CN103933601A - Novel chitosan composite styptic powder and preparation method thereof - Google Patents
Novel chitosan composite styptic powder and preparation method thereof Download PDFInfo
- Publication number
- CN103933601A CN103933601A CN201410131189.8A CN201410131189A CN103933601A CN 103933601 A CN103933601 A CN 103933601A CN 201410131189 A CN201410131189 A CN 201410131189A CN 103933601 A CN103933601 A CN 103933601A
- Authority
- CN
- China
- Prior art keywords
- chitosan
- calcium
- novel
- hemostatic powder
- compound hemostatic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses novel chitosan composite styptic powder and a preparation method thereof. The method comprises the following steps: dissolving chitosan of which the deacetylation degree is 50-80% and a calcium salt under an acid condition; carrying out alkaline coprecipitation, centrifuging, washing, dewatering, drying and crushing to obtain chitosan composite styptic powder; sieving and sterilizing to obtain the novel chitosan composite styptic powder. The chitosan styptic powder disclosed by the invention is capable of stopping bleeding quickly, and bonding and sealing a tissue wound, especially has a good hemostatic effect under the condition of large bleeding amount, and has antibacterial and analgesic effects. The preparation method disclosed by the invention is simple and fast in process, high in productivity, low in cost, free of pollution to environment, mild in reaction condition, stable in quality and applicable to industrialization.
Description
Technical field
The invention belongs to hemostatic material in medical use field, be specifically related to a kind of novel chitosan compound hemostatic powder and preparation method thereof.
Background technology
Coagulation process is very complicated, and the factor that participates in reaction approximately has 13, and calcium is exactly one of them.After handlebar eggshell among the people calcination, be used for hemostasis the practice, principle is exactly the effect of calcium.The anthemorrhagic performance of chitosan reported by lot of documents, and hemostatic mechanism is that the amino of positively charged is combined with electronegative erythrocyte and platelet surface, forms the grumeleuse of mucoadhesive and activates traditional approach that condenses.
Chitosan is by a kind of alkaline polysaccharide making after chitin deacetylase, owing to containing characteristic that amino makes it have multiple excellence in chitosan molecule as biocompatibility, biodegradable, there is hemostasis, antibacterial, anti-infectious function simultaneously, and can promote wound healing, this has all given the superperformance of chitosan as hemostatic material.The existing listing of hemostatic material product taking chitosan as substrate, but the chitosan hemostasia products of single component promotes the process that forms blood clot conventionally all to need a few minutes, so undesirable compared with massive hemorrhage situation lower hemostasia effect, be difficult to meet the requirement of war wound hemostasis and clinical quick-acting haemostatic powder, and preparation technology's more complicated, the production cycle of the product form such as sponge, membrane, binder are long, production cost is high.
Therefore, exploitation anthemorrhagic performance is good, to find the fast and convenient method of preparing high-quality chitosan compound hemostatic material very necessary.
Summary of the invention
The object of the invention is, in order to solve single chitosan styptic powder existing defect when compared with massive hemorrhage, provides a kind of novel hemostasis composite.It has multiple clotting mechanism, therefore has more excellent anthemorrhagic performance, can significantly shorten the healing time of wound, and the preparation method of this chitosan compound hemostatic powder is easy and simple to handle, and yield is high, and product purity is better, is applicable to industrialization and produces.
Realizing above-mentioned purpose technical scheme of the present invention is, by de-acetyl chitin generating chitosan, after chitosan and calcium salt dissolve under acid condition, makes chitosan hydrochlorate calcium through alkalization co-precipitation, centrifugal, washing, dehydration, dry, pulverizing, sterilizing.Deacetylating degree of chitosan is controlled at 50～80%, and the lower haemostatic effect of deacetylation is more obvious, but the co-precipitation effect that deacetylation can affect lower than 50% time.
Technical scheme of the present invention also relates to the preparation method of above-mentioned chitosan compound hemostatic powder, and the method comprises the following steps: (1) preparation has the chitosan of 50～80% deacetylations; (2) chitosan and calcium salt are dissolved under acid condition, filter, make the solution of homogeneous; (3) in above-mentioned uniform solution, add alkali, make chitosan and calcium salt co-precipitation, filter, centrifugal, dry, sieve, after sterilizing, make finished product.
The method that above-mentioned steps (1) is prepared deacetylation 50～80% chitosans is: chitin (cross 80 mesh sieves after product) is joined in 40～45% sodium hydroxide lye, 70 DEG C of stirring reaction 1.5h, filter, purified water washing is to neutral, 50 DEG C of forced air dryings, pulverize 80 mesh sieves, obtained the chitosan of deacetylation 50～80%.
The method that above-mentioned steps (2) is prepared chitosan salt and calcium salt uniform solution is: by chitosan and calcium chloride or calcium acetate or calcium lactate or calcium carbonate or calcium malate or Citric acid calcium dissolving jointly in acidic aqueous solution, remove by filter insoluble matter, make the uniform solution of chitosan salt and calcium salt, wherein the concentration of chitosan is 0.5～5%.
The method that above-mentioned steps (3) is prepared chitosan and calcium salt co-precipitation is: chitosan salt prepared by step (2) and calcium salt uniform solution neutralize with 1～10% aqueous slkali, make chitosan and calcium salt produce co-precipitation.Alkali used comprises the strong base-weak acid salt containing carbonate such as sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate.
Chitosan prepared by above-mentioned steps (3) and calcium salt coprecipitate filter, centrifugal, water washing is to neutral, dehydrated alcohol dehydration, 60 DEG C of forced air dryings 10 hours, cross 100 mesh sieves, packaging, sterilizing, obtain novel chitosan compound hemostatic powder.
The advantage that technical scheme of the present invention has comprises: (1) novel chitosan compound hemostatic powder has high viscosity, and the dynamic viscosity of the acetic acid solution of its 1% mass concentration is 500～8000mPaS.(2) the prepared novel chitosan compound hemostatic powder of the present invention, there is the double-hemostasis function function of chitosan and calcium, it can play anastalsis by number of ways, can obviously shorten clotting time, also has effect antibacterial, antibacterial, that ease pain, promote wound healing simultaneously.(3) the prepared novel chitosan compound hemostatic powder of the present invention, zoopery shows to have good biocompatibility, without allergy, stimulation and inflammatory reaction, and preparation method is simple, easy to use.
Detailed description of the invention
Embodiment 1
(1) chitosan preparation: take in the reaction bulb of 80 object chitin 200g as for 3L, add the sodium hydroxide solution of 1L40%, 70 DEG C of stirring reaction 1.5h, filter, ultrasonic 0.5h, purified water washing is to neutral, dry, pulverize 80 mesh sieves for subsequent use.Naoh concentration can be 30～60%, and consumption can be 600～2000ml, and reaction temperature can be 50～100 DEG C
(2) chitosan calcium preparation: the chitosan 20g that takes above-mentioned preparation, join in beaker, add 2 grams, calcium chloride, then add 1000ml purified water to stir 10min, slowly drip 10ml hydrochloric acid, stirring reaction 30min, add 0.1g active carbon to stir 10min, filter and remove active carbon and a small amount of insoluble matter, drip saturated solution of sodium carbonate and adjust pH7, obtain solid content.By deionized water wash to three for solid content, once, 60 DEG C of forced air drying 10h, pulverize dehydrated alcohol processed, cross 100 mesh sieves, and packaging sterilizing makes novel chitosan compound hemostatic powder.
Embodiment 2
(1) chitosan preparation: take in the reaction bulb of 80 object chitin 200g as for 3L, add the sodium hydroxide solution of 1.5L50%, 60 DEG C of stirring reaction 1h, filter, ultrasonic 0.5h, purified water washing is to neutral, dry, pulverize 80 mesh sieves for subsequent use.
(2) chitosan calcium compound hemostatic powder preparation: take 20 grams of the chitosans of above-mentioned preparation, join in beaker, add calcium acetate 2g, then add 1000ml purified water to stir 10min, slowly drip 15ml acetic acid, stirring reaction 30min, add 0.2g activated carbon to stir 15min
Filter and remove active carbon and a small amount of insoluble matter, drip saturated solution of sodium bicarbonate and adjust pH7, obtain solid content.By deionized water wash to 3 for solid content, dehydrated alcohol processed 1 time, 60 DEG C of forced air drying 10h, pulverize, and cross 100 mesh sieves, and packaging sterilizing makes novel chitosan compound hemostatic powder.
Embodiment 3
(1) chitosan preparation: take in the reaction bulb of 80 object chitin 200g as for 3L, add the sodium hydroxide solution of 1.5L50%, 80 DEG C of stirring reaction 1h, filter, ultrasonic 0.5h, purified water washing is to neutral, dry, pulverize 80 mesh sieves for subsequent use.
Naoh concentration can be 30～60%, and consumption can be 600～2000ml, and reaction temperature can be 50～100 DEG C
(2) preparation of chitosan calcium: the chitosan 20g that takes above-mentioned preparation, join in beaker, add calcium carbonate calcium 2.5g, then add 1000ml purified water to stir 15min, slowly drip 10ml hydrochloric acid, add stirring reaction 30min, add 0.1g active carbon to stir 15min, filter and remove active carbon and a small amount of insoluble matter, drip saturated solution of potassium carbonate and adjust pH7, obtain solid content.By deionized water wash to 3 for solid content, dehydrated alcohol processed 1 time, 60 DEG C of forced air drying 10h, pulverize, and cross 100 mesh sieves, and packaging sterilizing makes novel chitosan compound hemostatic powder.
After the chitosan that the novel chitosan compound hemostatic powder preparing by embodiment 1,2 and 3 is is 50～80% by deacetylation and calcium salt dissolve under acid condition, through alkalization co-precipitation, centrifugal, washing, dehydration, dry, pulverize and make chitosan calcium, then through sieving, sterilizing makes.Embodiment 4
Novel chitosan compound hemostatic powder hemostasis trial.
Adopt Rabbit Femoral Artery Hemorrhage Model.Experiment divides 4 groups: 1. medical absorbent cotton/gauze matched group; 2. chitosan calcium group; 3. chitosan hydrochlorate group; 4. novel chitosan compound hemostatic powder group.Every group of 10 animals.
The results are shown in following table:
Above-mentioned experimental result shows, the haemostatic effect of novel chitosan compound hemostatic powder is obviously better than medical absorbent cotton/gauze, chitosan calcium and chitosan hydrochlorate experimental group, the haemostatic effect of novel chitosan compound hemostatic powder is better, wide as a kind of medical hemostatic product development market prospect.
Above-described embodiment is only explanation technical conceive of the present invention and feature, and its object is to allow person skilled in the art can understand content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalences that spirit is done according to the present invention change or modify, within all should being encompassed in protection scope of the present invention.
Claims (7)
1. a novel chitosan compound hemostatic powder, it is characterized in that it is made up of chitosan and calcium, preparation method is, chitosan and calcium salt are dissolved under acid condition, adopt chemical coprecipitation technique, under alkali condition, produce co-precipitation, precipitate through centrifugal, wash, dewater, be dried, sieve, sterilizing makes.
2. novel chitosan compound hemostatic powder according to claim 1, it is characterized in that calcium content is 0.1～10% (W/W), chitosan-containing 50%～98% (W/W), the deacetylation of chitosan is 50%～80%, weight average molecular weight 100,000～1,000,000.
3. novel chitosan compound hemostatic powder according to claim 1, is characterized in that calcium salt is one or both and the two or more mixture in calcium chloride, calcium acetate, calcium carbonate, calcium lactate, calcium malate, Citric acid calcium.
4. novel chitosan compound hemostatic powder according to claim 1, is characterized in that acid used is hydrochloric acid, acetic acid; Alkalization agents useful for same is sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate and the strong base-weak acid salt containing carbonate.
5. novel chitosan compound hemostatic powder according to claim 1, the amount that it is characterized in that dissolving the acid used of 1g chitosan is 0.5～2ml.
6. novel chitosan compound hemostatic powder according to claim 1, is characterized in that preparation process is used comminution by gas stream, 60Co radiation sterilization.
7. novel chitosan compound hemostatic powder according to claim 1, is characterized in that preparation process chitosan used is the chitin being extracted by shrimp, Eriocheir sinensis, fly, maggot shell, then makes through deacetylation, or made by synthetic.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410131189.8A CN103933601B (en) | 2014-04-03 | 2014-04-03 | A kind of shitosan compound hemostatic powder and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410131189.8A CN103933601B (en) | 2014-04-03 | 2014-04-03 | A kind of shitosan compound hemostatic powder and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103933601A true CN103933601A (en) | 2014-07-23 |
| CN103933601B CN103933601B (en) | 2016-09-07 |
Family
ID=51181645
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410131189.8A Active CN103933601B (en) | 2014-04-03 | 2014-04-03 | A kind of shitosan compound hemostatic powder and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103933601B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104721222A (en) * | 2015-04-02 | 2015-06-24 | 石家庄亿生堂医用品有限公司 | Plant polysaccharide protective washing solution |
| CN105031708A (en) * | 2015-08-25 | 2015-11-11 | 东莞市达庆医疗器械有限公司 | Rapid hemostatic powder for injury and preparation method of rapid hemostatic powder |
| CN109529094A (en) * | 2018-11-05 | 2019-03-29 | 首都师范大学 | A kind of efficient hemostatic material and preparation method thereof can promote wound healing |
| CN115177781A (en) * | 2022-07-13 | 2022-10-14 | 温州市安多多医疗器械有限公司 | Chitosan-based hemostatic antibacterial powder, preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1814625A (en) * | 2005-11-26 | 2006-08-09 | 刘万顺 | Method for preparing calcium chitosan and itsuse for wound hemostasis |
| CN101730524A (en) * | 2007-04-21 | 2010-06-09 | 史密夫及内修公开有限公司 | A foam material for medical use and method for producing same |
-
2014
- 2014-04-03 CN CN201410131189.8A patent/CN103933601B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1814625A (en) * | 2005-11-26 | 2006-08-09 | 刘万顺 | Method for preparing calcium chitosan and itsuse for wound hemostasis |
| CN101730524A (en) * | 2007-04-21 | 2010-06-09 | 史密夫及内修公开有限公司 | A foam material for medical use and method for producing same |
Non-Patent Citations (1)
| Title |
|---|
| 曹佐英等: "微波能促进壳聚糖钙离子配合物的制备研究", 《食品工业科技》, vol. 21, no. 2, 31 December 2000 (2000-12-31), pages 11 - 13 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104721222A (en) * | 2015-04-02 | 2015-06-24 | 石家庄亿生堂医用品有限公司 | Plant polysaccharide protective washing solution |
| CN105031708A (en) * | 2015-08-25 | 2015-11-11 | 东莞市达庆医疗器械有限公司 | Rapid hemostatic powder for injury and preparation method of rapid hemostatic powder |
| CN105031708B (en) * | 2015-08-25 | 2018-03-23 | 东莞市达庆医疗器械有限公司 | A kind of wound rapid hemostasis powder and preparation method thereof |
| CN109529094A (en) * | 2018-11-05 | 2019-03-29 | 首都师范大学 | A kind of efficient hemostatic material and preparation method thereof can promote wound healing |
| CN115177781A (en) * | 2022-07-13 | 2022-10-14 | 温州市安多多医疗器械有限公司 | Chitosan-based hemostatic antibacterial powder, preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103933601B (en) | 2016-09-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106620824A (en) | Preparation method for efficient anti-bacterial composite hemostatic sponge | |
| JP7288108B2 (en) | Method for producing chitosan with low endotoxin | |
| CN103933601A (en) | Novel chitosan composite styptic powder and preparation method thereof | |
| CN105597144A (en) | Absorbable collagen styptic powder and preparing method thereof | |
| CN103055343B (en) | Potato starch-hyaluronic acid composite hemostatic powder and preparation method thereof | |
| CN106474523A (en) | Preparation method based on the polyelectrolyte sponge wound dressing of carboxymethyl chitosan | |
| CN103721247B (en) | The preparation method of collagen-based compound hemostatic powder | |
| CN104211833A (en) | Preparation method of chitosan | |
| CN106178088A (en) | A kind of preparation method of styptic powder | |
| CN111518296A (en) | Preparation method of chitosan membrane material | |
| CN106466492A (en) | A kind of preparation method of the polyelectrolyte styptic powder based on carboxymethyl chitosan | |
| CN104874011A (en) | Hemostatic and preparation method and application thereof | |
| CN104208741A (en) | Chitosan based adhesive bandage | |
| CN102886066B (en) | Preparation method of calcium-containing soluble hemostatic material | |
| CN106822987A (en) | A kind of porous ball hemostatic material preparation method of shitosan alginate | |
| CN105107006B (en) | A kind of degradable starch-based hemostatic material and its preparation method and application | |
| CN104069535B (en) | A kind of Preparation method and use of biological activity composite membrane bleeding-stopping dressing | |
| CN102585255A (en) | Pectin/cellulose hydrogel material and preparation method thereof | |
| CN106822986B (en) | A kind of preparation method of the porous ball hemostatic material of chitosan-agar oligosaccharide | |
| CN109646707A (en) | A kind of rapid hemostatic material and preparation method thereof | |
| CN106474524A (en) | A kind of degradable starch sthptic sponge and preparation method thereof | |
| CN106693029A (en) | Preparation method of chitosan oligosaccharide -based polyelectrolyte styptic powder | |
| CN103919119B (en) | Double glue Ganoderma spore powder with cellular wall broken of a kind of antioxidative and preparation method thereof | |
| CN103690956A (en) | Hemostatic powder and preparation method thereof | |
| CN105061695A (en) | Preparation method of Salicornia europaea salt-tolerant water-retaining agent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |