CN106693029A - Preparation method of chitosan oligosaccharide -based polyelectrolyte styptic powder - Google Patents

Preparation method of chitosan oligosaccharide -based polyelectrolyte styptic powder Download PDF

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CN106693029A
CN106693029A CN201510524236.XA CN201510524236A CN106693029A CN 106693029 A CN106693029 A CN 106693029A CN 201510524236 A CN201510524236 A CN 201510524236A CN 106693029 A CN106693029 A CN 106693029A
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acid
polyelectrolyte
chitosan oligosaccharide
styptic powder
preparation
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赵岩
张文昌
张劲松
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Institute of Metal Research of CAS
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Abstract

The invention belongs to the field of biological medicinal material preparation, and relates to a preparation method of chitosan oligosaccharide-based polyelectrolyte styptic powder. The preparation method comprises the following steps of firstly dissolving chitosan oligosaccharide and an anionic polyelectrolyte or ampholytic polyelectrolyte having biocompatibility in deionized water; reducing the pH (Potential of Hydrogen) value of the solution, protonizing and positively charging amino groups of chitosan oligosaccharide molecules, and interacting with the anionic polyelectrolyte or ampholytic polyelectrolyte through coulomb force, thus forming a compound; drying and smashing the polyelectrolyte compound, thus obtaining the chitosan oligosaccharide-based polyelectrolyte styptic powder. The chitosan oligosaccharide-based polyelectrolyte styptic powder prepared by the preparation method disclosed by the invention has good biocompatibility and good antibacterial activity, and an excellent hemostatic function is reflected.

Description

A kind of preparation method of the polyelectrolyte styptic powder based on chitosan oligosaccharide
Technical field
The invention belongs to biological medicine field of material preparation, it is related to a kind of polyelectrolyte styptic powder based on chitosan oligosaccharide Preparation method.
Background technology
Modern medical service theoretical proof wound healing is that cell is situated between with cell, cell and cellular matrix and with solubility The continuous dynamic process of matter interphase interaction.The reparation of the surface of a wound and the nutrition of local organization, microenvironment, growth because The interaction of many factors such as sub- content, microcirculation, hypoxia condition, infection is relevant, and medical dressing can rise To critical effect.As a main theoretical basis of high-tech medical dressing, British scientist in 1962 It was found that " wet method therapy " think when the surface of wound maintain one moistening microenvironment in when, epithelial cell Migration is significantly accelerated, and the healing rate of wound is faster than under dry environment.
The material that blood behaviour body weight is wanted, bleeding if that body by timely and effective prevention, can not caused weak, largely Bleeding will cause haemorrhagic shock even dead, thus no matter wartime live wire or pre hospital care be required for it is a kind of can be fast Speed, effectively hemostasis, mitigate the Hemostasis of the adverse effect that hemostasis are caused to suffering limb blood circulation.Research and development tool The wound dressing for having quick-acting haemostatic powder ability is the research field that the countries in the world particularly military extremely pays close attention to.
Hemostatic material has polytype from mechanism of action.Such as contain fibrinogen, fibrin ferment hemostatic material External hemostatic composition is directly or indirectly provided and accelerates coagulation process;Farina, zeolite etc. are by material Physically or chemically effect concentrates hemostatic composition, assembles and accelerate blood coagulation;The materials such as cyanoacrylate are to tissue There is very strong adhesion strength, directly can reach hemostasis purpose by wound closure.Main hemostatic material currently on the market There are the Celox hemostasis kings of the BioCer and Britain with shitosan as main material Germany, it is absorbable many with starch type Glycan is PerClot the and Arista styptic powders in the main material U.S., is the main component U.S. with zeolite QuikClot styptic powders, the WoundStat hemostatic materials with montmorillonite as main material, and combine mesoporous silicon, New hemostatic material TraumaStat of shitosan and polyethylene etc..
Preferable topical hemostatic agent should have rapid hemostasis, toxicity and tissue reaction is light, good biocompatibility, drop Solution is rapid, use, it is cheap, accelerate organization healing and adapt to different parts and different type bleeding Hemostasis etc. is required.But existing conventional Hemostasis and haemostatic medicament are also far from meeting these requirements.Inorganic Often there is certain defect in terms of biological safety in hemostatic material.Porous zeolite and farina are absorbing blood Can be highly exothermic after moisture in liquid, cause wound tissue to injure.Fibrin class hemostatic material environmental suitability Difference, the shelf-life is short, expensive.Polysaccharide hemostatic material absorption speed with tridimensional network is slow, water suction Multiplying power is low, and the gel viscosity formed after water suction is poor, it is impossible to effective viscosity envelope is produced to damaged tissue, blood vessel Stifled, haemostatic effect is also undesirable.
Chitin be widely present Yu Haiyang crustacean shell, mollusk endoskeleton, insect wing, mushroom and It is natural polysaccharide and second largest renewable resource that tellurian reserves are only second to cellulose in alga cells wall. Shitosan is the deacetylated product in strong base solution of chitin, is only a large amount of bands for existing in natural polysaccharide Positive charge basic amine group polysaccharide, it is and nontoxic with special physics, chemistry and physiologically active, it is biodegradable, Good biocompatibility, it is considered to be " vital principle of human body the 6th ".
Shitosan is readily dissolved in most of organic acids and inorganic acid, but water insoluble.Chitosan oligosaccharide is shitosan Molecular weight degradation is to less than 3000, the oligosaccharide being mainly formed by connecting by 2~10 Glucosamines.Chitosan oligosaccharide With good water solubility, bioactivity is high, function is big, be easily absorbed by the body etc. outstanding feature and many uniquenesses Function, be chitin, the high-grade products of shitosan series of products, application field has been directed to chemistry, doctor All many-sides such as medicine, food, cosmetics, agricultural, environmental protection, poultry industry, have a extensive future.
Numerous studies find that chitosan oligosaccharide has many physiological functions, if microbial metabolism in regulation animal intestinal tract Activity, improves intestinal microflora distribution, strengthens beneficial bacteria growing;Promote antibody tormation, improve body Immunocompetence, suppresses tumour growth;Chitosan oligosaccharide molecule can be acted on after protonation with the cell membrane of bacterium, interference Bacterial cell membrane function, causes bacterial body inner cell mass flow to lose, and shows obvious antibacterial and bacteriostasis;Have Reduce blood pressure blood sugar, blood fat, cholesterol is adsorbed, so as to be effectively reduced liver and cholesterol in serum;Reinforcing Liver function, prevents gout and gastric ulcer;Strengthen immunity and anti-disease ability.As a kind of biocompatibility Good, non-immunogenicity, nonirritant multifunctional material, chitosan oligosaccharide not only have very strong bacteriostasis, And with various functions such as acceleration blood coagulation, promotion wound healing, suppression cicatrization.
The pKa value of amino is about 6.5 in chitosan oligosaccharide molecule, when the pH value of solution is less than 6.0, chitosan oligosaccharide The aobvious electropositive of the protonated amino of molecule.Therefore when the pH value of solution is adjusted when 3.0 to 6.0 is interval, band is just The chitosan oligosaccharide molecule of electric charge can pass through Coulomb interactions with polyanion electrolyte or double property polyelectrolyte molecules Power and simultaneously form a kind of random compound.This compound is a kind of nonequilibrium condition, over time Passage, by other secondary phase interactions such as hydrogen bond, van der waals force, electric charge transfer and heat resistance and salt tolerance power With and gradually form more stable compound.The three-dimensional net structure formed using this compound polyelectrolyte, Can avoid the chemical cross-linking agent for having certain toxicity using such as glutaraldehyde in material preparation process, and can be compared with Good reservation polyelectrolyte material performance excellent in itself, has important application prospect in biological field.
The content of the invention
Present invention aim at a kind of preparation method of the polyelectrolyte styptic powder based on chitosan oligosaccharide of offer, acquisition Polyelectrolyte styptic powder shows excellent hemostatic function, solves existing conventional Hemostasis and haemostatic medicament not The problems such as requiring can be met.
The technical scheme is that:
A kind of preparation method of the polyelectrolyte styptic powder based on chitosan oligosaccharide, prepare first containing chitosan oligosaccharide and it is cloudy from The solution of sub- polyelectrolyte or polyampholyte, adjusting the pH value of the polyelectrolyte solution makes chitosan oligosaccharide molecule It is positively charged and interact to form compound by Coulomb force with anionic polyelectrolyte or polyampholyte, Compound polyelectrolyte obtains chitosan oligosaccharide polyelectrolyte styptic powder after drying and crushing.
The preparation method of the described polyelectrolyte styptic powder based on chitosan oligosaccharide, comprises the following steps that:
1) polyelectrolyte mixtures containing chitosan oligosaccharide and anionic polyelectrolyte or polyampholyte are prepared water-soluble Liquid;
2) pH value of the regulation polyelectrolyte mixtures aqueous solution makes the ammonia of chitosan oligosaccharide molecule to 3.0~6.0 intervals Base is protonated and shows electropositive;Positively charged chitosan oligosaccharide molecule is with anionic polyelectrolyte or polyampholyte Interacted by Coulomb force, form compound polyelectrolyte;
3) after compound polyelectrolyte is through drying and crushing, chitosan oligosaccharide polyelectrolyte styptic powder is obtained.
The preparation method of the described polyelectrolyte styptic powder based on chitosan oligosaccharide, step 1) polyelectrolyte mixtures In the aqueous solution, 500~5000, deacetylation is 60%~100% to chitosan oligosaccharide molecular weight, and content is described molten 0.1~13wt.% of liquid gross mass.
The preparation method of the described polyelectrolyte styptic powder based on chitosan oligosaccharide, step 1) polyelectrolyte mixtures In the aqueous solution, anionic polyelectrolyte or polyampholyte are to contain-COO with good biocompatibility-、 -SO3-、-O-CS2-、-O-PO3 2-Natural, semi-synthetic or synthesis the high-molecular organic material of anionic group, The content of anionic polyelectrolyte or polyampholyte is 0.3~20wt.% of the gross mass.
The preparation method of the described polyelectrolyte styptic powder based on chitosan oligosaccharide, the anionic polyelectrolyte of use or Polyampholyte is hyaluronic acid, chondroitin sulfate, dermatan sulfate, keratan sulfate, heparin, marine alga Sour sodium, xanthans, carragheen, pectin, gum arabic, Karaya Gum, tragacanth gum, sodium lignin sulfonate, Carboxylic Derivates of Starch, carboxymethylcellulose calcium, polyacrylic acid, polymethylacrylic acid, polystyrolsulfon acid, polyethylene sulphur In acid, polyvinylphosphonic acid, carboxymethyl chitosan, vinyl pyridine copolymer, nucleic acid, protein one Plant or two or more.
The preparation method of the described polyelectrolyte styptic powder based on chitosan oligosaccharide, step 2) regulation polyelectrolyte mix During the pH value of the compound aqueous solution to 3.0~6.0 interval, matter is added using in the polyelectrolyte mixtures aqueous solution One kind in processing method in acid atmosphere of sub- releasing agent, acid flux material or the polyelectrolyte mixtures aqueous solution or It is two or more.
The preparation method of the described polyelectrolyte styptic powder based on chitosan oligosaccharide, proton release agent uses gluconic acid Lactone, addition is 0.05~5wt.% of polyelectrolyte mixtures aqueous solution gross mass, and process time is 10 points Clock was to 8 hours;Acid solution is the water or alcohol solution of acid, using inorganic acid or organic acid:Hydrochloric acid, sulfuric acid, Phosphoric acid, nitric acid, formic acid, acetic acid, propionic acid, butyric acid, octanoic acid, adipic acid, ethanedioic acid, malonic acid, fourth two Acid, maleic acid, tartaric acid, benzoic acid, phenylacetic acid, phthalic acid, terephthalic acid (TPA), valeric acid, caproic acid, Capric acid, stearic acid, palmitic acid, acrylic acid, tartaric acid, malic acid, citric acid, ascorbic acid, during treatment Between be 0.5 hour to 20 hours;Acid atmosphere uses hydrochloric acid, nitric acid, formic acid, acetic acid, propionic acid, ethanedioic acid It is easy to the inorganic acid or organic acid of volatilization, process time is 20 minutes to 18 hours.
The preparation method of the described polyelectrolyte styptic powder based on chitosan oligosaccharide, step 3) compound polyelectrolyte By constant pressure and dry, drying under reduced pressure, spray drying, fluidized drying, freeze-drying, infrared drying, drying One or more dryings in the dry technology such as agent drying or microwave drying.
The preparation method of the described polyelectrolyte styptic powder based on chitosan oligosaccharide, step 3) dried poly- electrolysis Matter compound refines particle by pulverizer, ball mill or disintegrating machine, obtains chitosan oligosaccharide polyelectrolyte styptic powder.
Advantages of the present invention and beneficial effect are:
1st, the characteristic that the present invention can be dissolved using chitosan oligosaccharide in neutral water, prepares and contains chitosan oligosaccharide and anion The polyelectrolyte mixtures aqueous solution of polyelectrolyte or polyampholyte.Made by the pH value for adjusting the solution The poly- electricity of anionic polyelectrolyte or both sexes in the protonated amino of chitosan oligosaccharide molecule and become positively charged lotus, with solution Solution matter interacts to form compound by Coulomb force.Compound obtains chitosan oligosaccharide polyelectrolyte after drying and crushing Styptic powder.
2nd, the three-dimensional net structure that the present invention is formed using this compound polyelectrolyte, it is to avoid use (such as penta Dialdehyde etc.) there is the chemical cross-linking agent of certain toxicity, and can preferably retain the polyelectrolyte material sheet such as chitosan oligosaccharide The excellent performance of body, shows clear advantage:With biocidal property and excellent hemostatic function;Hemostasis powder particles Small, specific surface area is big, and imbibition ability is strong, can quickly absorb the moisture in blood, Platelet Concentrate and blood coagulation because Son;The surface of a wound, the capillary of closure surface of a wound rupture are adhered to after water swelling;After hemostasis water is formed in the surface of a wound Gelinite, for wound provides good wet environment, wound healing;It is non-stimulated to wound, possess good Biocompatibility and biodegradability.
Specific embodiment
In a specific embodiment, the preparation method of polyelectrolyte styptic powder of the present invention based on chitosan oligosaccharide, first Chitosan oligosaccharide and anionic polyelectrolyte or polyampholyte with biocompatibility are dissolved in deionized water.It is logical The pH value for reducing solution is crossed, makes the protonated amino of chitosan oligosaccharide molecule and the lotus that becomes positively charged, and it is poly- with anion Electrolyte or polyampholyte interact to form compound by Coulomb force.Compound polyelectrolyte is through drying Chitosan oligosaccharide polyelectrolyte styptic powder is obtained after crushing.It is concretely comprised the following steps:
1) polyelectrolyte mixtures containing chitosan oligosaccharide and anionic polyelectrolyte or polyampholyte are prepared water-soluble Liquid.Anionic polyelectrolyte or polyampholyte are to contain-COO with good biocompatibility-、-SO3-、 -O-CS2-、-O-PO3 2-It is such as saturating Deng the natural, semi-synthetic of anionic group or the high-molecular organic material of synthesis Bright matter acid, chondroitin sulfate, dermatan sulfate, keratan sulfate, heparin, sodium alginate, carboxymethyl cellulose Element, xanthans, carragheen, pectin, gum arabic, Karaya Gum, tragacanth gum (tragacanth Gum tragacanth), Sodium lignin sulfonate, Carboxylic Derivates of Starch, polyacrylic acid, polymethylacrylic acid, polystyrolsulfon acid, polyethylene sulphur In acid, polyvinylphosphonic acid, carboxymethyl chitosan, vinyl pyridine copolymer, nucleic acid, protein etc. One or more;
2) add proton release agent, acid flux material or polyelectrolyte mixed using in the polyelectrolyte mixtures aqueous solution One or more in the acid atmosphere in the method such as treatment of the compound aqueous solution, adjust polyelectrolyte mixtures The pH value of the aqueous solution makes the amino of chitosan oligosaccharide molecule be protonated aobvious electropositive to 3.0~6.0 intervals.Band is just The chitosan oligosaccharide molecule of electric charge is mutual by Coulomb force with negatively charged anionic polyelectrolyte or polyampholyte Effect, forms compound polyelectrolyte;
3) compound polyelectrolyte obtains chitosan oligosaccharide polyelectrolyte styptic powder after drying, crushing.
To make technical scheme and advantage clearer, carried out in detail below in conjunction with specific embodiment Description.
Embodiment 1
10 grams of chitosan oligosaccharides, 13 grams of Sodium Polyacrylates and 1g glucolactones dissolve in 1 liter of deionized water, 10 hours are incubated at 50 DEG C.After compound polyelectrolyte is dried 60 hours in 50 DEG C of blast driers, use Ball mill ball milling obtains chitosan oligosaccharide polyelectrolyte styptic powder for 1 hour.The styptic powder has good biocompatibility And biocidal property, show excellent hemostatic function.The external clotting index of the present embodiment is determined and shown, external solidifying Blood index<41%;The haemostatic effect testing result of rabbit arteria auricularis Hemorrhage Model shows, bleeding stopping period<97 seconds.
Embodiment 2
10 grams of chitosan oligosaccharides, 10 grams of hyaluronic acids and 1g glucolactones dissolve in 1 liter of deionized water, 50 DEG C Lower insulation 10 hours.After compound polyelectrolyte is dried 60 hours in 50 DEG C of blast driers, using ball milling Machine ball milling obtains chitosan oligosaccharide polyelectrolyte styptic powder for 1 hour.The styptic powder has good biocompatibility and suppression Bacterium property, shows excellent hemostatic function.The external clotting index of the present embodiment is determined and shown, external blood coagulation refers to Number<56%;The haemostatic effect testing result of rabbit arteria auricularis Hemorrhage Model shows, bleeding stopping period<140 seconds.
Embodiment 3
10 grams of chitosan oligosaccharides, 10 grams of hyaluronic acids and 3g glucolactones dissolve in 1 liter of deionized water, 50 DEG C Lower insulation 10 hours.After compound polyelectrolyte is dried 60 hours in 30 DEG C of blast driers, using ball milling Machine ball milling obtains chitosan oligosaccharide polyelectrolyte styptic powder for 1 hour.The styptic powder has good biocompatibility and suppression Bacterium property, shows excellent hemostatic function.The external clotting index of the present embodiment is determined and shown, external blood coagulation refers to Number<48%;The haemostatic effect testing result of rabbit arteria auricularis Hemorrhage Model shows, bleeding stopping period<90 seconds.
Embodiment 4
10 grams of chitosan oligosaccharides, 12 grams of gum arabics and 1g glucolactones dissolve in 1 liter of deionized water, 10 hours are incubated at 50 DEG C.After compound polyelectrolyte is dried 60 hours in 50 DEG C of blast driers, use Ball mill ball milling obtains chitosan oligosaccharide polyelectrolyte styptic powder for 1 hour.The styptic powder has good biocompatibility And biocidal property, show excellent hemostatic function.The external clotting index of the present embodiment is determined and shown, external solidifying Blood index<60%;The haemostatic effect testing result of rabbit arteria auricularis Hemorrhage Model shows, bleeding stopping period<170 seconds.
Embodiment 5
30 grams of chitosan oligosaccharides, 15 grams of sodium alginates and 3g glucolactones dissolve in 1 liter of deionized water, 50 DEG C Lower insulation 10 hours.After compound polyelectrolyte is dried 60 hours in 50 DEG C of blast driers, using ball milling Machine ball milling obtains chitosan oligosaccharide polyelectrolyte styptic powder for 1 hour.The styptic powder has good biocompatibility and suppression Bacterium property, shows excellent hemostatic function.The external clotting index of the present embodiment is determined and shown, external blood coagulation refers to Number<50%;The haemostatic effect testing result of rabbit arteria auricularis Hemorrhage Model shows, bleeding stopping period<121 seconds.
Embodiment 6
25 grams of chitosan oligosaccharides, 18 grams of Carboxylic Derivates of Starch and 1g glucolactones dissolve in 1 liter of deionized water, 50 DEG C Lower insulation 10 hours.After compound polyelectrolyte is dried 60 hours in 50 DEG C of blast driers, using ball milling Machine ball milling obtains chitosan oligosaccharide polyelectrolyte styptic powder for 1 hour.The styptic powder has good biocompatibility and suppression Bacterium property, shows excellent hemostatic function.The external clotting index of the present embodiment is determined and shown, external blood coagulation refers to Number<70%;The haemostatic effect testing result of rabbit arteria auricularis Hemorrhage Model shows, bleeding stopping period<160 seconds.
Embodiment 7
10 grams of chitosan oligosaccharides, 13 grams of Sodium Polyacrylates dissolve in 1 liter of deionized water.10mL hydrochloric acid solutions (rub You are concentration 0.1M) it is injected into the polyelectrolyte mixtures aqueous solution, process 4 hours at room temperature.Polyelectrolyte After compound is dried 40 hours in vacuum drying chamber, the poly- electrolysis of chitosan oligosaccharide is obtained for 1 hour using ball mill ball milling Matter styptic powder.The styptic powder has good biocompatibility and biocidal property, shows excellent hemostatic function. The external clotting index of the present embodiment is determined and shown, external clotting index<50%;Rabbit arteria auricularis Hemorrhage Model Haemostatic effect testing result shows, bleeding stopping period<130 seconds.
Embodiment 8
10 grams of chitosan oligosaccharides, 13 grams of Sodium Polyacrylates dissolve in 1 liter of deionized water, are then placed in acetic acid atmosphere, Process 8 hours at room temperature.After compound polyelectrolyte is dried 60 hours in 50 DEG C of blast driers, adopt Chitosan oligosaccharide polyelectrolyte styptic powder is obtained within 1 hour with ball mill ball milling.The styptic powder has good bio-compatible Property and biocidal property, show excellent hemostatic function.The external clotting index of the present embodiment is determined and shown, in vitro Clotting index<55%;The haemostatic effect testing result of rabbit arteria auricularis Hemorrhage Model shows, bleeding stopping period<140 Second.
Embodiment 9
15 grams of chitosan oligosaccharides, 18 grams of carboxymethylcellulose calciums dissolve in 1 liter of deionized water, are then placed in acetic acid atmosphere In, process 8 hours at room temperature.After compound polyelectrolyte is dried 60 hours in 50 DEG C of blast driers, Chitosan oligosaccharide polyelectrolyte styptic powder is obtained for 1 hour using ball mill ball milling.The styptic powder has good biofacies Capacitive and biocidal property, show excellent hemostatic function.The external clotting index of the present embodiment is determined and shown, body Outer clotting index<70%;The haemostatic effect testing result of rabbit arteria auricularis Hemorrhage Model shows, bleeding stopping period<180 Second.
Embodiment 10
10 grams of chitosan oligosaccharides are dissolved in 500mL distilled water.13 grams of Sodium Polyacrylates are dissolved in 400mL distilled water In.5g glucolactones are dissolved in 100mL distilled water.Merge chitosan oligosaccharide, Sodium Polyacrylate and grape Saccharic acid lactone solution, 10 hours are incubated at 50 DEG C.Compound polyelectrolyte dries 28 in infrared drier After hour, chitosan oligosaccharide polyelectrolyte styptic powder is obtained for 1 hour using ball mill ball milling.The styptic powder has good Biocompatibility and biocidal property, show excellent hemostatic function.The external clotting index of the present embodiment is determined Show, external clotting index<60%;The haemostatic effect testing result of rabbit arteria auricularis Hemorrhage Model shows, stops blooding Time<110 seconds.

Claims (9)

1. a kind of preparation method of the polyelectrolyte styptic powder based on chitosan oligosaccharide, it is characterised in that:Prepare first and contain There is the solution of chitosan oligosaccharide and anionic polyelectrolyte or polyampholyte, adjust the pH of the polyelectrolyte solution Value makes chitosan oligosaccharide molecule positively charged and passes through Coulomb force phase interaction with anionic polyelectrolyte or polyampholyte With compound is formed, compound polyelectrolyte obtains chitosan oligosaccharide polyelectrolyte styptic powder after drying and crushing.
2. the preparation method of the polyelectrolyte styptic powder based on chitosan oligosaccharide according to claim 1, its feature It is to comprise the following steps that:
1) polyelectrolyte mixtures containing chitosan oligosaccharide and anionic polyelectrolyte or polyampholyte are prepared water-soluble Liquid;
2) pH value of the regulation polyelectrolyte mixtures aqueous solution makes the ammonia of chitosan oligosaccharide molecule to 3.0~6.0 intervals Base is protonated and shows electropositive;Positively charged chitosan oligosaccharide molecule is with anionic polyelectrolyte or polyampholyte Interacted by Coulomb force, form compound polyelectrolyte;
3) after compound polyelectrolyte is through drying and crushing, chitosan oligosaccharide polyelectrolyte styptic powder is obtained.
3. the preparation method of the polyelectrolyte styptic powder based on chitosan oligosaccharide according to claim 2, its feature It is, step 1) in the polyelectrolyte mixtures aqueous solution, chitosan oligosaccharide molecular weight is in 500~5000, deacetylation It is 60%~100%, content is 0.1~13wt.% of the solution gross mass.
4. the preparation method of the polyelectrolyte styptic powder based on chitosan oligosaccharide according to claim 2, its feature It is, step 1) in the polyelectrolyte mixtures aqueous solution, anionic polyelectrolyte or polyampholyte are tool Have good biocompatibility contains-COO-、-SO3-、-O-CS2-、-O-PO3 2-Anionic group it is natural, half The content of synthesis or the high-molecular organic material of synthesis, anionic polyelectrolyte or polyampholyte is described total 0.3~20wt.% of quality.
5. the preparation method of the polyelectrolyte styptic powder based on chitosan oligosaccharide according to claim 2 or 4, its It is characterised by, the anionic polyelectrolyte or polyampholyte for using are hyaluronic acid, chondroitin sulfate, sulphur Sour dermatan, keratan sulfate, heparin, sodium alginate, xanthans, carragheen, pectin, gum arabic, Karaya Gum, tragacanth gum, sodium lignin sulfonate, Carboxylic Derivates of Starch, carboxymethylcellulose calcium, polyacrylic acid, poly- first Base acrylic acid, polystyrolsulfon acid, polyvinyl sulfonic acid, polyvinylphosphonic acid, carboxymethyl chitosan, acrylic acid second One or more in annulated pyridine copolymer, nucleic acid, protein.
6. the preparation method of the polyelectrolyte styptic powder based on chitosan oligosaccharide according to claim 2, its feature Be, step 2) pH value of the regulation polyelectrolyte mixtures aqueous solution to 3.0~6.0 it is interval when, using poly- Proton release agent, acid flux material or the polyelectrolyte mixtures aqueous solution are added in the electrolyte mixture aqueous solution in acid One or more in property atmosphere in processing method.
7. the preparation method of the polyelectrolyte styptic powder based on chitosan oligosaccharide according to claim 6, its feature It is,
Proton release agent uses glucolactone, and addition is polyelectrolyte mixtures aqueous solution gross mass 0.05~5wt.%, process time is 10 minutes to 8 hours;
Acid solution is the water or alcohol solution of acid, using inorganic acid or organic acid:Hydrochloric acid, sulfuric acid, phosphoric acid, Nitric acid, formic acid, acetic acid, propionic acid, butyric acid, octanoic acid, adipic acid, ethanedioic acid, malonic acid, succinic acid, horse Come sour, tartaric acid, benzoic acid, phenylacetic acid, phthalic acid, terephthalic acid (TPA), valeric acid, caproic acid, capric acid, Stearic acid, palmitic acid, acrylic acid, tartaric acid, malic acid, citric acid, ascorbic acid, process time are 0.5 Hour was to 20 hours;
Acid atmosphere using hydrochloric acid, nitric acid, formic acid, acetic acid, propionic acid, ethanedioic acid be easy to volatilization inorganic acid or Organic acid, process time is 20 minutes to 18 hours.
8. the preparation method of the polyelectrolyte styptic powder based on chitosan oligosaccharide according to claim 2, its feature Be, step 3) compound polyelectrolyte by constant pressure and dry, drying under reduced pressure, spray drying, fluidized drying, One or more dryings in the dry technologies such as freeze-drying, infrared drying, desiccant dryness or microwave drying.
9. the preparation method of the polyelectrolyte styptic powder based on chitosan oligosaccharide according to claim 2, its feature It is, step 3) dried compound polyelectrolyte makes particle thin by pulverizer, ball mill or disintegrating machine Change, obtain chitosan oligosaccharide polyelectrolyte styptic powder.
CN201510524236.XA 2015-08-24 2015-08-24 Preparation method of chitosan oligosaccharide -based polyelectrolyte styptic powder Pending CN106693029A (en)

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CN113072698A (en) * 2021-03-09 2021-07-06 东莞市华盈新材料有限公司 Antibacterial high-temperature-resistant polyamide and synthesis method thereof
CN114522270A (en) * 2021-12-22 2022-05-24 季华实验室 Preparation method of styptic powder
CN114681626A (en) * 2022-04-26 2022-07-01 华北理工大学 PH/enzyme dual-response type mesoporous silicon-based drug carrier MSN @ HA, and preparation method, drug loading condition and targeting application thereof

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* Cited by examiner, † Cited by third party
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CN113072698A (en) * 2021-03-09 2021-07-06 东莞市华盈新材料有限公司 Antibacterial high-temperature-resistant polyamide and synthesis method thereof
CN113072698B (en) * 2021-03-09 2021-09-03 东莞市华盈新材料有限公司 Antibacterial high-temperature-resistant polyamide and synthesis method thereof
CN114522270A (en) * 2021-12-22 2022-05-24 季华实验室 Preparation method of styptic powder
CN114522270B (en) * 2021-12-22 2023-02-21 季华实验室 Preparation method of styptic powder
CN114681626A (en) * 2022-04-26 2022-07-01 华北理工大学 PH/enzyme dual-response type mesoporous silicon-based drug carrier MSN @ HA, and preparation method, drug loading condition and targeting application thereof
CN114681626B (en) * 2022-04-26 2023-05-16 华北理工大学 PH/enzyme double-response mesoporous silicon-based drug carrier MSN@HA, preparation method thereof, drug loading condition and targeting application

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Application publication date: 20170524