CN114350009A - Hemostatic sponge and preparation method thereof - Google Patents
Hemostatic sponge and preparation method thereof Download PDFInfo
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- CN114350009A CN114350009A CN202111275978.5A CN202111275978A CN114350009A CN 114350009 A CN114350009 A CN 114350009A CN 202111275978 A CN202111275978 A CN 202111275978A CN 114350009 A CN114350009 A CN 114350009A
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Abstract
The invention relates to the technical field of hemostatic sponges, and particularly relates to a hemostatic sponge and a preparation method thereof. The preparation method comprises the following steps: mixing chitosan, acetic acid solution and a shaping agent to obtain chitosan solution; performing first freezing on the chitosan solution to form a film, and obtaining a chitosan freezing layer; and performing second freezing film formation on the collagen solution on the surface of the chitosan freezing layer, and freeze-drying to obtain the hemostatic sponge. The hemostatic sponge prepared by the preparation method can fully exert the excellent hemostatic performance of chitosan and the excellent liquid absorption capacity of collagen. According to the record of the embodiment, the whole liquid absorption amount of the sponge can reach 10-50 times of the self weight, and the quick hemostasis within 5min can be realized.
Description
Technical Field
The invention relates to the technical field of hemostatic sponges, and particularly relates to a hemostatic sponge and a preparation method thereof.
Background
The hemostatic sponge is a hemostatic product widely applied in hospital medical treatment, and currently, the commonly used hemostatic sponge mainly comprises products such as gelatin sponge, collagen sponge and the like, which mainly promote blood concentration by means of self liquid absorption capacity so as to realize hemostasis of patients, but the hemostatic sponge has limited hemostatic capacity and is usually used as an auxiliary hemostatic product.
The chitosan has excellent hemostatic ability, can perform hemostasis by a creep endogenous hemostatic mechanism and an exogenous hemostatic mechanism, and has good hemostatic effect on heparinized blood and patients with blood coagulation disorder. Therefore, chitosan sponge is an excellent nosocomial hemostatic product. Currently, most chitosan sponges are prepared by dissolving chitosan, blending the chitosan with gelatin, sodium alginate and the like to form a uniform solution, and then processing the uniform solution into a sponge-like product through processes such as freeze drying (for example, chinese patent application nos. 201810778574.X and 202011520641.1). However, the preparation method is to blend chitosan with other materials to obtain a porous product, and it is difficult to fully exert the excellent hemostatic ability of chitosan. In addition, because the chitosan has high hemostatic speed, the chitosan playing a hemostatic role is mainly positioned in a wound contact area, and the chitosan mixed in a non-contact area is wasted. In a comprehensive way, the existing chitosan sponge preparation method is simple and extensive, and the performance advantages of different materials are difficult to be fully exerted.
Disclosure of Invention
The invention aims to provide a hemostatic sponge and a preparation method thereof, and the hemostatic sponge prepared by the preparation method can fully exert the excellent hemostatic performance of chitosan and the excellent liquid absorption capacity of collagen.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a hemostatic sponge, which comprises the following steps:
mixing chitosan, acetic acid solution and a shaping agent to obtain chitosan solution;
performing first freezing on the chitosan solution to form a film, and obtaining a chitosan freezing layer;
and performing second freezing film formation on the collagen solution on the surface of the chitosan freezing layer, and freeze-drying to obtain the hemostatic sponge.
Preferably, the volume concentration of the acetic acid solution is 0.1-5%.
Preferably, the mass concentration of chitosan in the chitosan solution is 2-7%;
the mass concentration of the plasticizer in the chitosan solution is 0.5-4%.
Preferably, the shaping agent comprises one or more of glycerin, mannitol and sorbitol.
Preferably, the concentration of the collagen in the collagen solution is 5-9 mg/mL.
Preferably, the mixing is carried out under stirring;
the stirring speed is 300-1000 r/min, and the time is 0.5-5 h.
Preferably, the temperature of the first freezing film forming and the second freezing film forming is independently-20 ℃ to-45 ℃.
Preferably, the lyophilization comprises a first sublimation and a second sublimation performed in sequence;
the temperature of the first sublimation is-10 to-25 ℃, and the time is 40 to 60 hours; the temperature of the second sublimation is 0-50 ℃, and the time is 4-8 h.
The invention also provides the hemostatic sponge prepared by the preparation method in the technical scheme, which comprises a chitosan layer and a collagen layer which are arranged in a laminated manner;
the chitosan layer and the collagen layer are both in a sponge structure.
Preferably, the content of chitosan in the chitosan layer is 30-50 mg/cm2；
The content of the collagen in the collagen layer is 20-50 mg/cm2。
The invention provides a preparation method of a hemostatic sponge, which comprises the following steps: mixing chitosan, acetic acid solution and a shaping agent to obtain chitosan solution; performing first freezing on the chitosan solution to form a film, and obtaining a chitosan freezing layer; and performing second freezing film formation on the collagen solution on the surface of the chitosan freezing layer, and freeze-drying to obtain the hemostatic sponge. According to the invention, the chitosan layer and the collagen layer are prepared in a layered manner, so that the accurate control of the sponge structure of each layer is realized, and the excellent hemostatic performance of the chitosan material and the excellent liquid absorption capacity of the collagen sponge can be fully exerted; meanwhile, the chitosan with the sponge structure is easier to shape, so that the wound at different parts can be conveniently used, and the debridement treatment of later-period wounds can be conveniently carried out. According to the record of the embodiment, the whole liquid absorption amount of the sponge can reach 10-50 times of the self weight, and the quick hemostasis within 5min can be realized.
Detailed Description
The invention provides a preparation method of a hemostatic sponge, which comprises the following steps:
mixing chitosan, acetic acid solution and a shaping agent to obtain chitosan solution;
performing first freezing on the chitosan solution to form a film, and obtaining a chitosan freezing layer;
and performing second freezing film formation on the collagen solution on the surface of the chitosan freezing layer, and freeze-drying to obtain the hemostatic sponge.
In the present invention, all the starting materials for the preparation are commercially available products known to those skilled in the art unless otherwise specified.
The invention mixes chitosan, acetic acid solution and plasticizer to obtain chitosan solution.
In the invention, the volume concentration of the acetic acid solution is preferably 0.1-5%, more preferably 1-4%, and most preferably 2-3%.
The source of the acetic acid solution is not particularly limited in the present invention, and any source known to those skilled in the art may be used. In a particular embodiment of the invention, the acetic acid solution is preferably prepared; the preparation process of the acetic acid solution is specifically that a liquid transfer gun is adopted to add glacial acetic acid into water and mix the glacial acetic acid uniformly.
In the invention, the shaping agent comprises one or more of glycerol, mannitol and sorbitol; when the plasticizer is more than two of the above specific choices, the invention does not have any special limitation on the proportion of the specific substances, and the specific substances can be mixed according to any proportion.
In the present invention, the mixing is preferably performed under stirring; the rotating speed of the stirring is preferably 300-1000 r/min, more preferably 500-800 r/min, and most preferably 600-700 r/min; the stirring time is preferably 0.5-5 h, and more preferably 2-4 h.
In the invention, the mass concentration of chitosan in the chitosan solution is preferably 2-7%, more preferably 3-6%, and most preferably 4-5%.
In the invention, the mass concentration of the plasticizer in the chitosan solution is preferably 0.5-4%, more preferably 2-4%, and most preferably 3-4%.
After the chitosan solution is obtained, the chitosan solution is subjected to first freezing film formation to obtain a chitosan freezing layer.
In the present invention, the first freezing film-forming process is preferably performed by pouring the chitosan solution into a tray, controlling the thickness of the chitosan solution, and freezing. In the invention, the thickness of the chitosan solution in the tray is preferably 0.2-1 cm, and more preferably 0.3 cm.
In the present invention, the temperature of the first freeze film-forming is preferably-20 to-45 ℃, more preferably-25 to-40 ℃, and most preferably-30 to-35 ℃; the first freezing film forming time is preferably 1-5 h, more preferably 1-3 h, and most preferably 2 h.
After the chitosan freezing layer is obtained, the collagen solution is subjected to secondary freezing film formation on the surface of the chitosan freezing layer, and then is freeze-dried to obtain the hemostatic sponge.
In the present invention, the collagen solution is preferably prepared by a method which preferably comprises mixing collagen and water to obtain a collagen solution.
In the present invention, the mixing is preferably performed under stirring; the rotating speed of the stirring is preferably 300-1000 r/min, more preferably 500-800 r/min, and most preferably 600-700 r/min; the stirring time is preferably 0.5-5 h, and more preferably 2-4 h.
In the invention, the concentration of the collagen in the collagen solution is preferably 5-9 mg/mL, and more preferably 6-8 mg/mL.
In the present invention, the second freeze film-forming process is preferably the same as the first freeze film-forming process. In the present invention, the second freezing and film-forming process is preferably performed by pouring the collagen solution into a tray in which the chitosan layer is frozen, and freezing the collagen solution while controlling the thickness of the collagen solution. In the invention, the thickness of the collagen solution in the tray is preferably 0.3-1 cm, and more preferably 0.6 cm.
In the present invention, the temperature of the second frozen film-forming is preferably-20 to-45 ℃, more preferably-25 to-40 ℃, and most preferably-30 to-35 ℃; the second freezing film forming time is preferably 0.5-5 h, more preferably 1-3 h, and most preferably 2 h.
In the present invention, the lyophilization preferably comprises a first sublimation and a second sublimation performed in sequence. In the invention, the temperature of the first sublimation is preferably-10 to-25 ℃, more preferably-15 to-20 ℃, and the time is preferably 40 to 60 hours, more preferably 45 to 55 hours; the temperature of the second sublimation is preferably 0-50 ℃, more preferably 10-40 ℃, most preferably 20-30 ℃, and the time is preferably 4-8 hours, more preferably 5-6 hours. In the present invention, the first sublimation is sublimation drying; the second sublimation is desorption drying.
The invention also provides the hemostatic sponge prepared by the preparation method of the technical scheme, which comprises a chitosan layer and a collagen layer;
the chitosan layer and the collagen layer are both in a sponge structure.
In the invention, the content of chitosan in the chitosan layer is preferably 30-50 mg/cm2More preferably 35 to 45mg/cm2(ii) a Collagen in the collagen layerThe content of (b) is preferably 20-50 mg/cm2More preferably 30 to 40mg/cm2。
In the invention, the thickness of the chitosan layer is preferably 0.2-1 cm, and more preferably 0.3 cm; the thickness of the collagen layer is preferably 0.3-1 cm, and more preferably 0.6 cm.
The hemostatic sponge and the method for preparing the same according to the present invention will be described in detail with reference to the following examples, which should not be construed as limiting the scope of the present invention.
Example 1
Measuring 3mL of glacial acetic acid by using a pipette gun, and adding the glacial acetic acid into 97mL of water to obtain an acetic acid solution with the volume percentage of 3%;
mixing 5g of chitosan, 4g of glycerol and the acetic acid solution under the condition of stirring, wherein the rotating speed of stirring is 800r/min, and the time is 1h, so as to obtain a chitosan solution;
mixing 2.5g of collagen with 500mL of water under the condition of stirring, wherein the rotating speed of stirring is 800r/min, and the time is 2 hours, so as to obtain a collagen solution;
pouring the chitosan solution into a tray, wherein the thickness of the chitosan solution in the tray is 0.5cm, and freezing at-30 ℃ for 30min to obtain a chitosan freezing layer;
and pouring the collagen solution into a tray containing a chitosan freezing layer, controlling the thickness of the collagen solution to be 0.6cm, freezing at the temperature of minus 30 ℃ for 60min to obtain a collagen freezing layer, carrying out vacuum sublimation drying at the temperature of minus 15 ℃ for 40h, and carrying out resolution drying at the temperature of 10 ℃ for 6h to obtain the hemostatic sponge.
Example 2
Measuring 3mL of glacial acetic acid by using a pipette gun, and adding the glacial acetic acid into 97mL of water to obtain an acetic acid solution with the volume percentage of 3%;
mixing 5g of chitosan, 4g of glycerol and the acetic acid solution under the condition of stirring, wherein the rotating speed of stirring is 800r/min, and the time is 1h, so as to obtain a chitosan solution;
mixing 2.5g of collagen with 500mL of water under the condition of stirring, wherein the rotating speed of stirring is 800r/min, and the time is 2 hours, so as to obtain a collagen solution;
pouring the chitosan solution into a tray, wherein the thickness of the chitosan solution in the tray is 0.5cm, and freezing at-30 ℃ for 30min to obtain a chitosan freezing layer;
and pouring the collagen solution into a tray containing a chitosan freezing layer, controlling the thickness of the collagen solution to be 0.6cm, freezing at the temperature of minus 30 ℃ for 60min to obtain a collagen freezing layer, carrying out vacuum sublimation drying at the temperature of minus 15 ℃ for 40h, and carrying out resolution drying at the temperature of 10 ℃ for 6h to obtain the hemostatic sponge.
Test example 1
The test process is as follows: accurately weighing the weight m of the hemostatic sponge by an electronic balance0Putting the sponge into a beaker filled with pure water, holding one corner of the sponge by using tweezers after the sponge is saturated in liquid absorption, taking out the sponge and hovering the sponge for 10s, and testing the weight m of the sponge after the liquid absorption1Calculate (m)1-m0)/m0The result is recorded as the amount of the hemostatic sponge absorbed liquid, and the test result is as follows: the whole liquid absorption amount of the hemostatic sponge in the embodiment 1 can reach 25 times of the self weight; the whole liquid absorption amount of the hemostatic sponge in the embodiment 2 can reach 46 times of the self weight.
Test example 2
In the pig femoral artery hemostasis experiment, the test process is to lay the pig on the back on an operating table after being anaesthetized, cut the skin along the femoral artery, expose the femoral artery, cut the femoral artery 2/3 with an operation scissors, clean redundant blood with gauze after 5s of free bleeding, cover the wound with hemostatic sponge rapidly and press for 5min, observe the hemostasis effect, and record the hemostasis time. The test results are: the hemostatic sponge of example 1 successfully stopped bleeding after 5min of compression; the hemostatic sponge described in example 2 successfully stopped bleeding after 5min of compression.
It should be noted that, for those skilled in the art, without departing from the principle of the present invention, several improvements and modifications can be made, and these improvements and modifications should also be construed as the protection scope of the present invention.
Claims (10)
1. A preparation method of a hemostatic sponge is characterized by comprising the following steps:
mixing chitosan, acetic acid solution and a shaping agent to obtain chitosan solution;
performing first freezing on the chitosan solution to form a film, and obtaining a chitosan freezing layer;
and performing second freezing film formation on the collagen solution on the surface of the chitosan freezing layer, and freeze-drying to obtain the hemostatic sponge.
2. The method according to claim 1, wherein the acetic acid solution has a volume concentration of 0.1 to 5%.
3. The preparation method according to claim 1, wherein the mass concentration of chitosan in the chitosan solution is 2-7%;
the mass concentration of the plasticizer in the chitosan solution is 0.5-4%.
4. The method according to claim 1 or 3, wherein the plasticizer comprises one or more selected from the group consisting of glycerin, mannitol, and sorbitol.
5. The method according to claim 1, wherein the concentration of collagen in the collagen solution is 5 to 9 mg/mL.
6. The method of claim 1, wherein the mixing is performed under stirring;
the stirring speed is 300-1000 r/min, and the time is 0.5-5 h.
7. The method of claim 1, wherein the first and second frozen films are independently at a temperature of-20 ℃ to-45 ℃.
8. The preparation method according to claim 1, wherein the lyophilization comprises a first sublimation and a second sublimation which are performed in sequence;
the temperature of the first sublimation is-10 to-25 ℃, and the time is 40 to 60 hours; the temperature of the second sublimation is 0-50 ℃, and the time is 4-8 h.
9. The hemostatic sponge prepared by the preparation method of any one of claims 1 to 8, which comprises a chitosan layer and a collagen layer which are arranged in a stacked manner;
the chitosan layer and the collagen layer are both in a sponge structure.
10. The hemostatic sponge according to claim 9, wherein the chitosan content in the chitosan layer is 30-50 mg/cm2；
The content of the collagen in the collagen layer is 20-50 mg/cm2。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115970044A (en) * | 2022-12-29 | 2023-04-18 | 德晟康(苏州)生物科技有限公司 | Double-layer structured chitosan hemostatic sponge and preparation method thereof |
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| CN1387922A (en) * | 2002-04-30 | 2003-01-01 | 岳武 | Quick-hemagglutination hemostasis sponge |
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