CN103893204B - A kind of preparation method of chitosan hydrochloride calcium styptic powder - Google Patents
A kind of preparation method of chitosan hydrochloride calcium styptic powder Download PDFInfo
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- CN103893204B CN103893204B CN201410131204.9A CN201410131204A CN103893204B CN 103893204 B CN103893204 B CN 103893204B CN 201410131204 A CN201410131204 A CN 201410131204A CN 103893204 B CN103893204 B CN 103893204B
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Abstract
The present invention has introduced a kind of preparation method of chitosan hydrochloride calcium styptic powder. It, filters through deacetylation taking chitin as raw material, washing, dry, pulverize and sieve, prepare the shitosan of certain deacetylation, then shitosan, calcium chloride water are mixed with organic solvent, make shitosan fully swelling, add hydrochloric acid to stir, make mixture homogeneous reaction, finally by filtration, washing, dry, pulverize, packaging and sterilizing make the chitosan hydrochloride calcium styptic powder of finished product. Chitosan hydrochloride calcium styptic powder prepared by this method, can play anastalsis by number of ways, can obviously shorten the clotting time, has effect antibacterial, that ease pain, promote wound healing. Compared with traditional preparation method, that this method has is easy and simple to handle, process stabilizing, productive rate is high, cost is low, reaction condition is gentle, can keep preferably the advantage of chitosan molecule parameter.
Description
Technical field
The invention belongs to biomedical materials field, relate to specifically a kind of preparation method of chitosan hydrochloride calcium styptic powder.
Background technology
Shitosan is a kind of natural polymer alkaline polysaccharide, has that natural source is abundant, an advantage such as good stability, bioaffinity are good, biodegradable, safety non-toxic, broad-spectrum antiseptic, the suitable bio-medical material that is developed as. Many functions of shitosan, water-soluble with it with to carry positive charge closely related, can generate salt by shitosan and organic acid or inorganic acid reaction, make wound healing promoting agent and hemostatic material. At present existing multiple simple chitose haemostatic, as chitosan sponge, chitosan gel rubber, shitosan dry powder, shitosan tourniquet bandage etc., and apply, but simple shitosan hemostasia products promotes the process that forms blood clot conventionally all to need a few minutes, so undesirable to larger Bleeding.
In hemostasis, the effect of calcium ion is very crucial, calcium ion is one of 13 clotting factor, factor can be transformed into fibrin ferment, this is also a process of blood clotting, on chitosan hydrochloride, introducing calcium ion will increase hemostasis speed, and this also has great significance to short blood coagulation.
As shitosan is mixed with the powdery solid of calcium chloride, calcium acetate, calcium gluconae, calcium lactate, calcium malate or calcium citrate, can make after treatment chitosan calcium. Our experimental study shows, chitosan calcium prepared by this method has some defects, for example: cause more greatly product calcium content inhomogeneous because the inorganic salts such as shitosan and calcium chloride density differs; Shitosan density is less and water insolublely make it stick ability; Calcium adsorption reaction mostly occurs on chitosan particle surface, and adsorption rate is subject to the impact of granular size larger, and uniformity is also affected.
In order to overcome these defects, first we adopt the method that adds organic solvent, shitosan occurred swelling, and calcium more easily permeates, is adsorbed on the inside of chitosan molecule, and calcium content is more even, and can improve the ability that continues efficient hemostasis; Moreover we adopt highly acid hydrochloric acid to make shitosan protonated, increase from face the ability of sticking.
Summary of the invention
The object of the invention is the defect in order to overcome existing hemostatic material, a kind of preparation method of the hemostatic material chitosan hydrochloride calcium styptic powder that has multiple hemostasis approach is provided, the chitosan hydrochloride calcium styptic powder of preparing through the method can shorten the clotting time, improve haemostatic effect, promote wound healing, and develop as a kind of new type hemostat, promote its application in wound and operation.
The technical scheme of the present invention that realizes above-mentioned purpose is: it is in 30 ~ 50% sodium hydroxide solution that the chitin of certain particle size is joined to concentration, and 60 ~ 80 DEG C of stirring reaction 1 ~ 5h, filter, filter cake, dry, pulverize to neutral with purified water washing, sieve, obtain shitosan powder; The calcium chloride water that is 1 ~ 10% by concentration mixes in the ratio of 1:3 ~ 1:5 with organic solvent, add shitosan powder by 5 ~ 30ml/g, ultrasonic 5 ~ 20min, leaves standstill 0.5 ~ 2h, be warming up to 20 ~ 50 DEG C, add hydrochloric acid to stir, make mixture homogeneous reaction 0.5 ~ 4h, filter, solid organic solvent washing, vacuum drying is pulverized, packaging, and sterilizing obtains the chitosan hydrochloride calcium styptic powder of finished product; Wherein organic solvent used is one or more the combination in ethanol, propyl alcohol, isopropyl alcohol, acetone.
The preparation method of the chitin of certain particle size is: (1) cleans prawn carapace, removes attachment, dries and grinds, and the HCl solution that is 2 ~ 10% by concentration under room temperature soaks 20 ~ 48h, filters, and purified water is washed till neutrality; (2) joining concentration is in 60 ~ 80 DEG C of water-baths, to react 4 ~ 6h in 10 ~ 20% NaOH solution, filters, and purified water is washed till neutrality, obtains chitin crude product; (3) KMnO with 8 ~ 12g/L by chitin crude product4Solution soaks 1 ~ 2h, filters, and KMnO is removed in purified water eccysis4, decolour in 60 ~ 70 DEG C of stirred in water bath with the oxalic acid aqueous solution of 5 ~ 10g/L, be washed to neutrality, dry, pulverize, cross 80 mesh sieve, obtain chitin powder.
Technical scheme of the present invention has advantages of: (1) ultrasonic processing can improve calcium content; (2) calcium chloride water adds organic solvent, can control the adsorbance of calcium, and preparation process reappearance is greatly improved; (3) acidification makes shitosan protonated, thereby has the ability of better sticking; (4), compared with traditional preparation method, it is fast and convenient that this method has operation, stable preparation process, and productive rate is high, and cost is low, and reaction condition gentleness can keep the molecular parameter of shitosan, preferably as molecular weight, deacetylation etc.; (5) product of preparing is protonated even, has water-soluble and solubility in acid, and its aqueous solution pH is stable.
Chitosan hydrochloride calcium styptic powder of the present invention can play anastalsis by number of ways, comprise the red blood cell acting in blood, suppress solution fibrin in body, activate fibrin ferment, thereby the anastalsis of playing, can obviously shorten the clotting time, also there is effect antibacterial, antibacterial, that ease pain, promote wound healing simultaneously.
Detailed description of the invention
Embodiment 1
(1) preparation of shitosan: the chitin 100g that took 80 mesh sieve is placed in beaker, adds in the sodium hydroxide solution of 600ml40%, and 75 DEG C of stirring reaction 1.5h filter, collect solid, with purified water washing, to neutral, 60 DEG C dry, pulverize, cross 80 mesh sieve, make shitosan powder.
(2) preparation of chitosan hydrochloride calcium: take the shitosan 20g of above-mentioned preparation, join in the mixed solution of 300ml calcium chloride water and ethanol, the concentration of calcium chloride is 5%, the ratio of calcium chloride water and ethanol is 1:5, under room temperature, stirs, and ultrasonic 5min, place 2h, then the water-bath that is placed in 40 DEG C adds 10ml concentrated hydrochloric acid stirring reaction 2h, filters twice of absolute ethanol washing of solid, vacuum drying, pulverize packaging60Co radiation sterilization obtains chitosan hydrochloride calcium styptic powder.
Embodiment 2
(1) preparation of shitosan: with the step of embodiment 1 it (1)
(2) preparation of chitosan hydrochloride calcium styptic powder: other conditions are constant, changes the ethanol in embodiment 1 they (2) into isopropyl alcohol, can make chitosan hydrochloride calcium styptic powder.
Embodiment 3
(1) preparation of shitosan: with the step of embodiment 1 it (1)
(2) preparation of chitosan hydrochloride calcium: other conditions are constant, changes the ethanol in embodiment 1 they (2) into acetone, can make chitosan hydrochloride calcium styptic powder.
Embodiment 4
Chitosan hydrochloride calcium styptic powder hemostasis trial
Adopt Rabbit Femoral Artery Hemorrhage Model. Experiment divides 3 groups: (1) medical absorbent cotton/gauze control group; (2) chitosan calcium styptic powder experimental group; (3) chitosan hydrochloride calcium styptic powder experimental group; Every group of 10 animals.
The results are shown in following table:
。
Above-mentioned experimental result shows, the haemostatic effect of chitosan hydrochloride calcium styptic powder is obviously better than medical absorbent cotton/gauze and chitosan calcium styptic powder, can be used as a kind of novel bleeding-stopping dressing or styptic and develops.
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 Essence 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. the preparation method of a chitosan hydrochloride calcium styptic powder, it is characterized in that: the shitosan of being prepared 50～90% deacetylations by chitin, pulverized, sieved, mix with calcium chloride water, organic solvent, place 1～3h, add hydrochloric acid, in 20～50 DEG C of stirring reaction 0.5～4h, after filtration, washing, dry, pulverizing, packaging, sterilizing, obtain chitosan hydrochloride calcium styptic powder; Wherein organic solvent used is one or more the combination in ethanol, propyl alcohol, isopropyl alcohol, acetone.
2. the preparation method of chitosan hydrochloride calcium styptic powder according to claim 1, is characterized in that, the shitosan after pulverizing is crossed and is greater than 80 object sieves.
3. the preparation method of chitosan hydrochloride calcium styptic powder according to claim 1, is characterized in that, the ratio of calcium chloride water and organic solvent is 1:3～1:5, and the consumption of organic solvent and water is 5～30ml/g shitosan.
4. the preparation method of chitosan hydrochloride calcium styptic powder according to claim 1, is characterized in that, in calcium chloride water, the concentration of calcium chloride is 1～10%.
5. the preparation method of chitosan hydrochloride calcium styptic powder according to claim 1, it is characterized in that, after shitosan, calcium chloride water and organic solvent mix, through ultrasonic processing 5～20min, can make to shorten to standing time 0.5～2h, calcium content improves 0.1～1%.
6. the preparation method of chitosan hydrochloride calcium styptic powder according to claim 1, is characterized in that, the amount of hydrochloric acid is 0.3～1ml/g shitosan.
7. the preparation method of chitosan hydrochloride calcium styptic powder according to claim 1, is characterized in that, adopts60Co radiation sterilization.
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| CN1814625A (en) * | 2005-11-26 | 2006-08-09 | 刘万顺 | Method for preparing calcium chitosan and itsuse for wound hemostasis |
| CN101862469A (en) * | 2010-05-28 | 2010-10-20 | 武汉锐尔生物科技有限公司 | Chitosan derivative quick hemostasis granules and preparation method thereof |
| CN102028966A (en) * | 2010-12-29 | 2011-04-27 | 苏州方策科技发展有限公司 | Manufacturing method of chitosan hemostatic membrane with high water-absorbing swelling performance |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101029094B (en) * | 2007-04-12 | 2010-07-28 | 武汉大学 | Production of chitin chloride |
| WO2013096448A1 (en) * | 2011-12-22 | 2013-06-27 | Agenta Biotechnologies, Inc | Composition, preparation, and use of dense chitosan membrane materials |
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Patent Citations (3)
| 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 |
| CN101862469A (en) * | 2010-05-28 | 2010-10-20 | 武汉锐尔生物科技有限公司 | Chitosan derivative quick hemostasis granules and preparation method thereof |
| CN102028966A (en) * | 2010-12-29 | 2011-04-27 | 苏州方策科技发展有限公司 | Manufacturing method of chitosan hemostatic membrane with high water-absorbing swelling performance |
Non-Patent Citations (2)
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| 杨健等.壳聚糖的止血机理和应用.《国外医学生物医学工程分册》.2001,第24卷(第2期),第77-80页. * |
| 石凉等.壳聚糖止血材料及最新研究进展.《蚕业科学》.2009,第35卷(第4期),929-934页. * |
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