CN105536029B - A kind of preparation method of chitosan multi-porous styptic sponge - Google Patents
A kind of preparation method of chitosan multi-porous styptic sponge Download PDFInfo
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- CN105536029B CN105536029B CN201510990788.XA CN201510990788A CN105536029B CN 105536029 B CN105536029 B CN 105536029B CN 201510990788 A CN201510990788 A CN 201510990788A CN 105536029 B CN105536029 B CN 105536029B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
- A61L15/28—Polysaccharides or their derivatives
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/425—Porous materials, e.g. foams or sponges
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Abstract
The invention discloses a kind of preparation methods of chitosan multi-porous styptic sponge, include the following steps:Step 1, the preparation of solution;Step 2, the preparation of chitosan multi-porous styptic sponge, chitosan solution, gelatin solution and glycerite is taken to be thoroughly mixed in 25 DEG C of water bath conditions according to 3: 3: 1 volume ratio, obtain mixing milk white gel liquid, then calcium chloride solution is taken to be added, it is sufficiently stirred 30min in 25 DEG C of water bath conditions, tannic acid solution is taken to be added again, continue to stir 20min in 25 DEG C of water bath conditions, it obtains mixing red red gel liquid, calcium chloride solution and tannic acid solution distinguish accounting 0.5% and 0.01% in obtained mixing pellet red gel liquid;The red red gel liquid of mixing is taken, is poured into mold, pre-freeze 12h or more is in obtain chitosan multi-porous styptic sponge after ice cube shape, then vacuum freeze drying 48h.Advantageous effect is:Prepare simple, finished product chitosan content is high, can natural degradation, the fast, good anti-bacterial effect of anthemorrhagic speed etc..
Description
Technical field
The invention belongs to hemostatic material in medical use preparation field, the preparation side of specifically a kind of chitosan multi-porous styptic sponge
Method.
Background technology
For many years, more and more about the research of hemostatic material, mostly it is the hemostatic material that natural products can degrade in vivo
Material, such as Fibrin Glue, powdered collagen, gelfoam, but these materials all have some disadvantages, fiber egg
White glue is only limited to topical application, may infect the blood borne disease of human or animal in the blood plasma of people or mammal;Glue
Former albumen may lead to wound fever and allergy as a kind of foreign matter;Gelfoam bad mechanical property, is easily broken.Also one
The hemostatic material of a little foreign countries' imports, such as speed is yarn, expensive although haemostatic effect is good, is limited its scope of application.Cause
This, it is a kind of with good haemostatic effect, stronger antibiotic property, preferable wound healing promoting ability and can with degradation in vivo only
Blood material is particularly significant.
Currently, there is extensive research and application prospect as hemostatic material using chitosan as main component, have only
The different physiological roles such as blood, antibacterial, anticancer, lipid-loweringing, strengthen immunity and good histocompatbility and higher bioactivity,
And it is nontoxic, it is non-stimulated, it can be with natural degradation.Many researchers select chitosan to prepare porous hemostasis material, generally utilize relatively low
The acetum of concentration dissolves chitosan, is obtained by the method for freeze-drying.But the solubility of chitosan is relatively low, only
3%~4%.On the one hand the hemostatic material of relatively low chitosan concentration influences the haemostatic effect of hemostatic material, on the other hand influence to stop
The mechanical performance of blood material.In addition to this, acetic acid has human body larger irritation, and materials'use is increased as lytic agent
Insecurity.In order to improve the mechanical performance and bio-safety performance of material, it is necessary to select suitable natural biologic material
It is blended and is selected nontoxic crosslinking agent to be crosslinked, while needing to reduce or eliminate the containing in material of acetic acid
Amount.
As effective porous hemostasis material, suitable material or inadequate is selected, it is also necessary to by material preparation at tool
There is specified pore structure, there is stronger absorbent function.The method of general drilling has particle leaching, phase separation method, freeze-drying
Method, gas foaming method, sintering microballoon method etc., but suitable method for drilling how is selected, preparing has uniform pore size size, high
The pore structure of porosity, and the material with good hydrophily and some strength, are still a technical barrier.
Invention content
It is prepared simply technical problem to be solved by the invention is to provide a kind of, finished product chitosan content is high, can drop naturally
Solution, anthemorrhagic speed are fast, good anti-bacterial effect, nontoxic, non-stimulated, mechanical performance and bio-safety performance are good, pore size is uniform, high
The preparation method of the chitosan multi-porous styptic sponge of porosity.
The technical solution that the present invention solves above-mentioned technical problem is as follows:A kind of preparation side of chitosan multi-porous styptic sponge
Method includes the following steps:
Step 1, the preparation of solution:
1) chitosan solution is prepared, ascorbic acid is weighed and is added in distilled water, filled under 40 DEG C~50 DEG C water bath conditions
Divide stirring and dissolving, the ascorbic acid solution of 0.05mol/L~0.3mol/L is made;It measures acetic acid and is added to constant volume in volumetric flask,
The acetum that concentration expressed in percentage by volume is 0.1%~0.5% is made;Chitosan is weighed to be added in the ascorbic acid solution,
After being sufficiently mixed, the acetum is added, is stirred evenly under 40 DEG C~50 DEG C water bath conditions, obtaining mass percentage concentration is
5%~8% chitosan solution is preserved and is used, wherein the acetum being added accounts for the 0.2%~0.5% of total solution;
2) gelatin solution is prepared, gelatin is weighed and is added in distilled water, fully dissolved in 40 DEG C~85 DEG C water bath conditions,
The gelatin solution that mass percentage concentration is 0.5%~4% is made, preserves and uses;
3) glycerite is prepared, glycerine is weighed and is added in distilled water, stir evenly, it is 40% that mass percentage concentration, which is made,
~50% glycerite is preserved and is used;
4) prepare calcium chloride solution, weigh calcium chloride and be added in distilled water, be made mass percentage concentration be 10%~
30% calcium chloride solution is preserved and is used;
5) crosslinking agent is prepared, tannic acid is weighed and is added in distilled water, it is 0.5%~5% that mass percentage concentration, which is made,
Tannic acid solution is preserved and is used;
Step 2, the preparation of chitosan multi-porous styptic sponge:
Take the chitosan solution, gelatin solution and glycerite according to 3: 3: 1 volume ratio in 25 DEG C~50 DEG C water-baths
It is thoroughly mixed in condition, obtains mixing milk white gel liquid, then take the calcium chloride solution to be added, at 25 DEG C~50 DEG C
It is sufficiently stirred 30min~120min in water bath condition, then the tannic acid solution is taken to be added, in 25 DEG C~50 DEG C water bath conditions
Continue to stir 20min~50min, obtains mixing red red gel liquid, described in the obtained mixing pellet red gel liquid
Calcium chloride solution and tannic acid solution distinguish accounting 0.5%~4% and 0.01%~0.1%;Take the red red gel of the mixing
Liquid pours into mold, pre-freeze 12h or more be in ice cube shape, then vacuum freeze drying 48h~72h after obtain chitosan multi-porous hemostasis
Sponge.
The beneficial effects of the invention are as follows:Prepare simple, finished product chitosan content is high, can natural degradation, anthemorrhagic speed it is fast, anti-
Bacterium effect is good, nontoxic, non-stimulated, mechanical performance and have a safety feature, pore size uniformly (aperture is 100 μm~200 μm), high
Porosity.
Preferably, volumetric flask described in step 1 is the volumetric flask of 100ml, convenient for a small amount of acetum constant volume.
Preferably, the preservation of chitosan solution, glycerite, calcium chloride solution and tannic acid solution described in step 1 uses
Temperature environment is 30 DEG C~40 DEG C, it is ensured that the chitosan solution, glycerite, calcium chloride solution, tannic acid solution point
Minor structure stability is conducive to the preparation of chitosan multi-porous styptic sponge.
Preferably, the preservation temperature in use environment of step 1 institute gelatine solution is 30 DEG C~50 DEG C, it is ensured that the gelatin
The molecular structure stabilized of solution is conducive to the preparation of chitosan multi-porous styptic sponge.
Preferably, the pre-freezing temperature environment that red red gel liquid is mixed described in step 2 is -20 DEG C~-80 DEG C, it is ensured that institute
It is in ice cube shape that it is frozen, which to state the red red gel liquid of mixing, conducive to chitosan multi-porous styptic sponge is obtained.
Specific implementation mode
The principles and features of the present invention are described below, and the given examples are served only to explain the present invention, is not intended to limit
Determine the scope of the present invention.
A kind of embodiment 1, preparation method of chitosan multi-porous styptic sponge, includes the following steps:
Step 1, the preparation of solution:
1) chitosan solution is prepared, ascorbic acid is weighed and is added in distilled water, filled under 40 DEG C~50 DEG C water bath conditions
Divide stirring and dissolving, the ascorbic acid solution of 0.05mol/L~0.3mol/L is made;Acetic acid is measured to be added in 100ml volumetric flasks
The acetum that concentration expressed in percentage by volume is 0.1%~0.5% is made in constant volume;Chitosan is weighed to be added in ascorbic acid solution,
After being sufficiently mixed, acetum is added, is stirred evenly under 40 DEG C~50 DEG C water bath conditions, it is 5% to obtain mass percentage concentration
~8% chitosan solution is preserved and is used, wherein the acetum being added accounts for the 0.2%~0.5% of total solution;
2) gelatin solution is prepared, gelatin is weighed and is added in distilled water, fully dissolved in 40 DEG C~85 DEG C water bath conditions,
0.5%~4% gelatin solution is made, preserves and uses at 30 DEG C~50 DEG C;
3) glycerite is prepared, glycerine is weighed and is added in distilled water, stir evenly, obtained 40%~50% glycerine is molten
Liquid is preserved at 30%~40 DEG C and is used;
4) calcium chloride solution is prepared, calcium chloride is weighed and is added in distilled water, 10%~30% calcium chloride solution is made,
It preserves and uses at 30%~40 DEG C;
5) crosslinking agent is prepared, tannic acid is weighed and is added in distilled water, obtained 0.5%~5% tannic acid solution, 30%
It preserves and uses at~40 DEG C;
Step 2, the preparation of chitosan multi-porous styptic sponge:
Take the chitosan solution, gelatin solution and glycerite according to 3: 3: 1 volume ratio in 25 DEG C of water bath conditions
It is thoroughly mixed, obtains mixing milk white gel liquid, then take the calcium chloride solution to be added, filled in 25 DEG C of water bath conditions
Divide stirring 60min, then the tannic acid solution is taken to be added, continue to stir 50min in 25 DEG C of water bath conditions, it is red to obtain mixing pellet
Color coagulant liquid, the calcium chloride solution described in the obtained mixing pellet red gel liquid and tannic acid solution distinguish accounting
0.5% and 0.01%;The red red gel liquid of the mixing is taken, is poured into mold, pre-freeze 12h is in ice under -20 DEG C of temperature conditions
Chitosan multi-porous styptic sponge is obtained after bulk, then vacuum freeze drying 48h.
A kind of embodiment 2, preparation method of chitosan multi-porous styptic sponge, includes the following steps:
Step 1 is consistent with embodiment 1;
Step 2, the preparation of chitosan multi-porous styptic sponge:
Take the chitosan solution, gelatin solution and glycerite according to 3: 3: 1 volume ratio in 40 DEG C of water bath conditions
It is thoroughly mixed, obtains mixing milk white gel liquid, then take the calcium chloride solution to be added, filled in 40 DEG C of water bath conditions
Divide stirring 50min, then the tannic acid solution is taken to be added, continue to stir 40min in 40 DEG C of water bath conditions, it is red to obtain mixing pellet
Color coagulant liquid, the calcium chloride solution described in the obtained mixing pellet red gel liquid and tannic acid solution distinguish accounting 2%
With 0.05%;The red red gel liquid of the mixing is taken, is poured into mold, pre-freeze 12h is in ice cube shape under -50 DEG C of temperature conditions,
Again chitosan multi-porous styptic sponge is obtained after vacuum freeze drying 60h.
Embodiment 3, a kind of preparation method of chitosan multi-porous styptic sponge includes the following steps:
Step 1 is consistent with embodiment 1;
Step 2, the preparation of chitosan multi-porous styptic sponge:
Take the chitosan solution, gelatin solution and glycerite according to 3: 3: 1 volume ratio in 50 DEG C of water bath conditions
It is thoroughly mixed, obtains mixing milk white gel liquid, then take the calcium chloride solution to be added, filled in 50 DEG C of water bath conditions
Divide stirring 30min, then the tannic acid solution is taken to be added, continue to stir 20min in 50 DEG C of water bath conditions, it is red to obtain mixing pellet
Color coagulant liquid, the calcium chloride solution described in the obtained mixing pellet red gel liquid and tannic acid solution distinguish accounting
0.4% and 0.1%;The red red gel liquid of the mixing is taken, is poured into mold, pre-freeze 12h is in ice cube under -80 DEG C of temperature conditions
Chitosan multi-porous styptic sponge is obtained after shape, then vacuum freeze drying 72h.
Experiment case study 1:
Arteria auricularis hemostasis experiment is carried out with porous chitosan styptic sponge made from embodiment 1:Porous chitosan is stopped blooding
It is spare that sponge is cut into 30 × 30 × 5mm specifications, and New Zealand is taken to test White Rabbit, and anesthesia is fixed on operating table, and it is dynamic to shave off rabbit ear
Hair on arteries and veins takes left or right ear, cuts off arteria auricularis at away from have sharp ears 7cm, wipes floating blood, gently with porous chitosan styptic sponge
It pushes down, 200g weights is then taken to be pressed on styptic sponge, start timing, the gelfoam of market sale is selected in control, with market
The gelfoam of sale is compared, and bleeding stopping period shortening connects by about one time.
Experiment case study 2:
With porous chitosan styptic sponge liver hemostasis experiment made from embodiment 1:Porous chitosan styptic sponge is cut
It is spare at 30 × 30 × 5mm specifications, take the new blue White Rabbit of west experiment, anesthesia to be fixed on operating table, shave off the hair of rabbit abdomen,
The upper hepatic portion in abdomen, cuts the wound of about 4 centimeter lengths, takes out liver, cuts 1cm depths on liver, the wound of 1cm long,
It wipes liver surface and floats blood, wound is pushed down with porous chitosan styptic sponge, take 100g weights to be pressed on hemostasis sea, start to count
When, the gelfoam of market sale is selected in control, and compared with the gelfoam of market sale, bleeding stopping period shortening connects by about one time.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (5)
1. a kind of preparation method of chitosan multi-porous styptic sponge, which is characterized in that include the following steps:
Step 1, the preparation of solution:
1) chitosan solution is prepared, ascorbic acid is weighed and is added in distilled water, fully stirred under 40 DEG C~50 DEG C water bath conditions
Dissolving is mixed, the ascorbic acid solution of 0.05mol/L~0.3mol/L is made;It measures acetic acid and is added to constant volume in volumetric flask, be made
The acetum that concentration expressed in percentage by volume is 0.1%~0.5%;It weighs chitosan to be added in the ascorbic acid solution, fully
After mixing, the acetum is added, is stirred evenly under 40 DEG C~50 DEG C water bath conditions, it is 5% to obtain mass percentage concentration
~8% chitosan solution is preserved and is used, wherein the acetum being added accounts for the 0.2%~0.5% of total solution;
2) gelatin solution is prepared, gelatin is weighed and is added in distilled water, fully dissolved in 40 DEG C~85 DEG C water bath conditions, is made
The gelatin solution that mass percentage concentration is 0.5%~4% is preserved at 30 DEG C~50 DEG C and is used;
3) prepare glycerite, weigh glycerine and be added in distilled water, stir evenly, be made mass percentage concentration be 40%~
50% glycerite, lower preservation use;
4) calcium chloride solution is prepared, calcium chloride is weighed and is added in distilled water, it is 10%~30% that mass percentage concentration, which is made,
Calcium chloride solution, lower preservation use;
5) crosslinking agent is prepared, tannic acid is weighed and is added in distilled water, the tannin that mass percentage concentration is 0.5%~5% is made
Acid solution is preserved and is used;
Step 2, the preparation of chitosan multi-porous styptic sponge:
Take the chitosan solution, gelatin solution and glycerite according to 3: 3: 1 volume ratio in 25 DEG C~50 DEG C water bath conditions
In be thoroughly mixed, obtain mixing milk white gel liquid, then take the calcium chloride solution to be added, in 25 DEG C~50 DEG C water-baths
It is sufficiently stirred 30rnin~120min in condition, then the tannic acid solution is taken to be added, is relayed in 25 DEG C~50 DEG C water bath conditions
Continuous stirring 20min~50min, obtains mixing red red gel liquid, the chlorine described in the obtained mixing pellet red gel liquid
Change calcium solution and tannic acid solution distinguishes accounting 0.5%~4% and 0.01%~0.1%;The red red gel liquid of the mixing is taken,
It pours into mold, pre-freeze 12h or more is extra large in chitosan multi-porous hemostasis is obtained after ice cube shape, then vacuum freeze drying 48h~72h
It is continuous.
2. a kind of preparation method of chitosan multi-porous styptic sponge according to claim 1, which is characterized in that step 1 institute
State the volumetric flask that volumetric flask is 100ml.
3. a kind of preparation method of chitosan multi-porous styptic sponge according to claim 1 or 2, which is characterized in that step
One chitosan solution, glycerite, calcium chloride solution and tannic acid solution preservation temperature in use environment be 30 DEG C~
40℃。
4. a kind of preparation method of chitosan multi-porous styptic sponge according to claim 1 or 2, which is characterized in that step
The preservation temperature in use environment of one gelatine solution is 30 DEG C~50 DEG C.
5. a kind of preparation method of chitosan multi-porous styptic sponge according to claim 1 or 2, which is characterized in that step
The pre-freezing temperature environment of the two red red gel liquid of mixing is -20 DEG C~-80 DEG C.
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