CN104383586B - A kind of nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material and preparation method thereof - Google Patents
A kind of nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material and preparation method thereof Download PDFInfo
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Abstract
A kind of nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material and preparation method thereof, it relates to a kind of hemostatic material and preparation method thereof. The modifier that the object of the invention is to solve existing oxidized regenerated cellulose is deposited in use mammal skin and other body cells of contact position as hemostatic material and is produced excitant, and form the large granulation lump turning white in use location, hinder the bio-absorbable of material and anthemorrhagic performance to promote not high problem. A kind of nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material has the oxidized regenerated cellulose of lysine to prepare by nm of gold and surface grafting; Preparation method: one, oxidized regenerated cellulose chemical graft lysine; Two, preparation nm of gold aqueous dispersions; Three, the self assembly of nm of gold, obtains nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material. The present invention can obtain a kind of nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material and preparation method thereof.
Description
Technical field
The present invention relates to a kind of hemostatic material and preparation method thereof.
Background technology
Inevitably can there are in daily life various accidents, carrying out in emergency treatment and surgical procedure, all mayBecause massive haemorrhage causes malpractice even dead. Therefore, patient is local, and effectively quick-acting haemostatic powder is most important, effectively controlMake blood and reduce the important measures that the bleeding time becomes reduction mortality. Clinical conventional hemostatic material as hemostatic gauze,Stanch fibre, tourniquet bandage in use have limitation, as longer in bleeding stopping period, easily and wound adhesion and be difficult for changing dressings,Infection to wound and suppurate helpless. Quick-acting haemostatic powder and functional hemostasis are by the direction that is following haemostatic medicament development.
Conventional absorbable hemostatic material has Fibrin Glue, gelfoam, oxycellulose, microfibre collagen, shitosanAnd Sorbsan etc. Their mechanism of action and using method are not quite similar, and haemostatic effect also has difference. But, orderBefore the hemostatic gauze that is widely used be clinically the SURGICEL being produced by company of Johnson & Johnson of the U.S. (Johnson&Johnson)Series absorbable hemostatic product---SURGICELTM、SURGICELTMNu-Knit、SURGICELTMFibrillar，Claim again at home " speed is yarn ", the composition of above product is oxidized regenerated cellulose, and main difference is embodied in external manifestationForm, SURGICEL series of products have occupied extremely important status in the international market now, and have been subject to medical scienceDomain expert's consistent favorable comment. Meanwhile, domestic You Ji company has also produced similar hemostatic gauze, but due to materialIt is yarn that performance can not show a candle to speed, so mainly adopt clinically expensive import hemostatic material.
Oxidized regenerated cellulose is cellulosic derivative, has good anthemorrhagic performance, biodegradable performance and nontoxic, orderBefore be used to multiple industry, be included in medical field, generally adopt nitrogen oxide as oxidant, by cellulose unitHydroxyl oxidize on middle C-6 position is that carboxyl makes oxidized regenerated cellulose. When it uses as hemostatic material, carboxyl-content shouldBe 16%～24%, to ensure its haemostatic effect. Oxidized regenerated cellulose hemostatic mechanism is as follows: oxidized regenerated cellulose contactAfter blood, can adsorb a large amount of erythrocytes, then the acid carboxyl in oxidized regenerated cellulose structure can cause haemolysis,Erythrocyte dissolves, breaks, and discharges hemoglobin. Meanwhile, owing to containing ferric ion in hemoglobin, oxidationRegenerated cellulose can with Fe3+In conjunction with forming brown blob of viscose, sealing, stop up capillary end and stopping blooding. As can be seen here,The hemostasis of oxidized regenerated cellulose is a series of Biochemical Engineering, and carboxyl quantity in material structure hasLimit, therefore causes the anthemorrhagic speed of oxidized regenerated cellulose material relatively slow, causes such material cannot be applicable to artery etc.The massive haemorrhage situation at position.
Oxidized regenerated cellulose as the study on the modification of hemostatic material always in constantly making great efforts to carry out. The people such as Doub discloseThe method that adopts the aqueous solution of sodium acid carbonate or calcium acetate to neutralize oxidized regenerated cellulose, and use fibrin ferment impregnated carbonThe oxidized regenerated cellulose of acid hydrogen sodium neutralization, then freezes to process and be dried under this state, system to the fabric after dippingObtained a kind of efficient oxycellulose class operation hemostatic material. In United States Patent (USP), the people such as Saferstein has narrated useThe alcohol solution of salt of weak acid, as sodium acetate, is neutralized to pH value between 5～8 by oxidized regenerated cellulose, this methodNot only make oxidized regenerated cellulose can ambient-temp-stable store, and the sour sensitive materials of similar fibrin ferment on can load, enterAnd the anthemorrhagic performance of raising oxidized regenerated cellulose material. They also find simultaneously, and the people such as Doub adopt sodium acid carbonate neutralizationMethod can cause the gel of oxidized regenerated cellulose fabrics part, distortion, and cause the oxidation regeneration fiber of final neutralization to be knittedThe hot strength of thing is too low and cannot be applied in actual hemostasis. And the calcium acetate that the people such as Doub mention in patentAlthough the oxidized regenerated cellulose of neutralization has ensured original form of fabric, because material calcium content after neutralization is too high, makeWith producing excitant to the mammal skin of contact position and other body cells in process, and form large sending out in use locationWhite granulation lump, the bio-absorbable that hinders material.
In sum, although above achievement in research all the correlative study of oxidized regenerated cellulose is had a very big significance, simultaneouslyAlso make the anthemorrhagic performance of material obtain lifting to a certain degree, but lifting degree is generally less, improves effect poor;And the improvement method in research also can be to the mechanical strength of regenerated oxycellulose as styptic material and Bioabsorbable in the pastCan cause negative effect, for the anthemorrhagic performance promoting by a small margin, modified effect is lost more than gain.
Summary of the invention
The modifier that the object of the invention is to solve existing oxidized regenerated cellulose is deposited in use as hemostatic materialThe mammal skin of contact position and other body cells produce excitant, and form the large granuloma of turning white in use locationPiece, hinders the bio-absorbable of material and anthemorrhagic performance to promote not high problem, and provides a kind of nm of gold/lysine/oxidation againRaw cellulose compound hemostatic material and preparation method thereof.
A kind of nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material has lysine by nm of gold and surface graftingPrepared by oxidized regenerated cellulose; Described nm of gold and surface grafting have the mass ratio of the oxidized regenerated cellulose of lysine to be(0.01～0.5):100。
A preparation method for nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material, specifically complete according to the following stepsBecome:
One, oxidized regenerated cellulose chemical graft lysine: it is 1.0 × 10 that oxidized regenerated cellulose is immersed in to concentration-4g/mL～9.0×10-4In the lysine solution of g/mL, re-use oscillator oscillation treatment 1h～48h, obtain lysine water-solubleOxidized regenerated cellulose after immersion stain; Oxidized regenerated cellulose after lysine solution dipping is immersed in absolute ethyl alcohol4h～24h, re-uses absolute ethyl alcohol and washs 5 times～8 times, then is vacuum drying 24h～72h at-70～-20 DEG C in temperature,Obtaining surface grafting has the oxidized regenerated cellulose of lysine;
In oxidized regenerated cellulose described in step 1, carboxyl-content is 16%～24%;
The quality of the oxidized regenerated cellulose described in step 1 and concentration are 1.0 × 10-4g/mL～9.0×10-4The bad ammonia of g/mLThe volume ratio of aqueous acid is (0.0002g～0.02g): 1mL;
Two, preparation nm of gold aqueous dispersions: nm of gold is added to the water, then is that 60W～400W is ultrasonic at ultrasonic powerProcess 10min～45min, obtain nm of gold aqueous dispersions;
The quality of the nm of gold described in step 2 and the volume ratio of water are (0.01mg～0.2mg): 1mL;
Three, the self assembly of nm of gold: have the oxidized regenerated cellulose of lysine to join nm of gold aqueous dispersions surface graftingIn, be then ultrasonic processing 10min～60min under 200W～400W at ultrasonic power, re-use oscillator oscillation treatment1h～48h, obtains the oxidized regenerated cellulose of decorated by nano-gold; The oxidized regenerated cellulose of decorated by nano-gold is immersed in to nothingIn water-ethanol, 12h～36h, re-uses absolute ethyl alcohol and washs 5 times～8 times, then be immersed in absolute ethyl alcohol, ultrasonicPower is the ultrasonic processing of 160W～360W 20min～50min, re-uses absolute ethanol washing 3 times～5 times, finally in temperatureDegree, for vacuum drying 16h～48h at-70 DEG C～-20 DEG C, obtains nm of gold/lysine/oxidized regenerated cellulose compound hemostatic materialMaterial;
Surface grafting described in step 3 has the quality of oxidized regenerated cellulose and the body of nm of gold aqueous dispersions of lysineLong-pending than being (0.001g～0.1g): 1mL;
Nm of gold and surface grafting in nm of gold/lysine described in step 3/oxidized regenerated cellulose compound hemostatic materialThe mass ratio that has the oxidized regenerated cellulose of lysine is (0.01～0.5): 100.
Advantage of the present invention:
One, the present invention is intended to maintain on the basis of oxidized regenerated cellulose absorbable hemostatic material advantage, proposes one suitableeerSuitable method is carried out modification to oxidized regenerated cellulose; Advantage of the present invention is to inhale at oxidized regenerated cellulose material surface physicsAttached nano Au particle, and then the anthemorrhagic performance of raising material, the while can not be damaged again the mechanical strength of oxidized regenerated cellulose,And can also ensure the Bioabsorbable of oxidized regenerated cellulose;
Two, the nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material that uses the present invention to prepare stops blooding, hemostasisTime has reduced by 4.6%～12%.
The present invention can obtain a kind of nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material and preparation method thereof.
Detailed description of the invention
Detailed description of the invention one: present embodiment be a kind of nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material byNm of gold and surface grafting have the oxidized regenerated cellulose of lysine to prepare; Described nm of gold and surface grafting have lysineThe mass ratio of oxidized regenerated cellulose be (0.01～0.5): 100.
The advantage of present embodiment:
One, present embodiment is intended to maintain on the basis of oxidized regenerated cellulose absorbable hemostatic material advantage, proposes one moreAdd suitable method oxidized regenerated cellulose is carried out to modification; The advantage of present embodiment is at oxidized regenerated cellulose material listFace physical absorption nano Au particle, and then the anthemorrhagic performance of raising material, the while can not be damaged again the machine of oxidized regenerated celluloseTool intensity, and can also ensure the Bioabsorbable of oxidized regenerated cellulose;
Two, the nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material that uses present embodiment to prepare stops blooding,Bleeding stopping period has reduced by 4.6%～12%.
Present embodiment can obtain a kind of nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material and preparation method thereof.
Detailed description of the invention two: the difference of present embodiment and detailed description of the invention one is: surface grafting has the oxygen of lysineThe preparation method of change regenerated cellulose specifically completes according to the following steps:
It is 1.0 × 10 that oxidized regenerated cellulose is immersed in to concentration-4g/mL～9.0×10-4In the lysine solution of g/mL, thenUse oscillator oscillation treatment 1h～48h, obtain the oxidized regenerated cellulose after lysine solution dipping; By lysine waterOxidized regenerated cellulose after solution impregnation is immersed in 4h～24h in absolute ethyl alcohol, re-uses absolute ethyl alcohol and washs 5 times～8 times, then be vacuum drying 24h～72h at-70～-20 DEG C in temperature, obtaining surface grafting has the oxidation regeneration fibre of lysineDimension element;
In described oxidized regenerated cellulose, carboxyl-content is 16%～24%;
The quality of described oxidized regenerated cellulose and concentration are 1.0 × 10-4g/mL～9.0×10-4The lysine solution of g/mLVolume ratio be (0.0002g～0.02g): 1mL. Other are identical with detailed description of the invention one.
Detailed description of the invention three: the difference of present embodiment and detailed description of the invention one or two is: described oxidation regeneration fibreDimension element is to exist with the form of short silk, long filament or fabric. Other are identical with detailed description of the invention one or two.
Detailed description of the invention four: the difference of present embodiment and detailed description of the invention one to three is: the particle diameter of nm of gold is5nm～40nm. Other are identical with detailed description of the invention one to three.
Detailed description of the invention five: present embodiment is a kind of nm of gold/lysine/oxidized regenerated cellulose compound hemostatic materialPreparation method specifically completes according to the following steps:
One, oxidized regenerated cellulose chemical graft lysine: it is 1.0 × 10 that oxidized regenerated cellulose is immersed in to concentration-4g/mL～9.0×10-4In the lysine solution of g/mL, re-use oscillator oscillation treatment 1h～48h, obtain lysine water-solubleOxidized regenerated cellulose after immersion stain; Oxidized regenerated cellulose after lysine solution dipping is immersed in absolute ethyl alcohol4h～24h, re-uses absolute ethyl alcohol and washs 5 times～8 times, then is vacuum drying 24h～72h at-70～-20 DEG C in temperature,Obtaining surface grafting has the oxidized regenerated cellulose of lysine;
In oxidized regenerated cellulose described in step 1, carboxyl-content is 16%～24%;
The quality of the oxidized regenerated cellulose described in step 1 and concentration are 1.0 × 10-4g/mL～9.0×10-4The bad ammonia of g/mLThe volume ratio of aqueous acid is (0.0002g～0.02g): 1mL;
Two, preparation nm of gold aqueous dispersions: nm of gold is added to the water, then is that 60W～400W is ultrasonic at ultrasonic powerProcess 10min～45min, obtain nm of gold aqueous dispersions;
The quality of the nm of gold described in step 2 and the volume ratio of water are (0.01mg～0.2mg): 1mL;
Three, the self assembly of nm of gold: have the oxidized regenerated cellulose of lysine to join nm of gold aqueous dispersions surface graftingIn, be then ultrasonic processing 10min～60min under 200W～400W at ultrasonic power, re-use oscillator oscillation treatment1h～48h, obtains the oxidized regenerated cellulose of decorated by nano-gold; The oxidized regenerated cellulose of decorated by nano-gold is immersed in to nothingIn water-ethanol, 12h～36h, re-uses absolute ethyl alcohol and washs 5 times～8 times, then be immersed in absolute ethyl alcohol, ultrasonicPower is the ultrasonic processing of 160W～360W 20min～50min, re-uses absolute ethanol washing 3 times～5 times, finally in temperatureDegree, for vacuum drying 16h～48h at-70 DEG C～-20 DEG C, obtains nm of gold/lysine/oxidized regenerated cellulose compound hemostatic materialMaterial;
Surface grafting described in step 3 has the quality of oxidized regenerated cellulose and the body of nm of gold aqueous dispersions of lysineLong-pending than being (0.001g～0.1g): 1mL;
Nm of gold and surface grafting in nm of gold/lysine described in step 3/oxidized regenerated cellulose compound hemostatic materialThe mass ratio that has the oxidized regenerated cellulose of lysine is (0.01～0.5): 100.
The advantage of present embodiment:
One, present embodiment is intended to maintain on the basis of oxidized regenerated cellulose absorbable hemostatic material advantage, proposes one moreAdd suitable method oxidized regenerated cellulose is carried out to modification; The advantage of present embodiment is at oxidized regenerated cellulose material listFace physical absorption nano Au particle, and then the anthemorrhagic performance of raising material, the while can not be damaged again the machine of oxidized regenerated celluloseTool intensity, and can also ensure the Bioabsorbable of oxidized regenerated cellulose;
Two, the nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material that uses present embodiment to prepare stops blooding,Bleeding stopping period has reduced by 4.6%～12%.
Present embodiment can obtain a kind of nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material and preparation method thereof.
Detailed description of the invention six: the difference of present embodiment and detailed description of the invention five is: the nm of gold described in step 2Particle diameter be 5nm～40nm. Other are identical with detailed description of the invention five.
Detailed description of the invention seven: the difference of present embodiment and detailed description of the invention five or six is: the oxygen described in step 1Changing regenerated cellulose is to exist with the form of short silk, long filament or fabric. Other are identical with detailed description of the invention five or six.
Detailed description of the invention eight: the difference of present embodiment and detailed description of the invention five to seven is: receiving described in step 3In meter Jin/lysine/oxidized regenerated cellulose compound hemostatic material, nm of gold and surface grafting have the oxidation regeneration fibre of lysineTieing up plain mass ratio is (0.01～0.4): 100. Other are identical with detailed description of the invention five to seven.
Detailed description of the invention nine: the difference of present embodiment and detailed description of the invention five to eight is: the table described in step 3The quality of oxidized regenerated cellulose and the volume ratio of nm of gold aqueous dispersions that face is grafted with lysine are(0.001g～0.05g): 1mL. Other are identical with detailed description of the invention five to eight.
Detailed description of the invention ten: the difference of present embodiment and detailed description of the invention five to ten is: receiving described in step 2The quality of meter Jin and the volume ratio of water are (0.01mg～0.1mg): 1mL. Other are identical with detailed description of the invention five to ten.
Adopt following verification experimental verification beneficial effect of the present invention:
Test one: below the preparation method of a kind of nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material specifically pressesStep completes:
One, oxidized regenerated cellulose chemical graft lysine: 2.0g oxidized regenerated cellulose is immersed in to 350mL concentration is4.85×10-4In the lysine solution of g/mL, re-use oscillator oscillation treatment 24h, obtain lysine solution dippingAfter oxidized regenerated cellulose; Oxidized regenerated cellulose after lysine solution dipping is immersed in to 12h in absolute ethyl alcohol,Re-use absolute ethyl alcohol and wash 6 times, then be vacuum drying 30h at-53 DEG C in temperature, obtain surface grafting and depend on ammoniaThe oxidized regenerated cellulose of acid;
In oxidized regenerated cellulose described in step 1, carboxyl-content is 17.36%;
Oxidized regenerated cellulose described in step 1 is to exist with the form of fabric;
Two, preparation nm of gold aqueous dispersions: nm of gold is added to the water, then is the ultrasonic processing of 320W at ultrasonic power30min, obtains nm of gold aqueous dispersions;
The particle diameter of the nm of gold described in step 2 is 25nm;
The quality of the nm of gold described in step 2 and the volume ratio of water are 0.05mg:1mL;
Three, the self assembly of nm of gold: the surface grafting that step 1 is obtained has the oxidized regenerated cellulose of lysine to joinIn 50mL nm of gold aqueous dispersions, be then ultrasonic processing 30min under 360W at ultrasonic power, re-use oscillator and shakeSwing and process 36h, obtain the oxidized regenerated cellulose of decorated by nano-gold; The oxidized regenerated cellulose of decorated by nano-gold is immersed inIn absolute ethyl alcohol, 24h, re-uses absolute ethyl alcohol and washs 5 times, then be immersed in absolute ethyl alcohol, at ultrasonic power isThe ultrasonic processing of 320W 30min, re-uses absolute ethanol washing 5 times, is finally vacuum drying 32h at-53 DEG C in temperature,Obtain nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material;
Nm of gold and surface grafting in nm of gold/lysine described in step 3/oxidized regenerated cellulose compound hemostatic materialThe mass ratio that has the oxidized regenerated cellulose of lysine is 0.07:100.
Bleeding stopping period is measured: slowly inject after amobarbital sodium solution anesthetized animal, by its central authorities by 40mg/kg dosage veinArteria auricularis region preserved skin, sterilization, cut skin along arteria auricularis direction, and blunt separation goes out arteria auricularis, vein and nerve, then usesScalpel transversely cutting artery sticks in wound surface and uses by 1 layer of test material or control sample immediately after blood is gushed outPull and push dynamometer applies the pressure of 3N, observes hemostasis situation every 10s, until finally record bleeding stopping period after hemostasis completely.Test result is as follows: using the bleeding stopping period of the filament yarn fabric of the oxidized regenerated cellulose of carboxyl-content 17.36% is 130s,The bleeding stopping period of nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material that service test one obtains is 124s.
Test two: the preparation method of a kind of nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material, specifically by withLower step completes:
One, oxidized regenerated cellulose chemical graft lysine: 2.0g oxidized regenerated cellulose is immersed in to 600mL concentration is7.5×10-4In the lysine solution of g/mL, re-use oscillator oscillation treatment 36h, obtain after lysine solution dippingOxidized regenerated cellulose; Oxidized regenerated cellulose after lysine solution dipping is immersed in to 24h in absolute ethyl alcohol, thenUse absolute ethyl alcohol to wash 5 times, then be vacuum drying 60h at-53 DEG C in temperature, obtaining surface grafting has lysineOxidized regenerated cellulose;
In oxidized regenerated cellulose described in step 1, carboxyl-content is 17.36%;
Oxidized regenerated cellulose described in step 1 is to exist with the form of fabric;
Two, preparation nm of gold aqueous dispersions: nm of gold is added to the water, then is the ultrasonic processing of 320W at ultrasonic power30min, obtains nm of gold aqueous dispersions;
The quality of the nm of gold described in step 2 and the volume ratio of water are 0.1mg:1mL;
The particle diameter of the nm of gold described in step 2 is 30nm;
Three, the self assembly of nm of gold: have the oxidized regenerated cellulose of lysine to join 300mL nm of gold surface graftingIn aqueous dispersions, be then ultrasonic processing 45min under 400W at ultrasonic power, re-use oscillator oscillation treatment 48h,Obtain the oxidized regenerated cellulose of decorated by nano-gold; The oxidized regenerated cellulose of decorated by nano-gold is immersed in absolute ethyl alcohol,36h, re-uses absolute ethyl alcohol and washs 6 times, then be immersed in absolute ethyl alcohol, is the ultrasonic place of 360W at ultrasonic powerReason 40min, re-use absolute ethanol washing 5 times, be finally vacuum drying 40h at-53 DEG C in temperature, obtain nm of gold/Lysine/oxidized regenerated cellulose compound hemostatic material;
Nm of gold and surface grafting in nm of gold/lysine described in step 3/oxidized regenerated cellulose compound hemostatic materialThe mass ratio that has the oxidized regenerated cellulose of lysine is 0.33:100.
Bleeding stopping period is measured: slowly inject after amobarbital sodium solution anesthetized animal, by its central authorities by 40mg/kg dosage veinArteria auricularis region preserved skin, sterilization, cut skin along arteria auricularis direction, and blunt separation goes out arteria auricularis, vein and nerve, then usesScalpel transversely cutting artery sticks in wound surface and uses by 1 layer of test material or control sample immediately after blood is gushed outPull and push dynamometer applies the pressure of 3N, observes hemostasis situation every 10s, until finally record bleeding stopping period after hemostasis completely.Test result is as follows: using the bleeding stopping period of the filament yarn fabric of the oxidized regenerated cellulose of carboxyl-content 17.36% is 130s,The bleeding stopping period of nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material that service test two obtains is 115s.
Claims (7)
1. nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material, is characterized in that a kind of nm of gold/lysine/ oxidized regenerated cellulose compound hemostatic material has the oxidized regenerated cellulose of lysine to prepare by nm of gold and surface grafting; InstituteIt is (0.01～0.5) that the nm of gold of stating and surface grafting have the mass ratio of the oxidized regenerated cellulose of lysine: 100;
Described surface grafting has the preparation method of the oxidized regenerated cellulose of lysine specifically to complete according to the following steps:
It is 1.0 × 10 that oxidized regenerated cellulose is immersed in to concentration-4g/mL～9.0×10-4In the lysine solution of g/mL, then makeWith oscillator oscillation treatment 1h～48h, obtain the oxidized regenerated cellulose after lysine solution dipping; By lysine solutionOxidized regenerated cellulose after dipping is immersed in 4h～24h in absolute ethyl alcohol, and re-use absolute ethyl alcohol and wash 5 times～8 times,Be vacuum drying 24h～72h at-70～-20 DEG C in temperature again, obtaining surface grafting has the oxidized regenerated cellulose of lysine;
In described oxidized regenerated cellulose, carboxyl-content is 16%～24%;
The quality of described oxidized regenerated cellulose and concentration are 1.0 × 10-4g/mL～9.0×10-4The lysine solution of g/mLVolume ratio is (0.0002g～0.02g): 1mL;
Described oxidized regenerated cellulose is to exist with the form of short silk, long filament or fabric;
The particle diameter of described nm of gold is 5nm～40nm.
2. a preparation method for nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material, is characterized in that one receivesThe preparation method of meter Jin/lysine/oxidized regenerated cellulose compound hemostatic material specifically completes according to the following steps:
One, oxidized regenerated cellulose chemical graft lysine: it is 1.0 × 10 that oxidized regenerated cellulose is immersed in to concentration-4g/mL～9.0×10-4In the lysine solution of g/mL, re-use oscillator oscillation treatment 1h～48h, obtain lysine water-solubleOxidized regenerated cellulose after immersion stain; Oxidized regenerated cellulose after lysine solution dipping is immersed in absolute ethyl alcohol4h～24h, re-uses absolute ethyl alcohol and washs 5 times～8 times, then is vacuum drying 24h～72h at-70～-20 DEG C in temperature,Obtaining surface grafting has the oxidized regenerated cellulose of lysine;
In oxidized regenerated cellulose described in step 1, carboxyl-content is 16%～24%;
The quality of the oxidized regenerated cellulose described in step 1 and concentration are 1.0 × 10-4g/mL～9.0×10-4The lysine of g/mLThe volume ratio of the aqueous solution is (0.0002g～0.02g): 1mL;
Two, preparation nm of gold aqueous dispersions: nm of gold is added to the water, then is the ultrasonic place of 60W～400W at ultrasonic powerReason 10min～45min, obtains nm of gold aqueous dispersions;
The quality of the nm of gold described in step 2 and the volume ratio of water are (0.01mg～0.2mg): 1mL;
Three, the self assembly of nm of gold: have the oxidized regenerated cellulose of lysine to join nm of gold aqueous dispersions surface graftingIn, be then ultrasonic processing 10min～60min under 200W～400W at ultrasonic power, re-use oscillator oscillation treatment1h～48h, obtains the oxidized regenerated cellulose of decorated by nano-gold; The oxidized regenerated cellulose of decorated by nano-gold is immersed in anhydrousIn ethanol, 12h～36h, re-uses absolute ethyl alcohol and washs 5 times～8 times, then be immersed in absolute ethyl alcohol, in ultrasonic meritRate is the ultrasonic processing of 160W～360W 20min～50min, re-uses absolute ethanol washing 3 times～5 times, in temperature is finallyVacuum drying 16h～48h at-70 DEG C～-20 DEG C, obtains nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material;
Surface grafting described in step 3 has the quality of oxidized regenerated cellulose and the volume of nm of gold aqueous dispersions of lysineThan being (0.001g～0.1g): 1mL;
In nm of gold/lysine described in step 3/oxidized regenerated cellulose compound hemostatic material, nm of gold and surface grafting haveThe mass ratio of the oxidized regenerated cellulose of lysine is (0.01～0.5): 100.
3. the preparation side of a kind of nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material according to claim 2Method, the particle diameter that it is characterized in that the nm of gold described in step 2 is 5nm～40nm.
4. the preparation side of a kind of nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material according to claim 2Method, is characterized in that the oxidized regenerated cellulose described in step 1 is to exist with the form of short silk, long filament or fabric.
5. the preparation side of a kind of nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material according to claim 2Method, is characterized in that nm of gold and table in the nm of gold/lysine described in step 3/oxidized regenerated cellulose compound hemostatic materialThe mass ratio that face is grafted with the oxidized regenerated cellulose of lysine is (0.01～0.4): 100.
6. the preparation side of a kind of nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material according to claim 2Method, is characterized in that the surface grafting described in step 3 has quality and the nm of gold moisture of the oxidized regenerated cellulose of lysineThe volume ratio of loose liquid is (0.001g～0.05g): 1mL.
7. the preparation side of a kind of nm of gold/lysine/oxidized regenerated cellulose compound hemostatic material according to claim 2Method, is characterized in that the quality of the nm of gold described in step 2 and the volume ratio of water are for (0.01mg～0.1mg): 1mL.
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| BR112018009306B1 (en) * | 2015-11-08 | 2021-10-13 | Ethicon, Inc. | COMPOSITION OF FIBERS AND/OR HEMOSTATIC AGGREGATE BASED ON CELLULOSE, METHOD OF MANUFACTURING, GEL, AND METHOD FOR FORMATION OF A GEL |
| CN105477675B (en) * | 2015-12-15 | 2018-09-07 | 哈尔滨工业大学 | A kind of preparation method of RGD-M13 bacteriophages/polylysine/oxidized regenerated cellulose compound hemostatic material |
| CN106178079A (en) * | 2016-07-20 | 2016-12-07 | 国家纳米科学中心 | A kind of antibacterial chitosan dressing containing nanometer gold and preparation method thereof |
| CN111643714B (en) * | 2020-04-29 | 2021-10-22 | 诺一迈尔(山东)医学科技有限公司 | Nasal cavity filling material and preparation method thereof |
| CN115475271B (en) * | 2022-08-19 | 2023-11-24 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of amino acid/rare earth nanocrystalline/nanocellulose antibacterial hemostatic dressing |
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| EP1291460A4 (en) * | 2000-05-30 | 2004-03-31 | Ajinomoto Kk | Fiber product having antibacterial and deodorant function |
| US7019191B2 (en) * | 2003-03-25 | 2006-03-28 | Ethicon, Inc. | Hemostatic wound dressings and methods of making same |
| CN100379465C (en) * | 2005-12-31 | 2008-04-09 | 张博 | Inflammation-eliminating, pain-stopping, bacteria-resisting, pain-relieving soluble hemostatic gauze and its processing method |
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