, this lyophilized powder is applicable to the complex-shaped surface of a wound and cave type wound.Hydrogel lyophilized powder prepared by the inventive method is not owing to containing the components such as small molecule monomer, initiator, linking agent, and good biocompatibility, has larger superiority as dressing materials.
Description
Technical field
The invention belongs to biology medical material technical field, relate to a kind of can from the preparation method of the hydrogel lyophilized powder of gelling.
Background technology
Hydrogel material is that a class has hydrophilic radical and can be water-swellable but the water-fast polymkeric substance with three-dimensional net structure.Hydrogel can keep a large amount of moisture and very soft, be similar to bio-tissue, specifically good biocompatibility, tissue can be directly used in, thus be with a wide range of applications at biomedical sector, as can be used as fixing of Wound dressing, drug carrier material, medical coating, cell cultures base material, adherence preventing material and biological enzyme.
The preparation method of hydrogel has multiple, and being wherein cross-linked by monomer polymerization reactions is the most frequently used method, adopts the residual components such as the method weak point is small molecule monomer, initiator, linking agent to be difficult to remove completely.Prepare hydrogel by the interaction between macromole, can not small molecule monomer etc. be used, nontoxicity, good biocompatibility.Adopt the crosslinked technology preparing aerogel dressing of method of radiating generation to be applied between macromole to commercially produce.Radiation crosslinking weak point is the degraded that can cause molecular chain in the process of irradiation, saboteur's Structure and stability, adopts this technology to have limitation for the macromolecular material of easily degraded.
Also hydrogel can be formed by Physical interaction between macromole, Physical interaction can be electrostatic interaction, ionic interaction, hydrogen bond, hydrophobic interaction etc., the hydrogel formed has reversibility under certain condition, and physical action method has developed into a kind of novel method preparing hydrogel.Polyvinylpyrrolidone (PVP) is a kind of synthesis polymer with good biocompatibility, utilizes PVP to be combined with natural polymers such as chitosans the hydrogel preparing high-biocompatibility.Report and adopted radiation crosslinking and adopt the method for glutaraldehyde chemically crosslinked to prepare PVP-aquagel.Also molecular weight is not less than the PVP of K-60 through High Temperature High Pressure open loop process generation-COOH base to have document to point out, then with chitosan reaction, hydrogel is formed by both intermolecular hydrogen bond actions, if but polyvinylpyrrolidone does not do open loop process in the method, to be then difficult to directly and chitosan effect forms gel.
Summary of the invention
The object of the present invention is to provide a kind of can from the preparation method of the hydrogel lyophilized powder of gelling.
The technical solution used in the present invention is:
From a preparation method for the hydrogel lyophilized powder of gelling, can comprise the following steps:
1) chitosan is mixed with the aqueous solution, obtains solution A;
2) by polyvinylpyrrolidone or its multipolymer water-soluble, obtain solution B;
3) mixed solution A and solution B, room temperature leaves standstill 10 ~ 20 days, or under vacuum, leaves standstill 3 ~ 5 days, obtain gel system;
4) by after gel system precooling, lyophilize, grinding obtains lyophilized powder.
Preferably, in step 1), adjust pH to 1 ~ 6 with volatile acid, make chitosan water-soluble, obtained solution A.
Preferably, in solution A, the concentration of chitosan is 0.01 ~ 0.04g/mL.
Preferably, in solution B, the concentration of polyvinylpyrrolidone or its multipolymer is 0.1 ~ 0.4g/mL.
Preferably, the weight ratio of chitosan and polyvinylpyrrolidone or its multipolymer is 1:(8 ~ 15).
Preferably, in step 3), vacuum tightness is-0.5 ~-0.1MPa.
Preferably, in step 4), by gel system in-80 ~-20 DEG C of precoolings 10 ~ 24 hours.
Preferably, in step 4), the cryodesiccated time is 10 ~ 48 hours.
Preferably, polyvinylpyrrolidone multipolymer is at least one in the multipolymer of V-Pyrol RC and vinyl acetate, N, N dimethylamino methyl ethyl propenoate, quartenized vinyl imidazoles.
The invention has the beneficial effects as follows:
Lyophilized powder prepared by the inventive method has good water-absorbent, and after absorbing moisture, rapid swelling condensation forms the hydrogel of monoblock.Lyophilized powder can be used for the surface of a wound, is sprayed onto on the surface of a wound during use by lyophilized powder, and powder absorbs sepage or blood forms one deck hydrogel, plays the effect of hemostasis.This hydrogel has adaptivity, and therefore invention formulation is applicable to the complex-shaped surface of a wound and cave type wound.
Hydrogel lyophilized powder prepared by the inventive method is not owing to containing the components such as small molecule monomer, initiator, linking agent, and good biocompatibility, has larger superiority as dressing materials.Because lyophilized powder eliminates moisture, to preserve for a long time and unlikely rotten.
Embodiment
From a preparation method for the hydrogel lyophilized powder of gelling, can comprise the following steps:
1) chitosan is mixed with the aqueous solution, obtains solution A;
2) by polyvinylpyrrolidone or its multipolymer water-soluble, obtain solution B;
3) mixed solution A and solution B, room temperature leaves standstill 10 ~ 20 days, or under vacuum, leaves standstill 3 ~ 5 days, obtain gel system;
4) by after gel system precooling, lyophilize, grinding obtains lyophilized powder.
Preferably, in step 1), adjust pH to 1 ~ 6 with volatile acid, make chitosan water-soluble, obtained solution A.
Preferably, in solution A, the concentration of chitosan is 0.01 ~ 0.04g/mL.
Preferably, in solution B, the concentration of polyvinylpyrrolidone or its multipolymer is 0.1 ~ 0.4g/mL.
Preferably, the weight ratio of chitosan and polyvinylpyrrolidone or its multipolymer is 1:(8 ~ 15).
Preferably, in step 3), vacuum tightness is-0.5 ~-0.1MPa.
Preferably, in step 4), by gel system in-80 ~-20 DEG C of precoolings 10 ~ 24 hours.
Preferably, in step 4), the cryodesiccated time is 10 ~ 48 hours.
Preferably, polyvinylpyrrolidone multipolymer is at least one in the multipolymer of V-Pyrol RC and vinyl acetate, N, N dimethylamino methyl ethyl propenoate, quartenized vinyl imidazoles.
Vinylpyrrolidone polymer can be selected from PVP-K30, PVP-K60, PVP-K90, but is not limited thereto.
Studies have reported that and point out that PVP is through open loop process, crosslinking reaction can be carried out with chitosan and prepare hydrogel; If polyvinylpyrrolidone does not do open loop process, be then difficult to directly and chitosan effect.Contriver finds in research process, after the aqueous solution of the aqueous solution of chitosan and polyvinylpyrrolidone or its multipolymer is directly mixed, 10 ~ 20 days are left standstill in room temperature, or under vacuum, leave standstill 3 ~ 5 days, along with the volatilization of acetic acid etc., system pH rises, and finally can form the gel system of moisture softness; Further by this gel system by lyophilize process, obtain the spongy solid of fragility, grind and obtain thin freeze-drying powder.This powder has good water-absorbent, after absorbing moisture, rapid swelling condensation can form the hydrogel of monoblock.
Below in conjunction with embodiment, set forth content of the present invention further.
embodiment 1
1) be dispersed in 50mL deionized water by 2g chitosan, drip acetic acid under agitation condition, adjust pH to 6, leaving standstill the aqueous solution obtaining clear, is solution A;
2) under agitation condition, being dissolved in 160mL deionized water by 16g polyvinylpyrrolidone (PVP-K30), obtaining the aqueous solution of clear, is solution B;
3) mixed solution A and solution B, room temperature leaves standstill 14 days, obtains gel system;
4) by gel system in-30 DEG C of precoolings 10 hours, then lyophilize 15h, obtains the spongy solid of light yellow fragility, grinds and obtains thin freeze-drying powder.
embodiment 2
1) be dispersed in 100mL deionized water by 1g chitosan, drip hydrochloric acid under agitation condition, adjust pH to 3, leaving standstill the aqueous solution obtaining clear, is solution A;
2) under agitation condition, being dissolved in 40mL deionized water by 15g polyvinylpyrrolidone (PVP-K30), obtaining the aqueous solution of clear, is solution B;
3) mixed solution A and solution B, room temperature leaves standstill 10 days, obtains gel system;
4) by gel system in-20 DEG C of precoolings 24 hours, then lyophilize 10h, obtains the spongy solid of light yellow fragility, grinds and obtains thin freeze-drying powder.
embodiment 3
1) be dispersed in 100mL deionized water by 3g chitosan, drip hydrochloric acid under agitation condition, adjust pH to 1, leaving standstill the aqueous solution obtaining clear, is solution A;
2) under agitation condition, being dissolved in 150mL deionized water by 30g V-Pyrol RC-acetate copolymer, obtaining the aqueous solution of clear, is solution B;
3) mixed solution A and solution B, leaves standstill 5 days under-0.1MPa vacuum condition, obtains gel system;
4) by gel system in-60 DEG C of precoolings 15 hours, then lyophilize 24h, obtains the spongy solid of light yellow fragility, grinds and obtains thin freeze-drying powder.
embodiment 4
1) be dispersed in 100mL deionized water by 2g chitosan, drip hydrochloric acid under agitation condition, adjust pH to 4, leaving standstill the aqueous solution obtaining clear, is solution A;
2) under agitation condition, by 20g(vinyl pyrrolidone-N, N dimethylamino methyl ethyl propenoate cationic polymers (quaternary ammonium salt, PQ-11)) be dissolved in 80mL deionized water, obtaining the aqueous solution of clear, is solution B;
3) mixed solution A and solution B, leaves standstill 3 days under-0.5MPa vacuum condition, obtains gel system;
4) by gel system in-80 DEG C of precoolings 10 hours, then lyophilize 48h, obtains the spongy solid of light yellow fragility, grinds and obtains thin freeze-drying powder.
comparative example
1) 2g chitosan is dispersed in 49mL deionized water, under agitation condition, drips acetic acid, adjust pH to 6(with embodiment 1), leaving standstill the aqueous solution obtaining clear, is solution A;
2) under agitation condition, being dissolved in by 5gPVP-K30 in 45mL deionized water, obtaining the aqueous solution of clear, is solution B;
3) mixed solution A and solution B, in-30 DEG C of precoolings 10 hours, then in 0 DEG C of lyophilize, obtains the spongy solid of light yellow fragility, grinds and obtain thin freeze-drying powder.
The each 0.5g of lyophilized powder prepared by Example 1 ~ 4, sprays upper 4.5mL water respectively, all can form the hydrogel of monoblock, soak and do not dissolve for 1 day in 10min.Get lyophilized powder 0.5g prepared by comparative example, 4.5mL water in sprinkling, also can form hydrogel in 10min, but soaks gel structure after 1 day and start present unsetting and be partly dissolved.
Be contained in by lyophilized powder and can dust in the container at end, be sprayed onto on the surface of a wound, powder forms one deck hydrogel rapidly after absorbing the wound secretions such as a large amount of sepage, blood, can play the effect of hemostasis.The gel coat formed can comply with the shape of the surface of a wound, and has skin-adherent.Hydrogel can moisturizing, absorb wound exudate, promote wound healing.
Claims (8)
1. energy is from a preparation method for the hydrogel lyophilized powder of gelling, comprises the following steps:
1) chitosan is mixed with the aqueous solution, obtains solution A;
2) by polyvinylpyrrolidone or its multipolymer water-soluble, obtain solution B;
3) mixed solution A and solution B, room temperature leaves standstill 10 ~ 20 days, or under vacuum, leaves standstill 3 ~ 5 days, obtain gel system;
4) by after gel system precooling, lyophilize, grinding obtains lyophilized powder;
It is characterized in that: the weight ratio of chitosan and polyvinylpyrrolidone or its multipolymer is 1:(8 ~ 15).
2. preparation method according to claim 1, is characterized in that: in step 1), adjusts pH to 1 ~ 6, make chitosan water-soluble, obtained solution A with volatile acid.
3. preparation method according to claim 2, is characterized in that: in solution A, and the concentration of chitosan is 0.01 ~ 0.04g/mL.
4. preparation method according to claim 1, is characterized in that: in solution B, and the concentration of polyvinylpyrrolidone or its multipolymer is 0.1 ~ 0.4g/mL.
5. preparation method according to claim 1, is characterized in that: in step 3), and vacuum tightness is-0.5 ~-0.1MPa.
6. preparation method according to claim 1, is characterized in that: in step 4), by gel system in-80 ~-20 DEG C of precoolings 10 ~ 24 hours.
7. the preparation method according to claim 1 or 6, is characterized in that: in step 4), and the cryodesiccated time is 10 ~ 48 hours.
8. preparation method according to claim 1, is characterized in that: polyvinylpyrrolidone multipolymer is at least one in the multipolymer of V-Pyrol RC and vinyl acetate, N, N dimethylamino methyl ethyl propenoate, quartenized vinyl imidazoles.
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| CN109529094A (en) * | 2018-11-05 | 2019-03-29 | 首都师范大学 | A kind of efficient hemostatic material and preparation method thereof can promote wound healing |
| CN113429724A (en) * | 2021-06-22 | 2021-09-24 | 广东省科学院健康医学研究所 | Hydrogel of lubricating coating, preparation method of hydrogel, hydrogel freeze-dried powder and application |
| CN113563611B (en) * | 2021-07-16 | 2022-09-06 | 浙江大学 | Biocompatible hydrogel dry powder and preparation method and application thereof |
| CN113893386B (en) * | 2021-10-27 | 2022-06-03 | 四川大学华西医院 | Spray-coated dry powder gel dressing and preparation method thereof |
| CN115010981B (en) * | 2022-06-24 | 2023-12-05 | 遵义医科大学附属口腔医院 | Solid product containing amino indissolvable polymer, preparation method and application thereof |
| CN115845121A (en) * | 2022-12-07 | 2023-03-28 | 华南理工大学 | Hemostatic, antibacterial and healing promoting microgel assembly powder and preparation method thereof |
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| CN101664562A (en) * | 2009-09-30 | 2010-03-10 | 都本立 | Wound repair hydrogel material and preparation method thereof |
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Address after: No. 1307, Guangzhou Avenue middle, Tianhe District, Guangzhou, Guangdong 510500 Patentee after: Institute of health medicine, Guangdong Academy of Sciences Address before: No. 1307, Guangzhou Avenue middle, Tianhe District, Guangzhou, Guangdong 510500 Patentee before: GUANGDONG INSTITUTE OF MEDICAL INSTRUMENTS |
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Address after: No.10, shiliugang Road, Haizhu District, Guangzhou City, Guangdong Province 510000 Patentee after: Institute of biological and medical engineering, Guangdong Academy of Sciences Address before: No. 1307, Guangzhou Avenue middle, Tianhe District, Guangzhou, Guangdong 510500 Patentee before: Institute of health medicine, Guangdong Academy of Sciences |