CN102477590A - Electrostatic spinning method of low molecular weight collagen peptide and chitosan oligosacchaides biological membrane - Google Patents
Electrostatic spinning method of low molecular weight collagen peptide and chitosan oligosacchaides biological membrane Download PDFInfo
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- CN102477590A CN102477590A CN2010105566474A CN201010556647A CN102477590A CN 102477590 A CN102477590 A CN 102477590A CN 2010105566474 A CN2010105566474 A CN 2010105566474A CN 201010556647 A CN201010556647 A CN 201010556647A CN 102477590 A CN102477590 A CN 102477590A
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Abstract
The invention relates to an electrostatic spinning method of a low molecular weight collagen peptide and chitosan oligosacchaides biological membrane, wherein appropriate hydrophile carrier high polymer polyvinyl alcohol (PVA) is added to low molecular weight collagen peptide/ chitosan oligosacchaides solution to prepare collagen peptide/chitosan oligosacchaides/PVA blening spinning solution, and the blending solution with uniformly distributed charges is prepared through utilizing the properties of different solvents. Compared with the prior art, a biological membrane has the smooth fiber surface and more uniform fiber thickness, the fiber diameters are distributed between 50-100nm, the biocompatibility, adhesivity, wound healing capability and other performance can be improved, and the method can be better and more widely applied in the pharmaceuticals industry.
Description
Technical field
The present invention relates to the preparation field of composite nano-fiber membrane, especially relate to the biomembrane electrospinning process of a kind of low molecular weight collagen peptide and chitooligosaccharide-.
Background technology
Along with the development of the progress of modern science and technology, particularly materialogy and pharmacy, textile technology constantly develops in Application of Biomaterial.Especially in recent years, because the upsurge of nanometer technology, the report that the applying high voltage electrostatic spinning technique prepares functional nano fibrous membrane gets more and more.The researcher attempts various polymeric materials (comprising natural with synthetic macromolecule, protein even micromolecule such as lecithin etc.) to be prepared into nano fibrous membrane through electric spinning process, the functional effect of performance material under nanoscale.
Collagen peptide is the catabolite of collagen in the animal connective tissue, because of it has good trophic function and physiological function, has been widely used in industries such as food, cosmetics and medicine.Collagen is the structural protein of extracellular matrix, and the advantage that have low antigenicity, can be absorbed by the body, the vivo degradation product has no side effect receives extensive concern in the application aspect biomaterial.Along with the development of nanometer technology, the relevant nano material of collagen peptide also obtains broad research and application.Yet,, thereby limited its application because its degradation speed in the aqueous solution is too fast.Collagen peptide is as a kind of low-molecular-weight large biological molecule has excellent biological compatibility, low antigenicity equally, can be absorbed by the body, the vivo degradation product has no side effect characteristics; Therefore, the research and the application of the catabolite low molecular weight collagen peptide of collagen have feasibility.At present, the research of this respect is less, and vast potential for future development is arranged again.
Shitosan (chitosan) is main component glycosaminoglycan (GAGs) the similar good natural biologic material very in a kind of structure and the extracellular matrix, the only natural polysaccharide that has obvious alkalescence, has positive charge that also is now to be found.The shitosan good film-forming property, mechanical strength is high, has good biodegradability, biocompatibility and available active group, and efficient, the wide spectrum that has simultaneously, safe anti-microbial property are widely used it in the medicine and pharmacology field.Reason such as relatively poor owing to simple chitosan hydrophilic, that degradation rate is slow, fungistatic effect is not obvious need be improved to its modification or with other materials is compound.
PVA (polyvinyl alcohol) is a kind of water-soluble polymer that is formed by the polyvinyl acetate hydrolysis; Its molecular backbone is a carbochain, contains a hydroxyl on each repetitive, because the hydroxyl size is little; Polarity is strong; Form hydrogen bond easily, so PVA have good water-solubility, film forming, cohesion and emulsibility, good grease resistance and solvent resistance.PVA is a water-soluble polymer, good spinnability; And have preferably biological degradability and biocompatibility and some water-soluble polymers and be mixed and made into electricity and spin membrane material and have many potential purposes in biomedical materials field.
Through the high-voltage electrostatic spinning technology with water-soluble polypeptide and chitooligosaccharide-, PVA blending; Overcome that simple chitosan hydrophilic is relatively poor, degradation rate is slow, spinnability is relatively poor defective; Can obtain diameter uniform fibers film, can apply to wound dressing, not only improve its anti-inflammatory, bacteriostasis; And increased the adhesiveness with wound, promote the healing of tissue reconstruction and wound.Therefore, collagen polypeptide/chitooligosaccharide-composite cellulosic membrane has very big potentiality and exploitation value in the application aspect medical.
Summary of the invention
The object of the invention be exactly provide in order to overcome the defective that above-mentioned prior art exists a kind of biocompatibility that obtains product, adhesiveness better, the low molecular weight collagen peptide that has wide range of applications and the biomembrane electrospinning process of chitooligosaccharide-.
The object of the invention can be realized through following technical scheme:
The biomembrane electrospinning process of a kind of low molecular weight collagen peptide and chitooligosaccharide-is characterized in that, this method may further comprise the steps:
(1) preparing spinning solution:
Chitooligosaccharide-is dissolved in the formic acid, prepares mass concentration and be 3～5% chitooligosaccharide-formic acid solution;
The low molecular weight collagen peptide is dissolved in the distilled water, prepares mass concentration and be 8～16% the collagen peptide aqueous solution;
Polyvinyl alcohol is dissolved in the distilled water, prepares mass concentration and be 5～8% polyvinyl alcohol water solution;
(2) with chitooligosaccharide-formic acid solution and collagen peptide aqueous solution; In the mixture that obtains, add polyvinyl alcohol water solution then; Stir 1h it is mixed, place the micro-injection pump that is connected with high pressure generator to carry out spinning the mixed solution that obtains again, promptly obtain product.
Chitooligosaccharide-described in the step (1) is the chitooligosaccharide-of deacetylation＞90%, viscosity＜100cps.
The molecular weight of the low molecular weight collagen peptide described in the step (1) is 800Da.
The weight ratio of the chitooligosaccharide-formic acid solution and the collagen peptide aqueous solution is 1: 3,1: 2,1: 1,2: 1 or 3: 1 in the mixture described in the step (2).
The weight ratio of mixed solution described in the step (2) and polyvinyl alcohol water solution is 1: (1～3).
The control voltage of the micro-injection pump described in the step (2) is 19kv～23kv, and the propelling speed during this micro-injection pump spinning is 0.3ml/h～0.8ml/h.
The product that adopts the dull and stereotyped acceptance of aluminium foil to obtain when carrying out spinning in the step (2), the distance between micro-injection pump and the aluminium foil flat board is 8～13cm.
Compared with prior art; The present invention is with processing spinning solution in large biological molecule, low molecular weight inorganic constituents and fibre-forming polymer and other auxiliary element co-blended solvent; Composite nano-fiber membrane even thickness through the preparation of high-voltage electrostatic spinning technology; Diameter Distribution is between 50-100nm, and performances such as biocompatibility, adhesiveness and Wound healing ability also improve, and can be applied to pharmaceuticals industry better, widely.
Description of drawings
Fig. 1 prepares the SEM photo of product for Comparative Examples 1;
Fig. 2 prepares the SEM photo of product for Comparative Examples 2;
Fig. 3 prepares the SEM photo of product for embodiment 1.
The specific embodiment
Below in conjunction with accompanying drawing and specific embodiment the present invention is elaborated.
Comparative Examples 1
The biomembranous preparation of chitooligosaccharide-/PVA
One of configuration spinning solution: 0.1 gram chitooligosaccharide-is dissolved in 5 milliliters of formic acid solvent, and 4 ℃ of condition held are to dissolving fully.
Two of configuration spinning solution: 0.5 gram PVA is dissolved in 10 milliliters of distilled waters, the concussion mixing, room temperature leaves standstill to dissolving fully.
Above-mentioned two kinds of spinning solutions are mixed, put into the magnetic agitation rotor, about 3 hours of stirring and evenly mixing, 4 ℃ of refrigerations are for use.Need before blend spinning liquid uses to make it to mix in about 1 hour in magnetic stirrer, ultrasonic degas is 15 minutes before the last syringe pump liquid storage syringe.
Adopt syringe needle as the capillary that sprays thread; Connect high pressure generator (GDW-A; High-Voltage Technology research institute of High Technologies Co., Ltd., Beijing Electromechanical Academy); The spinning liquid measure is controlled by the propelling speed of spinning solution reservoir diameter and micro-injection pump (WZ-50C2, Zhejiang University, Zhejiang Medical Instrument Co., Ltd) jointly, adopts the aluminium foil flat board to accept fiber.Electricity spinning process parameter condition: propelling speed is 0.4cm/h, and the luxuriant spinning nozzle distance of dash receiver is 8cm, and voltage is 20kv, and environment temperature is 30 ℃.
Adopt ESEM that spin mixing nano fibrous membrane is carried out configuration of surface and observe, the result is as shown in Figure 1, and it is continuous to mix the nano fibrous membrane network-like structure, even structure.The tunica fibrosa smooth surface, fiber thickness is more even.
Comparative Examples 2
The biomembranous preparation of polypeptide/PVA
One of configuration spinning solution: 0.18 gram low molecular weight collagen peptide is dissolved in 6 milliliters of distilled waters, and the room temperature condition held is to dissolving fully.
Two of configuration spinning solution: 0.7 gram PVA is dissolved in 10 milliliters of distilled waters, the concussion mixing, room temperature leaves standstill to dissolving fully.
Above-mentioned two kinds of spinning solutions are mixed, put into the magnetic agitation rotor, about 3 hours of stirring and evenly mixing, 4 ℃ of refrigerations are for use.Need before blend spinning liquid uses to make it to mix in 1 hour at the agitator stir about, ultrasonic degas is 15 minutes before the last syringe pump liquid storage syringe.
Adopt syringe needle as the capillary that sprays thread; Connect high pressure generator (GDW-A; High-Voltage Technology research institute of High Technologies Co., Ltd., Beijing Electromechanical Academy); The spinning liquid measure is controlled by the propelling speed of spinning solution reservoir diameter and micro-injection pump (WZ-50C2, Zhejiang University, Zhejiang Medical Instrument Co., Ltd) jointly, adopts the aluminium foil flat board to accept fiber.Electricity spinning process parameter condition: propelling speed is 0.5cm/h, and the luxuriant spinning nozzle distance of dash receiver is 13cm, and voltage is 18kv, and environment temperature is 30 ℃.
Adopt ESEM that spin mixing nano fibrous membrane is carried out configuration of surface and observe, the result is as shown in Figure 2, and it is continuous to mix the nano fibrous membrane network-like structure.The tunica fibrosa smooth surface, fiber thickness is inhomogeneous.
The biomembranous preparation of polypeptide/chitooligosaccharide-/PVA
One of configuration spinning solution: 0.2 gram low molecular weight collagen peptide is dissolved in 6 milliliters of distilled waters, and the room temperature condition held is to dissolving fully.
Two of configuration spinning solution: 0.3 gram chitooligosaccharide-is dissolved in 5 milliliters of formic acid solvent, and 4 ℃ of condition held are to dissolving fully.
Three of configuration spinning solution: 0.6 gram PVA is dissolved in 10 milliliters of distilled waters, the concussion mixing, room temperature leaves standstill to dissolving fully.
Above-mentioned three kinds of spinning solutions are mixed, put into the magnetic agitation rotor, about 3 hours of stirring and evenly mixing, 4 ℃ of refrigerations are for use.Need before blend spinning liquid uses to make it to mix in 1 hour at the agitator stir about, ultrasonic degas is 15 minutes before the last syringe pump liquid storage syringe.
Adopt syringe needle as the capillary that sprays thread; Connect high pressure generator (GDW-A; High-Voltage Technology research institute of High Technologies Co., Ltd., Beijing Electromechanical Academy); The spinning liquid measure is controlled by the propelling speed of spinning solution reservoir diameter and micro-injection pump (WZ-50C2, Zhejiang University, Zhejiang Medical Instrument Co., Ltd) jointly, adopts the aluminium foil flat board to accept fiber.Electricity spinning process parameter condition: propelling speed is 0.2cm/h, and dash receiver is 8cm from the spinning nozzle distance, and voltage is 20kv, and environment temperature is 37 ℃.
Adopt ESEM that spin mixing nano fibrous membrane is carried out configuration of surface and observe, the result is as shown in Figure 3, and mixing nano fibrous membrane network-like structure is evenly distributed, the tunica fibrosa smooth surface, and fiber thickness is even, and fibre diameter is less, is distributed between the 50-200nm.
Embodiment 2
The biomembrane electrospinning process of a kind of low molecular weight collagen peptide and chitooligosaccharide-, this method may further comprise the steps:
(1) preparing spinning solution:
The chitooligosaccharide-of deacetylation＞90%, viscosity＜100cps is dissolved in the formic acid, prepares mass concentration and be 3% chitooligosaccharide-formic acid solution;
The low molecular weight collagen peptide is dissolved in the distilled water, prepares mass concentration and be 8% the collagen peptide aqueous solution;
Polyvinyl alcohol is dissolved in the distilled water, prepares mass concentration and be 5% polyvinyl alcohol water solution;
(2) with chitooligosaccharide-formic acid solution and the collagen peptide aqueous solution by weight being to mix at 1: 3; In the mixture that obtains, add polyvinyl alcohol water solution then; The weight ratio of mixed solution and polyvinyl alcohol water solution is 1: 1, stirs 1h it is mixed, and places the micro-injection pump that is connected with high pressure generator to carry out spinning the mixed solution that obtains again; The control voltage of control micro-injection pump is 19kv; Propelling speed during this micro-injection pump spinning is 0.3ml/h, the product that adopts the dull and stereotyped acceptance of aluminium foil to obtain, and the distance between micro-injection pump and the aluminium foil flat board is 8cm.
Embodiment 3
The biomembrane electrospinning process of a kind of low molecular weight collagen peptide and chitooligosaccharide-, this method may further comprise the steps:
(1) preparing spinning solution:
The chitooligosaccharide-of deacetylation＞90%, viscosity＜100cps is dissolved in the formic acid, prepares mass concentration and be 5% chitooligosaccharide-formic acid solution;
The low molecular weight collagen peptide is dissolved in the distilled water, prepares mass concentration and be 16% the collagen peptide aqueous solution;
Polyvinyl alcohol is dissolved in the distilled water, prepares mass concentration and be 8% polyvinyl alcohol water solution;
(2) with chitooligosaccharide-formic acid solution and the collagen peptide aqueous solution by weight being to mix at 1: 2; In the mixture that obtains, add polyvinyl alcohol water solution then; The weight ratio of mixed solution and polyvinyl alcohol water solution is 1: 2, stirs 1h it is mixed, and places the micro-injection pump that is connected with high pressure generator to carry out spinning the mixed solution that obtains again; The control voltage of control micro-injection pump is 23kv; Propelling speed during this micro-injection pump spinning is 0.8ml/h, the product that adopts the dull and stereotyped acceptance of aluminium foil to obtain, and the distance between micro-injection pump and the aluminium foil flat board is 13cm.
Embodiment 4
The biomembrane electrospinning process of a kind of low molecular weight collagen peptide and chitooligosaccharide-, this method may further comprise the steps:
(1) preparing spinning solution:
The chitooligosaccharide-of deacetylation＞90%, viscosity＜100cps is dissolved in the formic acid, prepares mass concentration and be 4% chitooligosaccharide-formic acid solution;
The low molecular weight collagen peptide is dissolved in the distilled water, prepares mass concentration and be 12% the collagen peptide aqueous solution;
Polyvinyl alcohol is dissolved in the distilled water, prepares mass concentration and be 6% polyvinyl alcohol water solution;
(2) with chitooligosaccharide-formic acid solution and the collagen peptide aqueous solution by weight being to mix at 1: 1; In the mixture that obtains, add polyvinyl alcohol water solution then; The weight ratio of mixed solution and polyvinyl alcohol water solution is 1: 3, stirs 1h it is mixed, and places the micro-injection pump that is connected with high pressure generator to carry out spinning the mixed solution that obtains again; The control voltage of control micro-injection pump is 20kv; Propelling speed during this micro-injection pump spinning is 0.5ml/h, the product that adopts the dull and stereotyped acceptance of aluminium foil to obtain, and the distance between micro-injection pump and the aluminium foil flat board is 10cm.
The biomembrane electrospinning process of a kind of low molecular weight collagen peptide and chitooligosaccharide-, this method may further comprise the steps:
(1) preparing spinning solution:
The chitooligosaccharide-of deacetylation＞90%, viscosity＜100cps is dissolved in the formic acid, prepares mass concentration and be 4% chitooligosaccharide-formic acid solution;
The low molecular weight collagen peptide is dissolved in the distilled water, prepares mass concentration and be 12% the collagen peptide aqueous solution;
Polyvinyl alcohol is dissolved in the distilled water, prepares mass concentration and be 6% polyvinyl alcohol water solution;
(2) with chitooligosaccharide-formic acid solution and the collagen peptide aqueous solution by weight being to mix at 2: 1; In the mixture that obtains, add polyvinyl alcohol water solution then; The weight ratio of mixed solution and polyvinyl alcohol water solution is 1: 1, stirs 1h it is mixed, and places the micro-injection pump that is connected with high pressure generator to carry out spinning the mixed solution that obtains again; The control voltage of control micro-injection pump is 20kv; Propelling speed during this micro-injection pump spinning is 0.5ml/h, the product that adopts the dull and stereotyped acceptance of aluminium foil to obtain, and the distance between micro-injection pump and the aluminium foil flat board is 10cm.
Embodiment 6
The biomembrane electrospinning process of a kind of low molecular weight collagen peptide and chitooligosaccharide-, this method may further comprise the steps:
(1) preparing spinning solution:
The chitooligosaccharide-of deacetylation＞90%, viscosity＜100cps is dissolved in the formic acid, prepares mass concentration and be 4% chitooligosaccharide-formic acid solution;
The low molecular weight collagen peptide is dissolved in the distilled water, prepares mass concentration and be 12% the collagen peptide aqueous solution;
Polyvinyl alcohol is dissolved in the distilled water, prepares mass concentration and be 6% polyvinyl alcohol water solution;
(2) with chitooligosaccharide-formic acid solution and the collagen peptide aqueous solution by weight being to mix at 3: 1; In the mixture that obtains, add polyvinyl alcohol water solution then; The weight ratio of mixed solution and polyvinyl alcohol water solution is 1: 1, stirs 1h it is mixed, and places the micro-injection pump that is connected with high pressure generator to carry out spinning the mixed solution that obtains again; The control voltage of control micro-injection pump is 20kv; Propelling speed during this micro-injection pump spinning is 0.5ml/h, the product that adopts the dull and stereotyped acceptance of aluminium foil to obtain, and the distance between micro-injection pump and the aluminium foil flat board is 10cm.
Claims (7)
1. the biomembrane electrospinning process of low molecular weight collagen peptide and chitooligosaccharide-is characterized in that this method may further comprise the steps:
(1) preparing spinning solution:
Chitooligosaccharide-is dissolved in the formic acid, prepares mass concentration and be 3～5% chitooligosaccharide-formic acid solution;
The low molecular weight collagen peptide is dissolved in the distilled water, prepares mass concentration and be 8～16% the collagen peptide aqueous solution;
Polyvinyl alcohol is dissolved in the distilled water, prepares mass concentration and be 5～8% polyvinyl alcohol water solution;
(2) with chitooligosaccharide-formic acid solution and collagen peptide aqueous solution; In the mixture that obtains, add polyvinyl alcohol water solution then; Stir 1h it is mixed, place the micro-injection pump that is connected with high pressure generator to carry out spinning the mixed solution that obtains again, promptly obtain product.
2. the biomembrane electrospinning process of a kind of low molecular weight collagen peptide according to claim 1 and chitooligosaccharide-is characterized in that the chitooligosaccharide-described in the step (1) is the chitooligosaccharide-of deacetylation＞90%, viscosity＜100cps.
3. the biomembrane electrospinning process of a kind of low molecular weight collagen peptide according to claim 1 and chitooligosaccharide-is characterized in that the molecular weight of the low molecular weight collagen peptide described in the step (1) is 800Da.
4. the biomembrane electrospinning process of a kind of low molecular weight collagen peptide according to claim 1 and chitooligosaccharide-; It is characterized in that the weight ratio of the chitooligosaccharide-formic acid solution and the collagen peptide aqueous solution is 1: 3,1: 2,1: 1,2: 1 or 3: 1 in the mixture described in the step (2).
5. the biomembrane electrospinning process of a kind of low molecular weight collagen peptide according to claim 1 and chitooligosaccharide-is characterized in that the weight ratio of mixed solution described in the step (2) and polyvinyl alcohol water solution is 1: (1～3).
6. the biomembrane electrospinning process of a kind of low molecular weight collagen peptide according to claim 1 and chitooligosaccharide-; It is characterized in that; The control voltage of the micro-injection pump described in the step (2) is 19kv～23kv, and the propelling speed during this micro-injection pump spinning is 0.3ml/h～0.8ml/h.
7. the biomembrane electrospinning process of a kind of low molecular weight collagen peptide according to claim 1 and chitooligosaccharide-; It is characterized in that; The product that adopts the dull and stereotyped acceptance of aluminium foil to obtain when carrying out spinning in the step (2), the distance between micro-injection pump and the aluminium foil flat board is 8～13cm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102808285A (en) * | 2012-07-26 | 2012-12-05 | 东华大学 | Method for preparing nano fiber membrane by using dipeptide monomers through electrostatic spinning |
| CN103100107A (en) * | 2013-01-25 | 2013-05-15 | 安吉县阳光医药用品有限责任公司 | Method for preparing medical chitin biological dressing |
| CN105401232A (en) * | 2015-11-02 | 2016-03-16 | 浙江纺织服装科技有限公司 | Method for preparing biological dressing composite micro-nano fiber membrane |
| CN115252518A (en) * | 2022-07-28 | 2022-11-01 | 上海应用技术大学 | Instant plant extract/polymer composite fiber membrane and preparation thereof |
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| CN101187111A (en) * | 2007-11-29 | 2008-05-28 | 东华大学 | Composite nanometer fiber felt containing nano silver gelatin/chitosan for medical dressing and its preparation |
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| CN100535212C (en) * | 2006-10-11 | 2009-09-02 | 东华大学 | Method for preparing collagen protein and chitosan composite nano fibre and film electro static spinning |
| CN101265621A (en) * | 2007-03-13 | 2008-09-17 | 成都佰乐金生物科技有限公司 | Collagen protein-polyvinyl alcohol-chitosan blending medical fibre and method for making same |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102808285A (en) * | 2012-07-26 | 2012-12-05 | 东华大学 | Method for preparing nano fiber membrane by using dipeptide monomers through electrostatic spinning |
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| CN105401232A (en) * | 2015-11-02 | 2016-03-16 | 浙江纺织服装科技有限公司 | Method for preparing biological dressing composite micro-nano fiber membrane |
| CN105401232B (en) * | 2015-11-02 | 2017-09-29 | 浙江纺织服装科技有限公司 | A kind of preparation method of biological dressing composite micro-nano rice tunica fibrosa |
| CN115252518A (en) * | 2022-07-28 | 2022-11-01 | 上海应用技术大学 | Instant plant extract/polymer composite fiber membrane and preparation thereof |
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Application publication date: 20120530 |