CN106620824B - A kind of preparation method of high-efficiency antimicrobial compound hemostatic sponge - Google Patents

A kind of preparation method of high-efficiency antimicrobial compound hemostatic sponge Download PDF

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CN106620824B
CN106620824B CN201611257131.3A CN201611257131A CN106620824B CN 106620824 B CN106620824 B CN 106620824B CN 201611257131 A CN201611257131 A CN 201611257131A CN 106620824 B CN106620824 B CN 106620824B
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preparation
emulsion
water
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CN106620824A (en
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李思东
王超
敖宁建
陈法锦
胡章
李普旺
李程鹏
廖铭能
欧阳茜茜
潘江球
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Guangdong Ocean University
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    • A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
    • A61L24/001—Use of materials characterised by their function or physical properties
    • A61L24/0015—Medicaments; Biocides
    • A—HUMAN NECESSITIES
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    • 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
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    • A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
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    • 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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Abstract

The invention discloses a kind of preparation method of high-efficiency antimicrobial compound hemostatic sponge, includes the following steps: that sodium chloride and quaternary salt is added in sodium alginate soln by S1., A liquid is prepared；S2. emulsifier is added in dispersion liquid, as B liquid；The calcium chloride solution of configuration 4 ~ 6% is as C liquid；S3. use emulsion-crosslinking method, be 1:(3 ~ 7 according to water-oil factor) volume ratio A liquid is added in B liquid, form emulsion after stirring, then C liquid be added in emulsion and is reacted, solidify, be centrifuged, washing obtains porous alginate drug bearing microsphere after dry；S4. aqueous solution is made in the molten water of chitosan hydrochloride, porous alginate drug bearing microsphere and haemostatic medicament obtained in S2 is added, carried out after being repeatedly freeze-dried, wash, sterilizing obtains the styptic sponge；Not only water imbibition is strong for styptic sponge of the invention, can stop blooding rapidly, blocks wound, but also can inhibit wound infection, effectively facilitates the healing of wound, evaded thrombosis risk.

Description

A kind of preparation method of high-efficiency antimicrobial compound hemostatic sponge
Technical field
The invention belongs to biomedical material technologies, more particularly, to a kind of high-efficiency antimicrobial compound hemostatic sponge Preparation method.
Background technique
Effectively hemostasis is to mitigate patient suffering, reduces the key of the death rate, and quickly and effectively stops blooding to become and solve this The emphasis of problem.The breakage of bodily tissue caused by various burst accidents, disaster can be inevitably encountered in daily life.Hemostasis is wound The first step of mouth processing, also directly affects subsequent wound healing.Currently, common hemostatic material has micropore class inorganic material (zeolite), more micropore starch, Fibrin Glue, gelfoam, carboxymethyl cellulose soluble stanching gauze, alpha-cyanoacrylate Although esters tissue glue etc., these materials have good haemostatic effect, but respectively have some limitations again.Gelatin and farther out Tissue adherence it is poor, be dissolved in and falling off from wound；The meeting after absorbing the moisture in blood of porous zeolite and more micropore starch Heat release increases the temperature of wound circumference and causes mouth of burning, it is difficult to heal, and the function of these dressing is relatively simple.
Therefore, it is very necessary to develop a kind of hemostatic material with antiseptic and quick-acting haemostatic powder effect.
Summary of the invention
The purpose of the present invention is to solve the having a single function of current hemostatic material, haemostatic effect is undesirable and there are thrombus The problem of forming risk, provides a kind of preparation method of high-efficiency antimicrobial compound hemostatic sponge.
Chitosan and alginic acid are combined together the compound hemostatic sponge of preparation by the present invention, both containing the amino of chitosan There is the carboxyl of sodium alginate again, effectively improves haemostatic effect under the collective effect of both functional groups.In addition, being mixed in chitosan Alginate porous microsphere has been closed, the defect of single chitosan styptic sponge is not only overcome, while having also overcomed alginic acid Salt porous microsphere is easily washed away by blood, reduces the possibility for causing thrombotic risk.Synergistic effect between the two is compound to be constituted A kind of hemostatic material of better effect.
Chitosan, alginic acid the ocean high molecular material natural as two kinds, not only have good biocompatibility, can Degradability, while there are also good hemostasis, antibacterial, the functions of promoting wound healing.Especially chitosan it is slightly sour under the conditions of band Positive charge can be very good that electrostatic interaction occurs with red blood cell in blood, to assemble a large amount of red blood cell in wound, accelerate Hemostasis, and sodium alginate formation gel can provide a wet environment for wound, be conducive to the healing of wound.Chitosan, Not only haemostatic effect is prominent but also avoids secondary injury caused by more conversion materials, energy for hemostatic material prepared by sodium alginate Overcome defect existing for traditional hemostatic material.
The purpose of the present invention is achieved through the following technical solutions:
The present invention provides a kind of preparation methods of high-efficiency antimicrobial compound hemostatic sponge, include the following steps:
S1. sodium chloride is added He quaternary alkylphosphonium salt, is prepared A liquid in sodium alginate soln；
S2. emulsifier is added in dispersion liquid, as B liquid；The calcium chloride solution of configuration 4 ~ 6% is as C liquid；
S3. use emulsion-crosslinking method, according to water-oil factor be 1:(3 ~ 7) volume ratio A liquid is added in B liquid, after stirring Emulsion is formed, then C liquid is added in emulsion and is reacted, is solidified, is centrifuged, washing obtains porous alginate after dry Drug bearing microsphere；
S4. the molten water of chitosan hydrochloride is made aqueous solution, be added in S2 porous alginate drug bearing microsphere obtained and Haemostatic medicament, carries out after being repeatedly freeze-dried, washs, and sterilizing obtains the high-efficiency antimicrobial compound hemostatic sponge；
The mass concentration of sodium alginate soln is 1.5 ~ 3%, and the mass-volume concentration of sodium chloride is 0.03 ~ 0.07g/L, season The concentration of phosphonium salt is 1.5 ~ 2.5 g/L；The mass ratio of porous alginate drug bearing microsphere and chitosan hydrochloride obtained in S4 For 1:(15 ~ 25).
For the present invention first using sodium alginate as carrier material, sodium chloride is pore-foaming agent, and calcium chloride is crosslinking agent, high-efficiency antimicrobial Ji quaternary alkylphosphonium salt is model drug, porous drug bearing microsphere is prepared using emulsion-crosslinking method, then by microballoon and Chinese medicine field thistle according to one Fixed weight ratio is added in chitosan hydrochloride solution, is freeze-dried after mixing, and last sterilized processing obtains efficient Antibacterial anti hemorrhagic sponge.
Preferably, the mass concentration of sodium alginate soln is 2% in S1, and the mass-volume concentration of sodium chloride is 0.05g/L, The concentration of quaternary alkylphosphonium salt is 2.0 g/L.
Preferably, dispersion liquid described in S2 is atoleine or isooctane, and the emulsifier is 3%span80 and 1% Tween80。
Preferably, 5% calcium chloride solution is configured as C liquid.
Preferably, emulsion-crosslinking method is used in S3, and A liquid is added in B liquid according to the volume ratio that water-oil factor is 1:5.
Preferably, the molecular weight of chitosan hydrochloride is 100,000 in S4, deacetylation 85%.
Preferably, the aqueous solution that mass volume ratio is 2% is made in the molten water of chitosan hydrochloride.
Preferably, the haemostatic medicament is Chinese medicine field thistle.
Preferably, then the freeze-drying operation is freeze-dried for 24 hours for first at -20 DEG C of pre-freeze 6h in -70 DEG C.
Preferably, the disinfecting action is to radiate 3 ~ 5h using ultraviolet lamp.
Compared with prior art, the invention has the following beneficial effects:
1, the present invention is using natural macromolecule polysaccharide, has good biocompatibility, biodegradable, nontoxic Etc. characteristics.
2, alginate porous microsphere is mixed with styptic sponge by the present invention, no It is only capable of improving the mechanical property of sponge, moreover it is possible to its water absorption and swelling is improved, so as to the visible component in rapid concentration blood, contracting Short bleeding stopping period reduces amount of bleeding.
3, quaternary alkylphosphonium salt antibacterial agent is also embedded in alginate microsphere by the present invention, and such microballoon plays certain delay to it Effect is released, so as to inhibit wound infection for a long time, promotes wound healing.
4, the present invention had both played quick-acting haemostatic powder and had efficiently resisted by porous alginate drug bearing microsphere in chitosan sponge The effect of bacterium wound healing promoting, and evaded material and entered the thrombosed risk of blood.
Specific embodiment
Further illustrate the present invention below in conjunction with specific embodiment, but embodiment the present invention is not done it is any type of It limits.Unless stated otherwise, the present invention uses reagent, method and apparatus is the art conventional reagents, method and apparatus.
Unless stated otherwise, agents useful for same and material of the present invention are commercially available.
Embodiment 1:
2g sodium alginate powder is dissolved in 100ml deionized water and obtains 2% sodium alginate soln, is added 0.005g's NaCl and 0.2g quaternary alkylphosphonium salt, stirs evenly, as A liquid；It is mixed that 3%span80 and 1%Tween80 preparation is added in atoleine Co-emulsifier solution is as B liquid；5% calcium chloride solution is configured as C liquid；Using emulsion-crosslinking method, according to water-oil factor 1:5 by A liquid It is added in B liquid, 15min is stirred under 470rpm revolving speed, 45 DEG C of waters bath with thermostatic control, form emulsion, then C liquid is added dropwise Into emulsion, control drop speed 30 drops/min reacts 20min again, isopropanol is added and solidifies 10min, is centrifuged, washes after being added dropwise It washs, dry to get porous alginate drug bearing microsphere；
2g chitosan hydrochloride (molecular weight be 100,000, deacetylation 85%) is dissolved in deionized water, 2%(w/v is made) The porous alginate microsphere and 0.05g Chinese medicine field thistle uniform stirring of the above-mentioned preparation of 0.1g is added, in -20 DEG C of pre-freezes in aqueous solution 6h, then in -70 DEG C freeze-drying for 24 hours, after being washed with lye and deionized water, again by material it is same as described above under the conditions of into Row pre-freeze and freeze-drying process.
The above-mentioned sponge being freeze-dried again is subjected to ultraviolet lamp radiation 4h sterilization treatment, finally obtains high-efficiency antimicrobial hemostasis Sponge.
Embodiment 2
2g sodium alginate powder is dissolved in 100ml deionized water and obtains 2% sodium alginate soln, the NaCl of 0.02g is added It with 1g quaternary alkylphosphonium salt, stirs evenly, as A liquid；3%span80 and 1%Tween80 is added in isooctane and prepares blended emulsifier Solution is as B liquid；5% calcium chloride solution is configured as C liquid；Using emulsion-crosslinking method, A liquid is added to B according to water-oil factor 1:10 In liquid, 15min is stirred under 470rpm revolving speed, 45 DEG C of waters bath with thermostatic control, forms emulsion, C liquid is then added dropwise to milkiness In liquid, speed 30 drops/min is dripped in control, reacts 30min after being added dropwise again, and isopropanol is added and solidifies 10min, centrifugation, is done washing It is dry to get porous alginate drug bearing microsphere；
2g chitosan hydrochloride (molecular weight be 100,000, deacetylation 90%) is dissolved in deionized water, 2%(w/v is made) The porous alginate microsphere and 0.2g Chinese medicine field thistle uniform stirring of the above-mentioned preparation of 0.4g is added, in -20 DEG C of pre-freezes in aqueous solution 12h, then in -80 DEG C of freeze-drying 48h, after being washed with lye and deionized water, again by material it is same as described above under the conditions of Carry out pre-freeze and freeze-drying process.
The above-mentioned sponge being freeze-dried again is subjected to ultraviolet lamp radiation 6h sterilization treatment, finally obtains high-efficiency antimicrobial hemostasis Sponge.
Embodiment 3
2g sodium alginate powder is dissolved in 100ml deionized water and obtains 2% sodium alginate soln, the NaCl of 0.01g is added It with 0.5g quaternary alkylphosphonium salt, stirs evenly, as A liquid；3%span80 and 1%Tween80 is added in atoleine and prepares mixing cream Agent solution is as B liquid；5% calcium chloride solution is configured as C liquid；Using emulsion-crosslinking method, A liquid is added according to water-oil factor 1:8 Into B liquid, 15min is stirred under 470rpm revolving speed, 45 DEG C of waters bath with thermostatic control, forms emulsion, C liquid is then added dropwise to cream In turbid, drop speed 30 drops/min is controlled, reacts 30min after being added dropwise again, isopropanol is added and solidifies 10min, be centrifuged, wash, Drying is to get porous alginate drug bearing microsphere；
2g chitosan hydrochloride (molecular weight be 100,000, deacetylation 88%) is dissolved in deionized water, 2%(w/v is made) The porous alginate microsphere and 0.1g Chinese medicine field thistle uniform stirring of the above-mentioned preparation of 0.3g is added, in -20 DEG C of pre-freezes in aqueous solution 8h, then in -75 DEG C of freeze-drying 36h, after being washed with lye and deionized water, again by material it is same as described above under the conditions of into Row pre-freeze and freeze-drying process.
The above-mentioned sponge being freeze-dried again is subjected to ultraviolet lamp radiation 5h sterilization treatment, finally obtains high-efficiency antimicrobial hemostasis Sponge.
Comparative example 1
The preparation method is the same as that of Example 1, unlike: the concentration of sodium alginate soln is 5%.
Comparative example 2
The preparation method is the same as that of Example 1, unlike: the concentration of the calcium chloride solution as C liquid is 8%.
Comparative example 3
The preparation method is the same as that of Example 1, unlike: the mass percent of chitosan hydrochloride is 15%.
Embodiment 4
Rush thrombotest has been carried out by the sponge sample obtained to embodiment 1 ~ 3.
It tests solution and uses D liquid, D liquid is the new fresh rabbit blood for adding anti-coagulants sodium citrate, the blood of simulation human body wound exudation Liquid.D liquid is stirred evenly by new fresh rabbit blood 10% sodium citrate of addition and is formulated.
Test method is that 3 test tubes is taken to be separately added into 1mlA liquid, heats 1h in 37 DEG C of waters bath with thermostatic control, is separately added into reality The sponge sample fragment 80mg that example 1 ~ 3 obtains is applied, heated at constant temperature is continued, rotates a test tube every half a minute, until in test tube Blood do not flow until, respectively record each group test tube in D liquid setting time.
Table 1 promotees thrombotest result
Group number Promote clotting time (min)
Embodiment 1 1.64
Embodiment 2 1.70
Embodiment 3 1.80
Comparative example 1 2.12
Comparative example 2 2.20
Comparative example 3 1.96
As seen from the above table, compound hemostatic sponge material of the invention has the performance of quick-acting haemostatic powder, and stopping than comparative example Blood effect is more preferable.

Claims (10)

1. a kind of preparation method of high-efficiency antimicrobial compound hemostatic sponge, which comprises the steps of:
S1. sodium chloride is added He quaternary alkylphosphonium salt, is prepared A liquid in sodium alginate soln；
S2. emulsifier is added in dispersion liquid, as B liquid；The calcium chloride solution of configuration 4 ~ 6% is as C liquid；
S3. use emulsion-crosslinking method, according to water-oil factor be 1:(3 ~ 7) volume ratio A liquid is added in B liquid, formed after stirring Then C liquid is added in emulsion and reacts by emulsion, solidify, and is centrifuged, washing, and porous alginate is obtained after dry and carries medicine Microballoon；
S4. chitosan hydrochloride is dissolved in water and aqueous solution is made, porous alginate load obtained in haemostatic medicament and S3 is added Medicine microballoon, carries out after being repeatedly freeze-dried, washs, and sterilizing obtains the high-efficiency antimicrobial compound hemostatic sponge；
The mass concentration of sodium alginate soln is 1.5 ~ 3%, and the mass-volume concentration of sodium chloride is 0.03 ~ 0.07g/L , quaternary alkylphosphonium salt Concentration be 1.5 ~ 2.5 g/L；The mass ratio of porous alginate drug bearing microsphere and chitosan hydrochloride obtained is 1 in S4: (15 ~ 25).
2. preparation method according to claim 1, which is characterized in that the mass concentration of sodium alginate soln is 2% in S1, The mass-volume concentration of sodium chloride is that the concentration of 0.05g/L , quaternary alkylphosphonium salt is 2.0 g/L.
3. preparation method according to claim 1, which is characterized in that dispersion liquid described in S2 is atoleine or different pungent Alkane, the emulsifier are 3%span80 and 1%Tween80.
4. preparation method according to claim 1, which is characterized in that configure 5% calcium chloride solution as C liquid.
5. preparation method according to claim 1, which is characterized in that use emulsion-crosslinking method in S3, be according to water-oil factor A liquid is added in B liquid by the volume ratio of 1:5.
6. preparation method according to claim 1, which is characterized in that the molecular weight of chitosan hydrochloride is 100,000 in S4, Deacetylation is 85%.
7. preparation method according to claim 1, which is characterized in that chitosan hydrochloride is dissolved in water, quality volume is made Than the aqueous solution for 2%.
8. preparation method according to claim 1, which is characterized in that the haemostatic medicament is Chinese medicine field thistle.
9. preparation method according to claim 1, which is characterized in that the freeze-drying operation is first in -20 DEG C of pre-freeze 6h, then for 24 hours in -70 DEG C of freeze-dryings.
10. preparation method according to claim 1, which is characterized in that the disinfecting action be using ultraviolet lamp radiation 3 ~ 5h。
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