CN104383584A - Graphene/oxidized regenerated cellulose compound hemostatic material and preparation method thereof - Google Patents
Graphene/oxidized regenerated cellulose compound hemostatic material and preparation method thereof Download PDFInfo
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- CN104383584A CN104383584A CN201410675529.3A CN201410675529A CN104383584A CN 104383584 A CN104383584 A CN 104383584A CN 201410675529 A CN201410675529 A CN 201410675529A CN 104383584 A CN104383584 A CN 104383584A
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Abstract
The invention discloses a graphene/oxidized regenerated cellulose compound hemostatic material and a preparation method thereof, relates to a hemostatic material and a preparation method of the hemostatic material, and aims at solving the problems that an existing hemostatic material is high in price, and low in bleeding-stopping rate, and cannot be applied to massive haemorrhage. The graphene/oxidized regenerated cellulose compound hemostatic material is prepared from redox graphene and filament fabric of the oxidized regenerated cellulose, wherein the mass ratio of the redox graphene to the filament fabric of the oxidized regenerated cellulose is (0.05-10) to 100. The method comprises the following steps: 1 preparing a graphene solution; and 2 ultrasonically treating and freeze-drying to obtain the graphene/oxidized regenerated cellulose compound hemostatic material. The graphene/oxidized regenerated cellulose compound hemostatic material prepared by the method is used for stopping bleeding; the bleeding-stopping time is reduced by 6%-15%. By adopting the preparation method, the graphene/oxidized regenerated cellulose compound hemostatic material can be obtained.
Description
Technical field
The present invention relates to a kind of hemostatic material and preparation method thereof.
Background technology
Inevitably there is various accident in daily life, carrying out in emergency treatment and operation process, all malpractice may be caused even dead because of massive hemorrhage.Therefore, the effective quick-acting haemostatic powder in patient local is then most important, and effective Bleeding control also reduces the important measures that the bleeding time becomes reduction mortality.Clinical conventional hemostatic material such as hemostatic gauze, stanch fibre, tourniquet bandage in use have limitation, as bleeding stopping period is longer, easily and wound adhesion and not easily changing dressings, to the infection of wound with suppurate helpless.The direction that quick-acting haemostatic powder and functional hemostasis will be the development of following haemostatic medicament.
Conventional Absorbable hemostatic material has Fibrin Glue, gelfoam, oxidized cellulose, microfibrillar collagen, chitosan and Sorbsan etc.Their mechanism of action and using method are not quite similar, and haemostatic effect also has difference.But the hemostatic gauze be widely used clinically is at present SURGICEL series absorbable hemostatic product---the SURGICEL produced by Johnson & Johnson of the U.S. (Johnson & Johnson) company
tM, SURGICEL
tMnu-Knit, SURGICEL
tMfibrillar, at home also known as " speed and yarn ", the composition of above product is oxidized regenerated cellulose, main difference is embodied in external expressive form, SURGICEL series of products have occupied extremely important status in the international market now, and receive the consistent favorable comment of medical domain expert.Meanwhile, domestic You Ji company has also produced similar hemostatic gauze, but can not show a candle to speed and yarn due to material property, adopts expensive import hemostatic material so main clinically.
Oxidized regenerated cellulose is cellulosic derivant, there are good anthemorrhagic performance, biodegradable performance and nontoxic, be used to multiple industry at present, comprise in the medical field, hydroxyl oxidize on C-6 position in cellulose unit, as oxidant, is that carboxyl obtains oxidized regenerated cellulose by general employing nitrogen oxide.When it uses as hemostatic material, carboxyl-content should be 16 ~ 24%, to ensure its haemostatic effect.Oxidized regenerated cellulose hemostatic mechanism is as follows: can adsorb a large amount of erythrocytes after oxidized regenerated cellulose contact blood, the acidic carboxypolymer then in oxidized regenerated cellulose structure can cause haemolysis, namely lyse red blood cells, break, and discharge hemoglobin.Meanwhile, due in hemoglobin containing ferric ion, oxidized regenerated cellulose can with Fe
3+in conjunction with the brown blob of viscose of formation, close, block blood capillary end and stop blooding.As can be seen here, the hemostasis of oxidized regenerated cellulose is a series of Biochemical Engineering, and the carboxyl limited amount in material structure, therefore cause the anthemorrhagic speed of oxidized regenerated cellulose material relatively slow, cause such material cannot be applicable to the massive hemorrhage situation at the positions such as tremulous pulse.
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 disclose the method adopting the aqueous solution of sodium bicarbonate or calcium acetate to neutralize oxidized regenerated cellulose, and with the oxidized regenerated cellulose of thrombin dipping sodium bicarbonate neutralization, then process is freezed to the fabric after dipping and drying in this case, obtained a kind of efficient oxidized cellulose class surgical operation hemostatic material.In United States Patent (USP), the people such as Saferstein describes the alcohol-water solution using salt of weak acid, as sodium acetate, oxidized regenerated cellulose is neutralized to pH value between 5 ~ 8, this method not only makes oxidized regenerated cellulose store by ambient-temp-stable, and can the acid-sensitive material of similar thrombin in load, and then improve the anthemorrhagic performance of oxidized regenerated cellulose material.They also find simultaneously, the method that the people such as Doub adopt sodium bicarbonate to neutralize can cause the gel of oxidized regenerated cellulose fabrics part, distortion, and causes the hot strength of the oxidation regeneration fabric of final neutralization too low and cannot be applied in actual hemostasis.And although the oxidized regenerated cellulose of the calcium acetate neutralization that the people such as Doub mention in the patent ensure that original form of fabric, but it is too high owing to neutralizing rear material calcium content, in use can produce zest to the mammal skin of contact position and other somatic cells, and the large granulation lump turned white is formed in use location, hinder the bio-absorbable of material.Said method utilizes modification can improve the anthemorrhagic performance of oxidized regenerated cellulose, but its Bioabsorbable significantly reduces.
Although above achievement in research all has a very big significance the correlational study of oxidized regenerated cellulose, also make the anthemorrhagic performance of material obtain lifting to a certain degree simultaneously, promote degree general less, namely improve effect poor; And the ameliorative way in the past in research also can cause negative effect to the mechanical strength of regenerated oxycellulose as styptic material and biological absorbable performance, and for the anthemorrhagic performance promoted by a small margin, modified effect is lost more than gain.
Summary of the invention
The object of the invention is to solve existing hemostatic material exists expensive, and anthemorrhagic speed is slow, can not be used in the problem of the situation of massive hemorrhage, and provide a kind of Graphene/oxidized regenerated cellulose compound hemostatic material and preparation method thereof.
A kind of Graphene/oxidized regenerated cellulose compound hemostatic material is prepared by the filament yarn fabric of oxidoreduction Graphene and oxidized regenerated cellulose; The mass ratio of described oxidoreduction Graphene and the filament yarn fabric of oxidized regenerated cellulose is (0.05 ~ 10): 100.
The preparation method of a kind of Graphene/oxidized regenerated cellulose compound hemostatic material specifically completes according to the following steps:
One, prepare graphene solution: join in solvent by oxidoreduction Graphene, be then supersound process 10min ~ 60min under the condition of 160W ~ 400W at ultrasonic power, obtain graphene solution;
The quality of the oxidoreduction Graphene described in step one and the volume ratio of solvent are (0.1mg ~ 2mg): 1mL;
Two, ultrasonic, lyophilization: the filament yarn fabric of oxidized regenerated cellulose is immersed in graphene solution, be supersound process 10min ~ 60min under the condition of 200W ~ 400W at ultrasonic power, and then use oscillator vibrates process 1h ~ 24h, again the filament yarn fabric of oxidized regenerated cellulose is taken out from the solution of Graphene, obtain the filament yarn fabric of the oxidized regenerated cellulose after flooding; By filament yarn fabric vacuum lyophilization 8h ~ 96h at temperature is-70 ~-20 DEG C of the oxidized regenerated cellulose after dipping, obtain Graphene/oxidized regenerated cellulose compound hemostatic material;
The quality of the filament yarn fabric of the oxidized regenerated cellulose described in step 2 and the volume ratio of graphene solution are (0.005g ~ 0.04g): 1mL;
In Graphene described in step 2/oxidized regenerated cellulose compound hemostatic material, the mass ratio of the filament yarn fabric of oxidoreduction Graphene and oxidized regenerated cellulose is (0.05 ~ 10): 100.
Advantage of the present invention:
One, Graphene/oxidized regenerated cellulose compound hemostatic material that prepared by the present invention directly adsorbs nano-graphene on the surface of the filament yarn fabric of oxidized regenerated cellulose, both improve the anthemorrhagic performance of material, simultaneously again can not the mechanical strength of attacking material and biological absorbable performance;
Two, the Graphene/oxidized regenerated cellulose compound hemostatic material using the present invention to prepare stops blooding, and bleeding stopping period reduces 6% ~ 15%.
The present invention can obtain a kind of Graphene/oxidized regenerated cellulose compound hemostatic material.
Detailed description of the invention
Detailed description of the invention one: present embodiment is a kind of Graphene/oxidized regenerated cellulose compound hemostatic material is prepared by the filament yarn fabric of oxidoreduction Graphene and oxidized regenerated cellulose; The mass ratio of described oxidoreduction Graphene and the filament yarn fabric of oxidized regenerated cellulose is (0.05 ~ 10): 100.
The advantage of present embodiment:
One, Graphene/oxidized regenerated cellulose compound hemostatic material that prepared by present embodiment directly adsorbs nano-graphene on the surface of the filament yarn fabric of oxidized regenerated cellulose, both improve the anthemorrhagic performance of material, simultaneously again can not the mechanical strength of attacking material and biological absorbable performance;
Two, the Graphene/oxidized regenerated cellulose compound hemostatic material using present embodiment to prepare stops blooding, and bleeding stopping period reduces 6% ~ 15%.
Present embodiment can obtain a kind of Graphene/oxidized regenerated cellulose compound hemostatic material.
Detailed description of the invention two: the difference of present embodiment and detailed description of the invention one is: in the filament yarn fabric of oxidized regenerated cellulose, carboxyl-content is 16% ~ 24%.Other are identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment is that the preparation method of a kind of Graphene/oxidized regenerated cellulose compound hemostatic material specifically completes according to the following steps:
One, prepare graphene solution: join in solvent by oxidoreduction Graphene, be then supersound process 10min ~ 60min under the condition of 160W ~ 400W at ultrasonic power, obtain graphene solution;
The quality of the oxidoreduction Graphene described in step one and the volume ratio of solvent are (0.1mg ~ 2mg): 1mL;
Two, ultrasonic, lyophilization: the filament yarn fabric of oxidized regenerated cellulose is immersed in graphene solution, be supersound process 10min ~ 60min under the condition of 200W ~ 400W at ultrasonic power, and then use oscillator vibrates process 1h ~ 24h, again the filament yarn fabric of oxidized regenerated cellulose is taken out from the solution of Graphene, obtain the filament yarn fabric of the oxidized regenerated cellulose after flooding; By filament yarn fabric vacuum lyophilization 8h ~ 96h at temperature is-70 ~-20 DEG C of the oxidized regenerated cellulose after dipping, obtain Graphene/oxidized regenerated cellulose compound hemostatic material;
The quality of the filament yarn fabric of the oxidized regenerated cellulose described in step 2 and the volume ratio of graphene solution are (0.005g ~ 0.04g): 1mL;
In Graphene described in step 2/oxidized regenerated cellulose compound hemostatic material, the mass ratio of the filament yarn fabric of oxidoreduction Graphene and oxidized regenerated cellulose is (0.05 ~ 10): 100.
Oxidoreduction Graphene described in step one carries out oxidation processes with Hummers method to Graphene, then obtains oxidation product through washing, drying; And then utilize hydrazine hydrate to carry out reduction treatment to oxidation product, the oxidoreduction Graphene obtained after washing, drying.
The advantage of present embodiment:
One, Graphene/oxidized regenerated cellulose compound hemostatic material that prepared by present embodiment directly adsorbs nano-graphene on the surface of the filament yarn fabric of oxidized regenerated cellulose, both improve the anthemorrhagic performance of material, simultaneously again can not the mechanical strength of attacking material and biological absorbable performance;
Two, the Graphene/oxidized regenerated cellulose compound hemostatic material using present embodiment to prepare stops blooding, and bleeding stopping period reduces 6% ~ 15%.
Present embodiment can obtain a kind of Graphene/oxidized regenerated cellulose compound hemostatic material.
Detailed description of the invention four: the difference of present embodiment and detailed description of the invention three is: the solvent described in step one to be water, dehydrated alcohol or mass fraction be 20% ~ 80% alcoholic solution.Other are identical with detailed description of the invention three.
Detailed description of the invention five: the difference of present embodiment and detailed description of the invention three or four is: join in solvent by oxidoreduction Graphene in step one, then be supersound process 10min ~ 30min under the condition of 160W ~ 400W at ultrasonic power, obtain graphene solution.Other are identical with detailed description of the invention three or four.
Detailed description of the invention six: the difference of present embodiment and detailed description of the invention three to five is: in step one, oxidoreduction Graphene is joined in solvent, then be supersound process 30min ~ 60min under the condition of 200W ~ 400W at ultrasonic power, obtain graphene solution.Other are identical with detailed description of the invention three to five.
Detailed description of the invention seven: the difference of present embodiment and detailed description of the invention three to six is: the quality of the oxidoreduction Graphene described in step one and the volume ratio of solvent are (0.1mg ~ 1mg): 1mL.Other are identical with detailed description of the invention three to six.
Detailed description of the invention eight: the difference of present embodiment and detailed description of the invention three to seven is: the quality of the filament yarn fabric of the oxidized regenerated cellulose described in step 2 and the volume ratio of graphene solution are (0.005g ~ 0.02g): 1mL.Other are identical with detailed description of the invention three to seven.
Detailed description of the invention nine: the difference of present embodiment and detailed description of the invention three to eight is: in the Graphene described in step 2/oxidized regenerated cellulose compound hemostatic material, the mass ratio of the filament yarn fabric of oxidoreduction Graphene and oxidized regenerated cellulose is (0.05 ~ 2): 100.Other are identical with detailed description of the invention three to eight.
Detailed description of the invention ten: the difference of present embodiment and detailed description of the invention three to nine is: in the filament yarn fabric of the oxidized regenerated cellulose described in step 2, carboxyl-content is 16% ~ 24%.Other are identical with detailed description of the invention three to nine.
Adopt following verification experimental verification beneficial effect of the present invention:
Test one: the preparation method of a kind of Graphene/oxidized regenerated cellulose compound hemostatic material specifically completes according to the following steps:
One, prepare graphene solution: join in 150mL water by 20mg oxidoreduction Graphene, be then supersound process 30min under the condition of 320W at ultrasonic power, obtain graphene solution;
Two, ultrasonic, lyophilization: the filament yarn fabric of 2.5g oxidized regenerated cellulose is immersed in the graphene solution obtained in step one, be supersound process 15min under the condition of 400W at ultrasonic power, and then use oscillator vibrates process 4h, again the filament yarn fabric of oxidized regenerated cellulose is taken out from the solution of Graphene, obtain the filament yarn fabric of the oxidized regenerated cellulose after flooding; By filament yarn fabric vacuum lyophilization 72h at temperature is-50 DEG C of the oxidized regenerated cellulose after dipping, obtain Graphene/oxidized regenerated cellulose compound hemostatic material;
In the filament yarn fabric of the oxidized regenerated cellulose described in step 2, carboxyl-content is 17.36%;
In Graphene described in step 2/oxidized regenerated cellulose compound hemostatic material, the mass ratio of the filament yarn fabric of oxidoreduction Graphene and oxidized regenerated cellulose is 0.28:100.
Bleeding stopping period measures: after slowly injecting Nembutal sodium solution anesthetized animal by 40mg/kg dose intravenous, by its central arteria auricularis region preserved skin, sterilization, skin is cut along arteria auricularis direction, blunt separation goes out arteria auricularis, vein and nerve, use scalpel transversely cutting tremulous pulse again, stick in wound surface with 1 layer of test material or control sample immediately after blood is gushed out and use pull and push dynamometer to apply the pressure of 3N, observing hemostasis every 10s, until record bleeding stopping period after final hemostasis completely.Test result is as follows: the bleeding stopping period using the filament yarn fabric of the oxidized regenerated cellulose of carboxyl-content 17.36% is 130s, the bleeding stopping period of the Graphene that service test one obtains/oxidized regenerated cellulose compound hemostatic material is 122s, and bleeding stopping period reduces 6.2%.
Test two: the preparation method of a kind of Graphene/oxidized regenerated cellulose compound hemostatic material specifically completes according to the following steps:
One, prepare graphene solution: join in 150mL dehydrated alcohol by 100mg oxidoreduction Graphene, be then supersound process 45min under the condition of 400W at ultrasonic power, obtain graphene solution;
Two, ultrasonic, lyophilization: the filament yarn fabric of 2.5g oxidized regenerated cellulose is immersed in the graphene solution obtained in step one, be supersound process 30min under the condition of 400W at ultrasonic power, and then use oscillator vibrates process 24h, again the filament yarn fabric of oxidized regenerated cellulose is taken out from the solution of Graphene, obtain the filament yarn fabric of the oxidized regenerated cellulose after flooding; By filament yarn fabric vacuum lyophilization 24h at temperature is-50 DEG C of the oxidized regenerated cellulose after dipping, obtain Graphene/oxidized regenerated cellulose compound hemostatic material;
In the filament yarn fabric of the oxidized regenerated cellulose described in step 2, carboxyl-content is 17.36%;
In Graphene described in step 2/oxidized regenerated cellulose compound hemostatic material, the mass ratio of the filament yarn fabric of oxidoreduction Graphene and oxidized regenerated cellulose is 1.36:100.
Bleeding stopping period measures: after slowly injecting Nembutal sodium solution anesthetized animal by 40mg/kg dose intravenous, by its central arteria auricularis region preserved skin, sterilization, skin is cut along arteria auricularis direction, blunt separation goes out arteria auricularis, vein and nerve, use scalpel transversely cutting tremulous pulse again, stick in wound surface with 1 layer of test material or control sample immediately after blood is gushed out and use pull and push dynamometer to apply the pressure of 3N, observing hemostasis every 10s, until record bleeding stopping period after final hemostasis completely.Test result is as follows: carboxyl-content is the bleeding stopping period of the filament yarn fabric of 17.36% oxidized regenerated cellulose is 130s, and the bleeding stopping period of the Graphene that service test two obtains/oxidized regenerated cellulose compound hemostatic material is 117s, and bleeding stopping period reduces 10%.
Claims (10)
1. Graphene/oxidized regenerated cellulose compound hemostatic material, is characterized in that a kind of Graphene/oxidized regenerated cellulose compound hemostatic material is prepared by the filament yarn fabric of oxidoreduction Graphene and oxidized regenerated cellulose; The mass ratio of described oxidoreduction Graphene and the filament yarn fabric of oxidized regenerated cellulose is (0.05 ~ 10): 100.
2. a kind of Graphene/oxidized regenerated cellulose compound hemostatic material according to claim 1, is characterized in that in the filament yarn fabric of oxidized regenerated cellulose, carboxyl-content is 16% ~ 24%.
3. a preparation method for Graphene/oxidized regenerated cellulose compound hemostatic material, is characterized in that what the preparation method of a kind of Graphene/oxidized regenerated cellulose compound hemostatic material specifically completed according to the following steps:
One, prepare graphene solution: join in solvent by oxidoreduction Graphene, be then supersound process 10min ~ 60min under the condition of 160W ~ 400W at ultrasonic power, obtain graphene solution;
The quality of the oxidoreduction Graphene described in step one and the volume ratio of solvent are (0.1mg ~ 2mg): 1mL;
Two, ultrasonic, lyophilization: the filament yarn fabric of oxidized regenerated cellulose is immersed in graphene solution, be supersound process 10min ~ 60min under the condition of 200W ~ 400W at ultrasonic power, and then use oscillator vibrates process 1h ~ 24h, again the filament yarn fabric of oxidized regenerated cellulose is taken out from the solution of Graphene, obtain the filament yarn fabric of the oxidized regenerated cellulose after flooding; By filament yarn fabric vacuum lyophilization 8h ~ 96h at temperature is-70 ~-20 DEG C of the oxidized regenerated cellulose after dipping, obtain Graphene/oxidized regenerated cellulose compound hemostatic material;
The quality of the filament yarn fabric of the oxidized regenerated cellulose described in step 2 and the volume ratio of graphene solution are (0.005g ~ 0.04g): 1mL;
In Graphene described in step 2/oxidized regenerated cellulose compound hemostatic material, the mass ratio of the filament yarn fabric of oxidoreduction Graphene and oxidized regenerated cellulose is (0.05 ~ 10): 100.
4. the preparation method of a kind of Graphene/oxidized regenerated cellulose compound hemostatic material according to claim 3, is characterized in that the solvent described in step one to be water, dehydrated alcohol or mass fraction is the alcoholic solution of 20% ~ 80%.
5. the preparation method of a kind of Graphene/oxidized regenerated cellulose compound hemostatic material according to claim 3, it is characterized in that in step one, oxidoreduction Graphene being joined in solvent, then be supersound process 10min ~ 30min under the condition of 160W ~ 400W at ultrasonic power, obtain graphene solution.
6. the preparation method of a kind of Graphene/oxidized regenerated cellulose compound hemostatic material according to claim 3, it is characterized in that in step one, oxidoreduction Graphene being joined in solvent, then be supersound process 30min ~ 60min under the condition of 200W ~ 400W at ultrasonic power, obtain graphene solution.
7. the preparation method of a kind of Graphene/oxidized regenerated cellulose compound hemostatic material according to claim 3, is characterized in that the quality of the oxidoreduction Graphene described in step one and the volume ratio of solvent are (0.1mg ~ 1mg): 1mL.
8. the preparation method of a kind of Graphene/oxidized regenerated cellulose compound hemostatic material according to claim 3, is characterized in that the quality of the filament yarn fabric of the oxidized regenerated cellulose described in step 2 and the volume ratio of graphene solution are (0.005g ~ 0.02g): 1mL.
9. the preparation method of a kind of Graphene/oxidized regenerated cellulose compound hemostatic material according to claim 3, is characterized in that the mass ratio of the filament yarn fabric of oxidoreduction Graphene and oxidized regenerated cellulose in the Graphene described in step 2/oxidized regenerated cellulose compound hemostatic material is for (0.05 ~ 2): 100.
10. the preparation method of a kind of Graphene/oxidized regenerated cellulose compound hemostatic material according to claim 3, is characterized in that in the filament yarn fabric of the oxidized regenerated cellulose described in step 2, carboxyl-content is 16% ~ 24%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106806049A (en) * | 2015-12-02 | 2017-06-09 | 珠海和凡医药股份有限公司 | A kind of medical application of novel graphite alkene material |
| CN108568034A (en) * | 2018-03-14 | 2018-09-25 | 广西中医药大学 | A kind of graphene strengthens medicine infrared treatment head-shield and its preparation, purposes and application process |
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| CN103418019A (en) * | 2013-08-13 | 2013-12-04 | 威海洁瑞医用制品有限公司 | Zwitterionic modified oxidized regenerated cellulose absorbable hemostatic material and preparation method thereof |
| CN104072809A (en) * | 2014-06-20 | 2014-10-01 | 南京林业大学 | Preparation method of graphene oxide/bacterial cellulose antibacterial compound material |
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| US2517772A (en) * | 1945-05-11 | 1950-08-08 | Parke Davis & Co | Neutralized oxidized cellulose products |
| CN103418019A (en) * | 2013-08-13 | 2013-12-04 | 威海洁瑞医用制品有限公司 | Zwitterionic modified oxidized regenerated cellulose absorbable hemostatic material and preparation method thereof |
| CN104072809A (en) * | 2014-06-20 | 2014-10-01 | 南京林业大学 | Preparation method of graphene oxide/bacterial cellulose antibacterial compound material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106806049A (en) * | 2015-12-02 | 2017-06-09 | 珠海和凡医药股份有限公司 | A kind of medical application of novel graphite alkene material |
| CN106806049B (en) * | 2015-12-02 | 2018-10-16 | 珠海和凡医药股份有限公司 | A kind of preparation method and medical application of novel graphite alkene material |
| CN108568034A (en) * | 2018-03-14 | 2018-09-25 | 广西中医药大学 | A kind of graphene strengthens medicine infrared treatment head-shield and its preparation, purposes and application process |
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