CN107029280B - A kind of preparation method of chitin-alginic acid salt soft capsule grain hemostatic material - Google Patents
A kind of preparation method of chitin-alginic acid salt soft capsule grain hemostatic material Download PDFInfo
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- CN107029280B CN107029280B CN201710224039.5A CN201710224039A CN107029280B CN 107029280 B CN107029280 B CN 107029280B CN 201710224039 A CN201710224039 A CN 201710224039A CN 107029280 B CN107029280 B CN 107029280B
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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
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/04—Surgical adhesives or cements; Adhesives for colostomy devices containing macromolecular materials
- A61L24/08—Polysaccharides
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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
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/001—Use of materials characterised by their function or physical properties
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
- C08L5/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
-
- 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
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/04—Materials for stopping bleeding
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/04—Alginic acid; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
Abstract
The invention discloses a kind of preparation methods of chitin-alginic acid salt soft capsule grain hemostatic material.The method includes S1. to prepare chitosan solution and sodium alginate aqueous solution containing calcium acetylacetonate；S2. sodium alginate aqueous solution is subjected to vortex concussion, the above-mentioned chitosan solution containing calcium acetylacetonate is injected into sodium alginate aqueous solution using syringe needle, electrostatic encystation is cross-linked in situ 0.5 ~ 1.5h；S3. separate soft capsule, wash, pure water dialysis for 24 hours after under the conditions of 500 ~ 800W microwave drying to get soft capsule grain.Hemostatic material good biocompatibility prepared by the present invention, it is safe and non-toxic；Blood clotting can be facilitated rapidly, there is efficient styptic activity；With certain volume, it is not easily accessible blood and causes thrombotic risk.Meanwhile having excellent wound adaptability, especially suitable for deep, narrow and irregular wound hemostasis.Preparation process of the present invention is simple, easy to industrialized production.
Description
Technical field
The invention belongs to biomedical materials fields, stop blooding more particularly to a kind of chitin-alginic acid salt soft capsule grain
The preparation method of material.
Background technique
The main reason for uncontrollable big bleeding is war, traffic accident and other accident deaths.It develops in the short time
The emergency survival hemostatic material of hemostasis, can be effectively reduced death caused by bleeding.Traditional hemostasis cotton yarn, bandage etc. be not for
The haemostatic effect of the wounds such as regular shape, deep, narrow, arteriorrhexis is very unsatisfactory；Although styptic powder is applicable in excellent wound
Property, but easily enter blood obstruction distal aorta and flow to form thrombus.Therefore need it is a kind of be applicable on site with clinical emergency treatment,
Quickly, safe and efficient hemostatic material replaces traditional hemostatic material.
Chitosan is a kind of natural biological polysaccharide generated after chitin is deacetylated, is that the unique alkalinity of nature is more so far
Sugar, natural resources very abundant.Due to excellent biocompatibility, broad spectrum antibacterial, hemostasis wound healing promoting effect,
And it is biodegradable safe and non-toxic, it is widely used in the fields such as medicine, food, bioengineering.Alginate is brown from ocean
A kind of algal polysaccharides extracted in algae, it is nontoxic, there are good biological degradability and compatibility.Stop blooding since it has, is antitumor,
Immunological regulation, anti-oxidant, lipidemia, reduce blood glucose, it is anti-radiation the effects of, have been developed that into Medical coating in biomedicine field
The materials such as material, cartilage tissue engineered reparation, medicine sustained and controlled release carrier, protein and DNA carrier.It is contacted with wound fluid
When, with the sodium ion in body fluid ion exchange can occur for the calcium ion in alginate, make it have good hygroscopicity and at
Colloidality energy.The liquid of 20 times or more oneself volumes can be absorbed in alginate, and the exudate of wound can be absorbed, and reduces microorganism
It multiplies and its issuable peculiar smell of institute.When alginate material is used to contact wound surface, its phase interaction between wound
With meeting forms one layer of stable network gel in wound surface, can keep certain humidity, be maintained at wound surface temperature
37 DEG C or so, be conducive to the formation of granulation tissue and reinforce the function of macrophage, mitigate pain and decompose necrotic tissue, provides
The preferable healing environment of wound.
In hemostatic material product, U.S.'s Celox styptic powder, HemCon tourniquet bandage all mainly with chitosan be hemostasis
The alginate fiber dressing of trade name Sorbsan is just answered in the 80's of last century by agent, Courtaulds company, Britain
For field of stopping blooding, but there is some critical bottleneck problems, their extensive use, especially irregular shape are limited
The hemostasis of the wounds such as shape, deep, narrow, arteriorrhexis.2002, QuikClot Zeolite hemostatic powder was by FDA approval for seriously going out
The first aid of blood wound, but QuikClot styptic powder haves the defects that exothermic reaction can be more than 100 DEG C of high temperature in use, causes to create
Covering weave injury.Powdered hemostatic material is easy to remain in vascular lumen, and obstruction distal aorta flows to form thrombus.
WoundStat hemostat is approved in acquisition U.S. FDA in 2008 and is widely used in army in the same year, but discovery exists later
Cause the risk of tip thrombus into blood circulation system, considered based on bio-safety, U.S. army has announced to forbid forever for 2009
Use WoundStat.
Summary of the invention
The purpose of the present invention is overcoming the shortcomings of the prior art, while a kind of energy quick-acting haemostatic powder is provided, have both good
Good biology and histocompatbility, and solve particulate matter easily remain bring bio-safety hidden danger chitin-alginic acid salt it is soft
The preparation method of capsule grain hemostatic material.
Above-mentioned purpose of the invention is achieved by the following technical programs:
A kind of preparation method of chitin-alginic acid salt soft capsule grain hemostatic material, includes the following steps:
S1. chitosan solution and acetylacetone,2,4-pentanedione calcium solution are prepared respectively, and solvent is 1% ~ 3%(V/V) aqueous acetic acid, by shell
Glycan solution and the mixing of acetylacetone,2,4-pentanedione calcium solution, stir evenly to get the chitosan solution containing calcium acetylacetonate；
S2. sodium alginate aqueous solution is subjected to vortex concussion, 800 ~ 1500 turns/min of revolving speed of concussion will be upper using syringe needle
It states the chitosan solution containing calcium acetylacetonate to be injected into sodium alginate aqueous solution, electrostatic encystation is cross-linked in situ 0.5 ~ 1.5h；
S3. separate soft capsule, wash, pure water dialysis for 24 hours after under the conditions of 500 ~ 800W microwave drying to get soft capsule
Grain.
Crosslinking agent of the present invention improves material safety instead of conventional toxic crosslinking agent for calcium acetylacetonate；Instead of
Traditional calcium salt can be cross-linked in situ, when being cross-linked in situ since dissociation calcium ion concentration is moderate while material encystation
It is shaken using whirlpool, is crosslinked more uniformization, improve swelling behavior；Using microwave drying, instead of traditional heated-air drying
The methods of, the capsule grain of particulate form is obtained, has excellent wound adaptability, especially suitable for deep, narrow and irregular wound
Hemostasis.
Preferably, washing described in S3 refers to successively is washed soft capsule 3 times or more with acetone and 50% ethanol water respectively.
Preferably, the chitin-alginic acid salt soft capsule grain hemostatic material that the above method prepares includes following weight
Percent composition:
55% ~ 70% chitosan；
28% ~ 42% sodium alginate；
1% ~ 4% calcium acetylacetonate.
Preferably, it is in granular form when the soft capsule grain drying regime, average grain diameter is 0.8 ~ 2 mm, is approximate after swelling
Spherical or ellipse soft capsule, volume increase to original 8 ~ 15 times.
It is highly preferred that the soft capsule grain drying regime is particle, it is approximate after swelling that average grain diameter, which is 1.0 ~ 1.6 mm,
Spherical or ellipse soft capsule, volume increase to original 11 ~ 15 times.
Preferably, in the above method, the molecular weight of chitosan is 100 ~ 250 kDa, deacetylation 75% ~ 95%；It is described
Sodium alginate is food-grade or pharmaceutical grade, and viscosity is 400 ~ 1000 mPas.
Compared with prior art, the invention has the following beneficial effects:
Crosslinking agent improves material instead of conventional toxic crosslinking agent using calcium acetylacetonate in preparation method of the present invention
Safety；It can be while material encystation since calcium acetylacetonate dissociation calcium ion concentration is moderate instead of traditional calcium salt
It is cross-linked in situ, is shaken when being cross-linked in situ using whirlpool, be crosslinked more uniformization, improve swelling behavior；It is dry using microwave
It is dry, instead of traditional the methods of heated-air drying, the capsule grain of particulate form is obtained, has excellent wound adaptability, it is especially suitable
For deep, narrow and irregular wound hemostasis.Preparation process is simple, easy to industrialized production.
Specific embodiment
Explanation is further expalined to the present invention combined with specific embodiments below, the description thereof is more specific and detailed, but
It cannot be construed as a limitation to the scope of the present invention, as long as the form using equivalent substitution or equivalent transformation is obtained
The technical solution obtained should all include within the scope of protection of the claims of the present invention.
Embodiment 1
The preparation method of chitin-alginic acid salt soft capsule grain hemostatic material, comprising the following steps:
S1. 5.7 g chitosans (250 kDa of molecular weight, deacetylation are dissolved with 200 milliliters of 3%(V/V) aqueous acetic acid
75%) chitosan solution, is prepared；0.1 g calcium acetylacetonate is dissolved with 20 milliliters of 3%(V/V) aqueous acetic acid, prepares acetylacetone,2,4-pentanedione
Calcium solution；Said two devices solution is mixed, is stirred evenly to get the chitosan solution containing calcium acetylacetonate；It is pure water-soluble with 100 milliliters
It solves 4.2g sodium alginate (food-grade, 600 mPas of viscosity), sodium alginate aqueous solution is made；
S2. sodium alginate aqueous solution is placed on eddy mixer and is shaken, 1000 turns/min of revolving speed will using No. 7 syringe needles
The above-mentioned chitosan solution containing calcium acetylacetonate is injected into sodium alginate aqueous solution, and electrostatic encystation is cross-linked in situ 1h；
S3. soft capsule is separated, is successively washed respectively with acetone and 50% ethanol water, pure water is dialysed for 24 hours, and 500W is micro-
Wave is drying to obtain.
The soft capsule grain hemostatic material drying regime be particle, average grain diameter be 1.6 mm, can rapid water absorption and swelling, swelling
It is afterwards almost spherical or the soft capsule of ellipse, volume is 13 times originally.
Embodiment 2
The preparation method of chitin-alginic acid salt soft capsule grain hemostatic material, comprising the following steps:
S1. 6.0 g chitosans (200 kDa of molecular weight, deacetylation are dissolved with 200 milliliters of 2%(V/V) aqueous acetic acid
80%) chitosan solution, is prepared；0.3 g calcium acetylacetonate is dissolved with 20 milliliters of 2%(V/V) aqueous acetic acid, prepares acetylacetone,2,4-pentanedione
Calcium solution；Said two devices solution is mixed, is stirred evenly to get the chitosan solution containing calcium acetylacetonate；It is pure water-soluble with 100 milliliters
It solves 3.7g sodium alginate (pharmaceutical grade, 800 mPas of viscosity), sodium alginate aqueous solution is made；
S2. sodium alginate aqueous solution is placed on eddy mixer and is shaken, 800 turns/min of revolving speed will be upper using No. 7 syringe needles
It states the chitosan solution containing calcium acetylacetonate to be injected into sodium alginate aqueous solution, electrostatic encystation is cross-linked in situ 0.5h；
S3. soft capsule is separated, is successively washed respectively with acetone and 50% ethanol water, pure water is dialysed for 24 hours, and 600W is micro-
Wave is drying to obtain.
The soft capsule grain hemostatic material drying regime be particle, average grain diameter be 1.2 mm, can rapid water absorption and swelling, swelling
It is afterwards almost spherical or the soft capsule of ellipse, volume is 11 times originally.
Embodiment 3
The preparation method of chitin-alginic acid salt soft capsule grain hemostatic material, comprising the following steps:
S1. 6.3 g chitosans (150 kDa of molecular weight, deacetylation are dissolved with 200 milliliters of 2%(V/V) aqueous acetic acid
85%) chitosan solution, is prepared；0.2 g calcium acetylacetonate is dissolved with 20 milliliters of 2%(V/V) aqueous acetic acid, prepares acetylacetone,2,4-pentanedione
Calcium solution；Said two devices solution is mixed, is stirred evenly to get the chitosan solution containing calcium acetylacetonate；It is pure water-soluble with 100 milliliters
It solves 3.5g sodium alginate (pharmaceutical grade, 800 mPas of viscosity), sodium alginate aqueous solution is made；
S2. sodium alginate aqueous solution is placed on eddy mixer and is shaken, 1200 turns/min of revolving speed will using No. 7 syringe needles
The above-mentioned chitosan solution containing calcium acetylacetonate is injected into sodium alginate aqueous solution, and electrostatic encystation is cross-linked in situ 1h；
S3. soft capsule is separated, is successively washed respectively with acetone and 50% ethanol water, pure water is dialysed for 24 hours, and 600W is micro-
Wave is drying to obtain.
The soft capsule grain hemostatic material drying regime be particle, average grain diameter be 1.0 mm, can rapid water absorption and swelling, swelling
It is afterwards almost spherical or the soft capsule of ellipse, volume is 15 times originally.
Embodiment 4
The preparation method of chitin-alginic acid salt soft capsule grain hemostatic material, comprising the following steps:
S1. 5.5 g chitosans (100 kDa of molecular weight, deacetylation are dissolved with 200 milliliters of 1%(V/V) aqueous acetic acid
95%) chitosan solution, is prepared；0.4 g calcium acetylacetonate is dissolved with 20 milliliters of 1%(V/V) aqueous acetic acid, prepares acetylacetone,2,4-pentanedione
Calcium solution；Said two devices solution is mixed, is stirred evenly to get the chitosan solution containing calcium acetylacetonate；It is pure water-soluble with 100 milliliters
It solves 4.1g sodium alginate (pharmaceutical grade, 1000 mPas of viscosity), sodium alginate aqueous solution is made；
S2. sodium alginate aqueous solution is placed on eddy mixer and is shaken, 1500 turns/min of revolving speed will using No. 7 syringe needles
The above-mentioned chitosan solution containing calcium acetylacetonate is injected into sodium alginate aqueous solution, and electrostatic encystation is cross-linked in situ 1h；
S3. soft capsule is separated, is successively washed respectively with acetone and 50% ethanol water, pure water is dialysed for 24 hours, and 700W is micro-
Wave is drying to obtain.
The soft capsule grain hemostatic material drying regime be particle, average grain diameter be 2.2 mm, can rapid water absorption and swelling, swelling
It is afterwards almost spherical or the soft capsule of ellipse, volume is 8 times originally.
Embodiment 5
The preparation method of chitin-alginic acid salt soft capsule grain hemostatic material, comprising the following steps:
S1. 7.0 g chitosans (150 kDa of molecular weight, deacetylation are dissolved with 200 milliliters of 1%(V/V) aqueous acetic acid
85%) chitosan solution, is prepared；0.2 g calcium acetylacetonate is dissolved with 20 milliliters of 1%(V/V) aqueous acetic acid, prepares acetylacetone,2,4-pentanedione
Calcium solution；Said two devices solution is mixed, is stirred evenly to get the chitosan solution containing calcium acetylacetonate；It is pure water-soluble with 100 milliliters
It solves 2.8g sodium alginate (food-grade, 400 mPas of viscosity), sodium alginate aqueous solution is made；
S2. sodium alginate aqueous solution is placed on eddy mixer and is shaken, 900 turns/min of revolving speed will be upper using No. 7 syringe needles
It states the chitosan solution containing calcium acetylacetonate to be injected into sodium alginate aqueous solution, electrostatic encystation is cross-linked in situ 1.5h；
S3. soft capsule is separated, is successively washed respectively with acetone and 50% ethanol water, pure water is dialysed for 24 hours, and 800W is micro-
Wave is drying to obtain.
The soft capsule grain hemostatic material drying regime be particle, average grain diameter be 0.8 mm, can rapid water absorption and swelling, swelling
It is afterwards almost spherical or the soft capsule of ellipse, volume is 10 times originally.
Comparative example 1
The preparation method of chitin-alginic acid salt soft capsule grain hemostatic material, comprising the following steps:
S1. 7.0 g chitosans (150 kDa of molecular weight, deacetylation are dissolved with 200 milliliters of 1%(V/V) aqueous acetic acid
85%) chitosan solution, is prepared；0.2 g calcium chloride is dissolved with 20 milliliters of 1%(V/V) aqueous acetic acid, prepares calcium chloride solution；
Said two devices solution is mixed, is stirred evenly to get the chitosan solution of chloride containing calcium；With 100 milliliters of dissolved in purified water 2.8g seaweed
Sodium alginate aqueous solution is made in sour sodium (food-grade, 400 mPas of viscosity)；
S2. sodium alginate aqueous solution is placed on eddy mixer and is shaken, 900 turns/min of revolving speed will be upper using No. 7 syringe needles
It states the chitosan solution containing calcium acetylacetonate to be injected into sodium alginate aqueous solution, electrostatic encystation is cross-linked in situ 1.5h；
S3. soft capsule is separated, is successively washed respectively with acetone and 50% ethanol water, pure water is dialysed for 24 hours, and 800W is micro-
Wave is drying to obtain.
The soft capsule grain hemostatic material drying regime be particle, average grain diameter be 1.0 mm, can water absorption and swelling, be after swelling
The soft capsule of almost spherical or ellipse, volume are 3 times originally.
Comparative example 2
The preparation method of chitin-alginic acid salt soft capsule grain hemostatic material, comprising the following steps:
S1. 7.0 g chitosans (150 kDa of molecular weight, deacetylation are dissolved with 200 milliliters of 1%(V/V) aqueous acetic acid
85%) chitosan aqueous solution, is prepared；0.2 g calcium acetylacetonate is dissolved with 20 milliliters of 1%(V/V) aqueous acetic acid, prepares levulinic
Ketone calcium aqueous solution；Said two devices solution is mixed, is stirred evenly to get the chitosan aqueous solution containing calcium acetylacetonate；It is pure with 100 milliliters
2.8g sodium alginate (food-grade, 400 mPas of viscosity) is dissolved in water purification, and sodium alginate aqueous solution is made；
S2. sodium alginate aqueous solution is placed on magnetic stirring apparatus, 900 turns/min of revolving speed, is contained using No. 7 syringe needles by above-mentioned
The chitosan solution of calcium acetylacetonate is injected into sodium alginate aqueous solution, and electrostatic encystation is cross-linked in situ 1.5h；
S3. soft capsule is separated, is successively washed respectively with acetone and 50% ethanol water, pure water is dialysed for 24 hours, and 800W is micro-
Wave is drying to obtain.
The soft capsule grain hemostatic material drying regime be particle, average grain diameter be 3.5 mm, can water absorption and swelling, be after swelling
Gel piece in irregular shape, volume are 4 times originally.
Comparative example 3
The preparation method of chitin-alginic acid salt soft capsule grain hemostatic material, comprising the following steps:
S1. 7.0 g chitosans (150 kDa of molecular weight, deacetylation are dissolved with 200 milliliters of 1%(V/V) aqueous acetic acid
85%) chitosan aqueous solution, is prepared；0.2 g calcium acetylacetonate is dissolved with 20 milliliters of 1%(V/V) aqueous acetic acid, prepares levulinic
Ketone calcium aqueous solution；Said two devices solution is mixed, is stirred evenly to get the chitosan aqueous solution containing calcium acetylacetonate；It is pure with 100 milliliters
2.8g sodium alginate (food-grade, 400 mPas of viscosity) is dissolved in water purification, and sodium alginate aqueous solution is made；
S2. sodium alginate aqueous solution is placed on eddy mixer and is shaken, 900 turns/min of revolving speed will be upper using No. 7 syringe needles
It states the chitosan solution containing calcium acetylacetonate to be injected into sodium alginate aqueous solution, electrostatic encystation is cross-linked in situ 1.5h；
S3. soft capsule is separated, is successively washed respectively with acetone and 50% ethanol water, pure water is dialysed for 24 hours, air blast 80
It DEG C is drying to obtain.
The soft capsule hemostatic material drying regime be it is membranaceous, can water absorption and swelling, after swelling for almost spherical or ellipse
Soft capsule.
External clotting assay:
From new zealand rabbit auricular vein take blood in vacuum blood collection tube (containing sodium citrate anticoagulant, 3.8% sodium citrate:
Blood=1: 9), spare；The plastic test tube for taking cleaning transparent, the sample being separately added into 50mg above-described embodiment and comparative example, gently
Shaking test tube spreads out sample as far as possible.Blank cuvette makees negative control, and Yunnan Baiyao powder makees positive control, and every sample sets three test tubes
Do parallel test.Successively the fresh anticoagulant rabbit blood of 1 mL is added in above-mentioned test tube, smoothly moves into 37 DEG C of water-baths, starts to count
When；Every group of test tube is slowly tilted into primary (angle is less than 30 °) every 30s, until test tube is slowly inverted blood and is not flowed and is
Only, by second hand stop table, this group of clotting time is write down, the time surpasses 30 minutes and is denoted as " not blood coagulation ", and experimental data is with " x ± s " table
Show, as a result see the table below.
1 clotting assay result of table
| Sample | Form | Clotting time (s) |
| Blank control | —— | Not blood coagulation |
| Yunnan Baiyao | Powder | 256 ±4 |
| Embodiment 1 | Particle | 208±3 |
| Embodiment 2 | Particle | 224±5 |
| Embodiment 3 | Particle | 172±3 |
| Embodiment 4 | Particle | 231±3 |
| Embodiment 5 | Particle | 247±4 |
| Comparative example 1 | Particle | 511±5 |
| Comparative example 2 | Particle | 463±3 |
| Comparative example 3 | It is membranaceous | 417±6 |
As can be seen from Table 1, the chitin-alginic acid salt soft capsule grain hemostatic material blood coagulation activity of embodiment preparation is high,
It is shorter than the clotting time of Yunnan Baiyao, and partial size will not enter greatly blood, solve the easy lower tape of the particulate matters such as Yunnan Baiyao
The bio-safety hidden danger come, and it is safe and non-toxic.
Claims (5)
1. a kind of preparation method of chitin-alginic acid salt soft capsule grain hemostatic material, which comprises the steps of:
S1. chitosan solution and acetylacetone,2,4-pentanedione calcium solution are prepared respectively, and solvent is 1% ~ 3%(V/V) aqueous acetic acid, by chitosan
Solution and the mixing of acetylacetone,2,4-pentanedione calcium solution, stir evenly to get the chitosan solution containing calcium acetylacetonate；
S2. sodium alginate aqueous solution is subjected to vortex concussion, 800 ~ 1500 turns/min of revolving speed of concussion is contained using syringe needle by above-mentioned
The chitosan solution of calcium acetylacetonate is injected into sodium alginate aqueous solution, and electrostatic encystation is cross-linked in situ 0.5 ~ 1.5h；
S3. separate soft capsule, wash, pure water dialysis for 24 hours after under the conditions of 500 ~ 800W microwave drying to get soft capsule grain；
The soft capsule grain includes following weight percent composition:
55% ~ 70% chitosan；
28% ~ 42% sodium alginate；
1% ~ 4% calcium acetylacetonate.
2. the preparation method of chitin-alginic acid salt soft capsule grain hemostatic material according to claim 1, which is characterized in that
Washing refers to described in S3 is successively washed soft capsule 3 times or more with acetone and 50% ethanol water respectively.
3. the preparation method of chitin-alginic acid salt soft capsule grain hemostatic material according to claim 2, which is characterized in that
It is in granular form when the soft capsule grain drying regime, average grain diameter is 0.8 ~ 2 mm, is almost spherical or ellipse after swelling
Soft capsule, volume increase to original 8 ~ 15 times.
4. the preparation method of chitin-alginic acid salt soft capsule grain hemostatic material according to claim 3, which is characterized in that
The soft capsule grain drying regime be particle, average grain diameter be 1.0 ~ 1.6 mm, after swelling for almost spherical or ellipse it is soft
Capsule, volume increase to original 11 ~ 15 times.
5. the preparation method of chitin-alginic acid salt soft capsule grain hemostatic material according to claim 1, which is characterized in that
The molecular weight of chitosan is 100 ~ 250 kDa, deacetylation 75% ~ 95%；The sodium alginate is food-grade or pharmaceutical grade, is glued
Degree is 400 ~ 1000 mPas.
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| CN1810867A (en) * | 2006-02-16 | 2006-08-02 | 武汉理工大学 | Prepn of sodium alginate/chitosan mixture gel |
| CN101024094A (en) * | 2007-01-11 | 2007-08-29 | 南京零一新材料工程研究中心 | Biological-degradable chitosan porous hemostasis material and its preparing method |
| CN104548189A (en) * | 2015-01-28 | 2015-04-29 | 浙江三创生物科技有限公司 | Microsphere and application thereof in hemostasis of wound |
| CN105534952A (en) * | 2016-01-08 | 2016-05-04 | 福建师范大学 | Preparation method of composite porous microspheres of core-shell structure |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1810867A (en) * | 2006-02-16 | 2006-08-02 | 武汉理工大学 | Prepn of sodium alginate/chitosan mixture gel |
| CN101024094A (en) * | 2007-01-11 | 2007-08-29 | 南京零一新材料工程研究中心 | Biological-degradable chitosan porous hemostasis material and its preparing method |
| CN104548189A (en) * | 2015-01-28 | 2015-04-29 | 浙江三创生物科技有限公司 | Microsphere and application thereof in hemostasis of wound |
| CN105534952A (en) * | 2016-01-08 | 2016-05-04 | 福建师范大学 | Preparation method of composite porous microspheres of core-shell structure |
Non-Patent Citations (1)
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| 乙酰丙酮钙的制备、表征及其在热稳定剂中的应用;沈冠华等;《广东化工》;20141231;第41卷(第16期);第35-36页 |
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