CN110420348A - A kind of fibroin albumen hemostatic material and preparation method thereof - Google Patents
A kind of fibroin albumen hemostatic material and preparation method thereof Download PDFInfo
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- CN110420348A CN110420348A CN201910654456.2A CN201910654456A CN110420348A CN 110420348 A CN110420348 A CN 110420348A CN 201910654456 A CN201910654456 A CN 201910654456A CN 110420348 A CN110420348 A CN 110420348A
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- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
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Abstract
The invention discloses a kind of fibroin albumen hemostatic material and preparation method thereof, preparation method includes the following steps: that photosensitizer riboflavin is added into silk fibroin water solution, is uniformly mixed and obtains mixed liquor；It is continually fed into oxygen into the mixed liquor, keeps oxygen partial pressure in the mixed liquor in a saturated state；The oxygen-saturated mixed liquor is poured into transparent mould and cooled down；The mixed liquor described in ultraviolet light, the silk fibroin hydrogel being crosslinked, control ultraviolet light during the mixed liquor temperature be 0~8 DEG C；The silk fibroin hydrogel is removed from the molds and is dried, fibroin albumen xerogel is obtained；The fibroin albumen dry gel powder is broken into powder, obtains fibroin albumen hemostatic material.Preparation method of the invention can effectively reduce reaction temperature by being crosslinked at low ambient temperatures, the generation of effective limiting crystal structure, the performance for greatly promoting the Swelling Capacity of material and quickly sucking blood.
Description
Technical field
The present invention relates to biomaterials and bio-medical technology field, and in particular to a kind of system of fibroin albumen hemostatic material
Preparation Method and the fibroin albumen hemostatic material being prepared using the preparation method.
Background technique
Developing efficient, quick, safe, economic hemostatic material is clinical operation, key difficulties urgently to be solved in first aid.
Existing hemostatic material in medical use mainly have chitosan, fiber collagen, Fibrin Glue, oxycellulose, calcium alginate fibre element,
Gelfoam etc..But these hemostatic materials all exist that biocompatibility is high, complicated, the expensive, anthemorrhagic speed of synthesis not
Fastly, Yi Yinfa infected with the disadvantages of.Develop a kind of material with good biocompatibility, cheap, anthemorrhagic performance is excellent
With very big social benefit.
Fibroin albumen is a natural fiber material, has necessary several amino acid in human body, nontoxic to body, stingless
Swash effect, it is biodegradable；Furthermore fibroin albumen can also be processed into the material of various forms as needed, pass through different changes
Agent modifier is learned, there is very big plasticity, be widely used in textile industry, biomedicine field.Existing fibroin albumen stops
Blood material mostly uses collagen and chitosan to be developed, and in quick-acting haemostatic powder aspect of performance existing defects, therefore in reality
It is not widely used in the life of border, research fibroin albumen rapid hemostatic material has realistic meaning.
At present in the field, 2016, the CaCl that Wang Xin et al. is 10%, 20%, 40% with concentration2Solution to fibroin into
Row slightly soluble processing, then fibroin -80 DEG C of freezing 2h, 4h, 6h, 12, for 24 hours, after 48h drying or freeze-drying.It is mentioned by modification
The water imbibition of high fibroin, while clot-promoting factor is added to improve the anthemorrhagic performance of fibroin, while to the biofacies of resulting materials
Capacitive, degeneration can be carried out research, and research finds its anthemorrhagic performance of fibroin hemostatic yarn obtained better than hospital gauze.But its
Degeneration is poor, quick-acting haemostatic powder performance existing defects.Such as number of patent application CN201710088690.4, entitled " fibroin egg
It is disclosed in the patent of invention of white hemostatic material and preparation method thereof " by silk fibroin protein solution and polyglycol solution with volume ratio
10:0.25-10:3 ratio be mutually mixed, obtained by freeze drying fibroin albumen hemostatic material；The fibroin albumen hemostatic material,
Good water absorption is tightly combined with wound and is not easy to fall, but holds in mixing with polyglycol solution fibroin albumen in preparation process
Easily that the complete induced synthesis of fibroin albumen is stable beta sheet structure does not have tissue adhension characteristic, influences haemostatic effect.
Summary of the invention
In view of this, in order to overcome the drawbacks of the prior art, the object of the present invention is to provide a kind of fibroin albumen hemostatic materials
The preparation method of material, and the fibroin albumen hemostatic material being prepared using the preparation method.
In order to achieve the above objectives, the following technical solution is employed by the present invention:
A kind of preparation method of fibroin albumen hemostatic material, comprising the following steps:
(1) photosensitizer riboflavin is added into silk fibroin water solution, is uniformly mixed and obtains mixed liquor；
(2) it is continually fed into oxygen in Xiang Suoshu mixed liquor, keeps oxygen partial pressure in the mixed liquor in a saturated state；
(3) the oxygen-saturated mixed liquor is poured into transparent mould and is cooled down；
(4) mixed liquor described in ultraviolet light, the silk fibroin hydrogel being crosslinked control ultraviolet light process
Described in mixed liquor temperature be 0~8 DEG C, can be realized by the way that mixed liquor to be placed under condition of ice bath；
(5) silk fibroin hydrogel is removed from the molds and is dried, obtain fibroin albumen xerogel；
(6) the fibroin albumen dry gel powder is broken into powder, obtains fibroin albumen hemostatic material.
Some preferred aspects according to the present invention, the concentration of silk fibroin water solution described in step (1) be 15g/L~
30g/L；The concentration of riboflavin is 0.1mmol/L~0.5mmol/L in the mixed liquor.Riboflavin participate in vivo biodistribution oxidation with
Energetic supersession, it is related with the metabolism of carbohydrate, protein, nucleic acid and fat, human body can be improved to the utilization rate of protein,
Enhancing development safeguards the integrality of skin and cell membrane, has the function of protecting skin follicle mucous membrane and sebaceous glands.It is added
Riboflavin it is more, on the one hand can reduce the time of illumination, on the other hand, remaining riboflavin can be improved after material sucks blood
Organization healing ability.
Some preferred aspects according to the present invention, the depth of the mixed liquor in transparent mould described in step (3) are 10mm
~30mm.The depth for reducing mixed liquor can make crosslinking points be more evenly distributed, the generation of limiting crystal structure.
Some preferred aspects according to the present invention, the parameter of ultraviolet light in step (4) are as follows: the distance of ultraviolet light
For 10cm~20cm；The time of ultraviolet light is 5min~30min.
Some preferred aspects according to the present invention, the parameter of ultraviolet light described in step (4) are as follows: in step (4)
The ultraviolet light that ultraviolet light is power 50W~500W, the ultraviolet lamp of 350~400nm of wavelength issues.
Some preferred aspects according to the present invention, dry environment is 20~30 DEG C of temperature, relative humidity 10 in step (5)
~50% constant-temperature constant-humidity environment.
Some preferred aspects according to the present invention, the partial size of powder described in step (6) are 0.1~1mm.By fibroin albumen
The lesser powder of partial size, which is made, after crushing in xerogel can increase material specific surface area, promote material and quickly suck blood ability.
The present invention also provides a kind of fibroin albumen hemostatic materials being prepared using preparation method as described above, should
The multiplying power of sucking blood of the fibroin albumen hemostatic material is 7.5~11.5, and the clotting time is 55~80s.Multiplying power of sucking blood is unit matter
The fibroin material of amount (1 gram) is sucked blood the ratio between increased quality and former dry mass after saturation；Clotting time refer to blood from
Blood vessel is opened, the time solidified in vitro.
The principle of the present invention is: under the irradiation of ultraviolet light, the transfer that energy occurs generates based on singlet oxygen riboflavin
Active oxygen radical, active oxygen radical can react with various molecules, induce the tyrosine in fibroin albumen macromolecular
Residue groups generate chemical crosslinking, so that gelation, the dry shearing of hydrogel is pulverized into powder, hemostatic material is obtained.This
Riboflavin solution is added into silk fibroin protein solution in the low temperature environment of ice bath for invention, and is passed through oxygen in advance and makes mixed liquor
Oxygen saturation reduces the depth of mixed liquor using the light sensitivity of riboflavin, and making it, Quick cross-linking solidifies under ultraviolet light, prepares
Journey is simple and convenient, and the time is short, high-efficient, can sufficiently keep the biocompatibility of fibroin itself.Due to the depth as shallow of mixed liquor, system
The standby powder formed, large specific surface area not only have and are quickly combined the performance being swollen again with water, same to have the property quickly sucked blood
Energy.There is biggish porosity inside powdered gel, ensure that the height of the hemostatic material is sucked blood multiplying power and speed of sucking blood.It is made
Fibroin albumen hemostatic material can reach physics and block blood vessel and hemostasis purpose, anthemorrhagic performance is excellent.Contain fibroin albumen and core
The mixed liquor of flavine can also absorb a large amount of thermal energy of ultraviolet light releasing while photocuring, and the temperature of mixed liquor is excessively high to be promoted
Molecular conformation changes, and generates part beta sheet structure, by improving irradiation distance, and is crosslinked under the low temperature environment of ice bath
It can effectively reduce reaction temperature, the gel to be formed made to keep the random coil structure in mixed liquor, thus effectively limiting crystal knot
The generation of structure greatly promotes the Swelling Capacity of material.The depth for reducing mixed liquor can make crosslinking points be more evenly distributed, limiting crystal
The generation of structure.
Due to the technical solution more than using, the present invention has following usefulness: this hair compared with prior art
Bright preparation method can effectively reduce reaction temperature by being crosslinked at low ambient temperatures, keep the gel to be formed in mixed liquor
Random coil structure greatly promotes the Swelling Capacity of material and quickly sucks blood thus the generation of effectively limiting crystal structure
Performance；In preparation process, riboflavin only joined, therefore the fibroin albumen hemostatic material has good biocompatibility and can
Degradability；Fibroin albumen hemostatic material is powdered, large specific surface area, not only has and is quickly combined the performance being swollen again with water,
It is same that there is the performance quickly sucked blood；Fibroin material be it is powdered, there is biggish porosity inside powdered gel, protect
The height for having demonstrate,proved the hemostatic material is sucked blood multiplying power and speed of sucking blood fastly.
Detailed description of the invention
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings other
Attached drawing.
Fig. 1 is the blood coagulation photo one of the fibroin albumen hemostatic material prepared in the preferred embodiment of the present invention 2；
Fig. 2 is the blood coagulation photo two of the fibroin albumen hemostatic material prepared in the preferred embodiment of the present invention 2.
Specific embodiment
In order that those skilled in the art will better understand the technical solution of the present invention, implement below in conjunction with the present invention
Attached drawing in example, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment
Only a part of the embodiments of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work, all should belong to protection of the present invention
Range.
The preparation of 1 silk fibroin protein solution of embodiment
In the 4L deionized water boiled, weighed 3g anhydrous Na HCO is added3With 1g anhydrous Na2CO3, after completely dissolution
80g silk cocoon is added, adjust solution state be it is slightly boiled, stirred every 10min with glass bar primary, be washed with deionized water after 30min
It washs completely, repeats aforesaid operations 3 times；After sufficiently cleaning, silk is ripped and is paved, is put into 60 DEG C of baking ovens and dries.Take 100mL
The lithium-bromide solution of 9.3mol/L pour into conical flask, 65 DEG C are heated in constant temperature blender with magnetic force, by the degumed silk of 15g
Element is added several times, and 30~40min is dissolved at 65 ± 2 DEG C, and sealing is fitted into bag filter after being fully cooled and is dialysed, under low temperature
Dialyse 3~4d in deionized water, after the completion of dialysis, is packed into reagent bottle after obtained silk fibroin protein solution is filtered with absorbent cotton
In, cryo-conservation is spare.
The preparation of 2 fibroin albumen hemostatic material of embodiment
(1) adjusting the concentration of the pure silk fibroin protein solution in embodiment 1 with deionized water is 15g/L, obtains fibroin albumen
Aqueous solution.Riboflavin is added into silk fibroin water solution, is uniformly mixed and obtains mixed liquor, the concentration of riboflavin is in mixed liquor
0.1mM。
Under the irradiation of ultraviolet light, the active oxygen radical based on the transfer generation singlet oxygen of energy occurs for riboflavin,
Active oxygen radical can react with various molecules, and the tyrosine residue group in fibroin albumen macromolecular is induced to generate chemistry
Crosslinking, thus gelation.
(2) pure oxygen is produced using oxygenerator, oxygen 15min is continually fed into mixed liquor, keep oxygen in the mixed liquor
Gas partial pressure is in a saturated state.
(3) oxygen-saturated mixed liquor is poured into transparent mould such as beaker, so that the depth of mixed liquor is 10mm, and is put into
Cooling in ice bath, ice bath temperature is 4 DEG C.
Due to mixed liquor depth as shallow, the powder of formation is prepared, large specific surface area not only has quickly to be combined with water and is swollen again
Performance, it is same that there is the performance quickly sucked blood.And mixed liquor depth is shallower that crosslinking points is made to be more evenly distributed, limiting crystal knot
The generation of structure.
(4) mixed liquor is used to ultraviolet light, the silk fibroin hydrogel being crosslinked in the low temperature environment of ice bath.
Ice bath temperature be 4 DEG C, the parameter of ultraviolet light are as follows: light source be power 300W, 350~400nm of wavelength it is ultraviolet
Lamp；The distance of ultraviolet light is 10cm；The time of ultraviolet light is 15min.
Mixed liquor containing fibroin albumen and riboflavin can also absorb the big calorimetric of ultraviolet light releasing while photocuring
Can, mixeding liquid temperature is excessively high to promote molecular conformation to change, part beta sheet structure is generated, by improving irradiation distance,
And crosslinking can effectively reduce reaction temperature under the low temperature environment of ice bath, and the gel to be formed is made to keep the random coil in mixed liquor
Structure, so that the generation of effectively limiting crystal structure, greatly promotes the Swelling Capacity of material.Reducing mixed liquor depth can make to be crosslinked
Point is more evenly distributed, the generation of limiting crystal structure.
(5) silk fibroin hydrogel is removed from the molds, and in 20 DEG C of temperature, the constant temperature low moisture environments that humidity is 40%
Middle forced air drying 8h, obtains fibroin albumen xerogel.
(6) fibroin albumen dry gel powder is broken into the powder that partial size is 0.5mm, obtains fibroin albumen hemostatic material.
There is biggish porosity inside powdered gel, ensure that the height of the hemostatic material is sucked blood multiplying power and speed of sucking blood
Degree.Fibroin albumen hemostatic material obtained can reach physics and block blood vessel and hemostasis purpose, and anthemorrhagic performance is excellent.And by fibroin egg
The lesser powder of partial size, which is made, after crushing in white spirit gel can increase material specific surface area, promote material and quickly suck blood ability.
The preparation method of the present embodiment can effectively reduce reaction temperature by being crosslinked under the low temperature environment of ice bath, make to be formed
Gel keep the random coil structure in mixed liquor, so that the generation of effectively limiting crystal structure, greatly promotes the molten of material
Swollen ability and the performance quickly sucked blood；In preparation process, riboflavin only joined, therefore the fibroin albumen hemostatic material has
Good biocompatibility and degradability；Fibroin albumen hemostatic material is powdered, large specific surface area, is not only had fast with water
Speed combines the performance being swollen again, same to have the performance quickly sucked blood；Fibroin material be it is powdered, inside powdered gel
With biggish porosity, it ensure that the height of the hemostatic material is sucked blood multiplying power and speed of sucking blood.
The preparation of 3 fibroin albumen hemostatic material of embodiment
(1) adjusting the concentration of the pure silk fibroin protein solution in embodiment 1 with deionized water is 15g/L, obtains fibroin albumen
Aqueous solution.Riboflavin is added into silk fibroin water solution, is uniformly mixed and obtains mixed liquor, the concentration of riboflavin is in mixed liquor
0.2mM。
(2) pure oxygen is produced using oxygenerator, oxygen 10min is continually fed into mixed liquor, keep oxygen in the mixed liquor
Gas partial pressure is in a saturated state.
(3) oxygen-saturated mixed liquor is poured into transparent mould such as beaker, so that the depth of mixed liquor is 15mm, and is put into
Cooling in ice bath, ice bath temperature is 6 DEG C.
(4) mixed liquor is used to ultraviolet light, the silk fibroin hydrogel being crosslinked in the low temperature environment of ice bath.
Ice bath temperature be 6 DEG C, the parameter of ultraviolet light are as follows: light source be power 100W, 350~400nm of wavelength it is ultraviolet
Lamp；The distance of ultraviolet light is 15cm；The time of ultraviolet light is 20min.
(5) silk fibroin hydrogel is removed from the molds, and in 25 DEG C of temperature, the constant temperature low moisture environments that humidity is 30%
Middle forced air drying 5h, obtains fibroin albumen xerogel.
(6) fibroin albumen dry gel powder is broken into the powder that partial size is 0.4mm, obtains fibroin albumen hemostatic material.
The preparation of 4 fibroin albumen hemostatic material of embodiment
(1) adjusting the concentration of the pure silk fibroin protein solution in embodiment 1 with deionized water is 20g/L, obtains fibroin albumen
Aqueous solution.Riboflavin is added into silk fibroin water solution, is uniformly mixed and obtains mixed liquor, the concentration of riboflavin is in mixed liquor
0.3mM。
(2) pure oxygen is produced using oxygenerator, oxygen 8min is continually fed into mixed liquor, keep oxygen in the mixed liquor
It divides in a saturated state.
(3) oxygen-saturated mixed liquor is poured into transparent mould such as beaker, so that the depth of mixed liquor is 18mm, and is put into
Cooling in ice bath, ice bath temperature is 8 DEG C.
(4) mixed liquor is used to ultraviolet light, the silk fibroin hydrogel being crosslinked in the low temperature environment of ice bath.
Ice bath temperature be 8 DEG C, the parameter of ultraviolet light are as follows: light source be power 50WW, 350~400nm of wavelength it is ultraviolet
Lamp；The distance of ultraviolet light is 20cm；The time of ultraviolet light is 22min.
(5) silk fibroin hydrogel is removed from the molds, and in 28 DEG C of temperature, the constant temperature low moisture environments that humidity is 30%
Middle forced air drying 2h, obtains fibroin albumen xerogel.
(6) fibroin albumen dry gel powder is broken into the powder that partial size is 0.3mm, obtains fibroin albumen hemostatic material.
The preparation of 5 fibroin albumen hemostatic material of embodiment
(1) adjusting the concentration of the pure silk fibroin protein solution in embodiment 1 with deionized water is 20g/L, obtains fibroin albumen
Aqueous solution.Riboflavin is added into silk fibroin water solution, is uniformly mixed and obtains mixed liquor, the concentration of riboflavin is in mixed liquor
0.4mM。
(2) pure oxygen is produced using oxygenerator, oxygen 13min is continually fed into mixed liquor, keep oxygen in the mixed liquor
Gas partial pressure is in a saturated state.
(3) oxygen-saturated mixed liquor is poured into transparent mould such as beaker, so that the depth of mixed liquor is 20mm, and is put into
Cooling in ice bath, ice bath temperature is 2 DEG C.
(4) mixed liquor is used to ultraviolet light, the silk fibroin hydrogel being crosslinked in the low temperature environment of ice bath.
Ice bath temperature be 2 DEG C, the parameter of ultraviolet light are as follows: light source be power 150W, 350~400nm of wavelength it is ultraviolet
Lamp；The distance of ultraviolet light is 18cm；The time of ultraviolet light is 17min.
(5) silk fibroin hydrogel is removed from the molds, and in 30 DEG C of temperature, the constant temperature low moisture environments that humidity is 35%
Middle forced air drying 3h, obtains fibroin albumen xerogel.
(6) fibroin albumen dry gel powder is broken into the powder that partial size is 0.6mm, obtains fibroin albumen hemostatic material.
The preparation of 6 fibroin albumen hemostatic material of embodiment
(1) adjusting the concentration of the pure silk fibroin protein solution in embodiment 1 with deionized water is 20g/L, obtains fibroin albumen
Aqueous solution.Riboflavin is added into silk fibroin water solution, is uniformly mixed and obtains mixed liquor, the concentration of riboflavin is in mixed liquor
0.5mM。
(2) pure oxygen is produced using oxygenerator, oxygen 9min is continually fed into mixed liquor, keep oxygen in the mixed liquor
It divides in a saturated state.
(3) oxygen-saturated mixed liquor is poured into transparent mould such as beaker, so that the depth of mixed liquor is 20mm, and is put into
Cooling in ice bath, ice bath temperature is 0 DEG C.
(4) mixed liquor is used to ultraviolet light, the silk fibroin hydrogel being crosslinked in the low temperature environment of ice bath.
Ice bath temperature be 0 DEG C, the parameter of ultraviolet light are as follows: light source be power 250W, 350~400nm of wavelength it is ultraviolet
Lamp；The distance of ultraviolet light is 12cm；The time of ultraviolet light is 15min.
(5) silk fibroin hydrogel is removed from the molds, and in 27 DEG C of temperature, the constant temperature low moisture environments that humidity is 45%
Middle forced air drying 8h, obtains fibroin albumen xerogel.
(6) fibroin albumen dry gel powder is broken into the powder that partial size is 0.7mm, obtains fibroin albumen hemostatic material.
The preparation of 7 fibroin albumen hemostatic material of embodiment
(1) adjusting the concentration of the pure silk fibroin protein solution in embodiment 1 with deionized water is 30g/L, obtains fibroin albumen
Aqueous solution.Riboflavin is added into silk fibroin water solution, is uniformly mixed and obtains mixed liquor, the concentration of riboflavin is in mixed liquor
0.1mM。
(2) pure oxygen is produced using oxygenerator, oxygen 11min is continually fed into mixed liquor, keep oxygen in the mixed liquor
Gas partial pressure is in a saturated state.
(3) oxygen-saturated mixed liquor is poured into transparent mould such as beaker, so that the depth of mixed liquor is 14mm, and is put into
Cooling in ice bath, ice bath temperature is 4 DEG C.
(4) mixed liquor is used to ultraviolet light, the silk fibroin hydrogel being crosslinked in the low temperature environment of ice bath.
Ice bath temperature be 4 DEG C, the parameter of ultraviolet light are as follows: light source be power 300W, 350~400nm of wavelength it is ultraviolet
Lamp；The distance of ultraviolet light is 14cm；The time of ultraviolet light is 20min.
(5) silk fibroin hydrogel is removed from the molds, and in 23 DEG C of temperature, the constant temperature low moisture environments that humidity is 38%
Middle forced air drying 8h, obtains fibroin albumen xerogel.
(6) fibroin albumen dry gel powder is broken into the powder that partial size is 0.2mm, obtains fibroin albumen hemostatic material.
The preparation of 8 fibroin albumen hemostatic material of embodiment
(1) adjusting the concentration of the pure silk fibroin protein solution in embodiment 1 with deionized water is 30g/L, obtains fibroin albumen
Aqueous solution.Riboflavin is added into silk fibroin water solution, is uniformly mixed and obtains mixed liquor, the concentration of riboflavin is in mixed liquor
0.2mM。
(2) mixed liquor is poured into transparent mould such as beaker, so that the depth of mixed liquor is 10mm, and is put into cold in ice bath
But, ice bath temperature is 6 DEG C.
(3) pure oxygen is produced using oxygenerator, oxygen 15min is continually fed into mixed liquor, keep oxygen in the mixed liquor
Gas partial pressure is in a saturated state.
(4) mixed liquor is used to ultraviolet light, the silk fibroin hydrogel being crosslinked in the low temperature environment of ice bath.
Ice bath temperature be 6 DEG C, the parameter of ultraviolet light are as follows: light source be power 500W, 350~400nm of wavelength it is ultraviolet
Lamp；The distance of ultraviolet light is 16cm；The time of ultraviolet light is 20min.
(5) silk fibroin hydrogel is removed from the molds, and the dry 20h film forming in constant temperature low moisture environments, obtains silk
Fibroin xerogel.
(6) fibroin albumen dry gel powder is broken into the powder that partial size is 0.2mm, obtains fibroin albumen hemostatic material.
The preparation of 9 fibroin albumen hemostatic material of embodiment
(1) adjusting the concentration of the pure silk fibroin protein solution in embodiment 1 with deionized water is 30g/L, obtains fibroin albumen
Aqueous solution.Riboflavin is added into silk fibroin water solution, is uniformly mixed and obtains mixed liquor, the concentration of riboflavin is in mixed liquor
0.3mM。
(2) mixed liquor is poured into transparent mould such as beaker, so that the depth of mixed liquor is 10mm, and is put into cold in ice bath
But, ice bath temperature is 8 DEG C.
(3) pure oxygen is produced using oxygenerator, oxygen 15min is continually fed into mixed liquor, keep oxygen in the mixed liquor
Gas partial pressure is in a saturated state.
(4) mixed liquor is used to ultraviolet light, the silk fibroin hydrogel being crosslinked in the low temperature environment of ice bath.
Ice bath temperature be 8 DEG C, the parameter of ultraviolet light are as follows: light source be power 400W, 350~400nm of wavelength it is ultraviolet
Lamp；The distance of ultraviolet light is 20cm；The time of ultraviolet light is 20min.
(5) silk fibroin hydrogel is removed from the molds, and the dry 20h film forming in constant temperature low moisture environments, obtains silk
Fibroin xerogel.
(6) fibroin albumen dry gel powder is broken into the powder that partial size is 0.2mm, obtains fibroin albumen hemostatic material.
The preparation of 10 fibroin albumen hemostatic material of embodiment
(1) adjusting the concentration of the pure silk fibroin protein solution in embodiment 1 with deionized water is 30g/L, obtains fibroin albumen
Aqueous solution.Riboflavin is added into silk fibroin water solution, is uniformly mixed and obtains mixed liquor, the concentration of riboflavin is in mixed liquor
0.4mM。
(2) mixed liquor is poured into transparent mould such as beaker, so that the depth of mixed liquor is 10mm, and is put into cold in ice bath
But, ice bath temperature is 4 DEG C.
(3) pure oxygen is produced using oxygenerator, oxygen 15min is continually fed into mixed liquor, keep oxygen in the mixed liquor
Gas partial pressure is in a saturated state.
(4) mixed liquor is used to ultraviolet light, the silk fibroin hydrogel being crosslinked in the low temperature environment of ice bath.
Ice bath temperature be 4 DEG C, the parameter of ultraviolet light are as follows: light source be power 450W, 350~400nm of wavelength it is ultraviolet
Lamp；The distance of ultraviolet light is 20cm；The time of ultraviolet light is 30min.
(5) silk fibroin hydrogel is removed from the molds, and constant temperature low moisture environments in dry 20h film forming, obtain
Fibroin albumen xerogel.
(6) fibroin albumen dry gel powder is broken into the powder that partial size is 0.3mm, obtains fibroin albumen hemostatic material.
The preparation of 11 fibroin albumen hemostatic material of embodiment
(1) adjusting the concentration of the pure silk fibroin protein solution in embodiment 1 with deionized water is 30g/L, obtains fibroin albumen
Aqueous solution.Riboflavin is added into silk fibroin water solution, is uniformly mixed and obtains mixed liquor, the concentration of riboflavin is in mixed liquor
0.5mM。
(2) mixed liquor is poured into transparent mould such as beaker, so that the depth of mixed liquor is 10mm, and is put into cold in ice bath
But, ice bath temperature is 4 DEG C.
(3) pure oxygen is produced using oxygenerator, oxygen 15min is continually fed into mixed liquor, keep oxygen in the mixed liquor
Gas partial pressure is in a saturated state.
(4) mixed liquor is used to ultraviolet light, the silk fibroin hydrogel being crosslinked in the low temperature environment of ice bath.
Ice bath temperature be 4 DEG C, the parameter of ultraviolet light are as follows: light source be power 400W, 350~400nm of wavelength it is ultraviolet
Lamp；The distance of ultraviolet light is 10cm；The time of ultraviolet light is 20min.
(5) silk fibroin hydrogel is removed from the molds, and the dry 20h film forming in constant temperature low moisture environments, obtains silk
Fibroin xerogel.
(6) fibroin albumen dry gel powder is broken into the powder that partial size is 0.3mm, obtains fibroin albumen hemostatic material.
Comparative example 1
This comparative example and the preparation process in embodiment 2 are almost the same, and distinctive points are the ultraviolet lighting in this comparative example
Penetrating environment is room temperature, i.e., handles in ultraviolet light without cooling.
Comparative example 2
This comparative example and the preparation process in embodiment 2 are almost the same, and distinctive points are the ultraviolet lighting in this comparative example
Keep the distance between ultraviolet light and reaction solution within 5cm when penetrating.
Comparative example 3
This comparative example and the preparation process in embodiment 2 are almost the same, and distinctive points are in this comparative example ultraviolet in progress
The depth of reaction solution is 50mm in transparent mould when light irradiates.
The test of embodiment 6 and analysis
The fibroin albumen hemostatic material test that embodiment 2-11 and comparative example 1-3 are prepared suck blood multiplying power, blood coagulation when
Between.Wherein, the test method for multiplying power of sucking blood be unit quality (1 gram) fibroin material suck blood saturation after increased quality with
The ratio between former dry mass；Clotting time measurement is that fibroin material is sucked blood time for solidifying of blood after saturation.As a result
It is shown in Table 1.
1 experimental result of table
| Sample | It sucks blood multiplying power | Clotting time (S) |
| Embodiment 2 | 11.1 | 58 |
| Embodiment 3 | 8.9 | 63 |
| Embodiment 4 | 8.6 | 69 |
| Embodiment 5 | 8.3 | 79 |
| Embodiment 6 | 7.9 | 80 |
| Embodiment 7 | 9.8 | 59 |
| Embodiment 8 | 8.7 | 67 |
| Embodiment 9 | 9.3 | 71 |
| Embodiment 10 | 10.8 | 55 |
| Embodiment 11 | 8.5 | 68 |
| Comparative example 1 | 4.5 | 90 |
| Comparative example 2 | 6.6 | 85 |
| Comparative example 3 | 3.5 | 98 |
The fibroin egg of embodiment 2-11 is prepared as can be seen from Table 1 fibroin albumen hemostatic material and comparative example 1-3
White hemostatic material is compared, since mixed liquor being placed under the low temperature environment of ice bath when ultraviolet light irradiates in embodiment 2-11, and
It elongated the distance of ultraviolet light, be thinned the depth of reaction solution, so that obtained fibroin albumen hemostatic material effectively limits
The generation of crystalline texture is random coil structure, has suck blood well multiplying power and speed of sucking blood faster.
The present invention is by having the fibroin albumen hemostatic material of quick-acting haemostatic powder performance using fibroin albumen as raw material preparation, in silk
Riboflavin is added in fibroin aqueous solution, is continually fed into oxygen, and uses ultraviolet light in the low temperature environment of ice bath, forms water
Gel, hydrogel is dry and is ground into powder, forms fibroin albumen hemostatic material, preparation process is simple and convenient, the core yellow of addition
Cellulose content is extremely low, can sufficiently keep the biocompatibility of fibroin itself, and fibroin albumen hemostatic material obtained can reach physics envelope
Stifled blood vessel and hemostasis purpose, anthemorrhagic performance are excellent；It can effectively reduce reaction temperature by being crosslinked under the low temperature environment of ice bath, make
The gel of formation keeps the random coil structure in mixed liquor, so that the generation of effectively limiting crystal structure, greatly promotes material
Swelling Capacity and the performance quickly sucked blood.The fibroin albumen hemostatic material being prepared is powdered, large specific surface area, no
Only have and is quickly combined the performance being swollen again with water, it is same that there is the performance quickly sucked blood.Have inside powdered gel larger
Porosity, ensure that the height of the hemostatic material is sucked blood and multiplying power and suck blood speed.Therefore the fibroin albumen hemostatic material has wink
When the good performance of swelling, multiplying power of sucking blood height, quick-acting haemostatic powder, degradability, can be used for the hemostatic material of wound and tissue repair.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention, it is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of fibroin albumen hemostatic material, which comprises the following steps:
(1) photosensitizer riboflavin is added into silk fibroin water solution, is uniformly mixed and obtains mixed liquor；
(2) it is continually fed into oxygen in Xiang Suoshu mixed liquor, keeps oxygen partial pressure in the mixed liquor in a saturated state；
(3) the oxygen-saturated mixed liquor is poured into transparent mould and is cooled down；
(4) mixed liquor described in ultraviolet light, the silk fibroin hydrogel being crosslinked control institute during ultraviolet light
The temperature for stating mixed liquor is 0~8 DEG C；
(5) silk fibroin hydrogel is removed from the molds and is dried, obtain fibroin albumen xerogel；
(6) the fibroin albumen dry gel powder is broken into powder, obtains fibroin albumen hemostatic material.
2. the preparation method of fibroin albumen hemostatic material according to claim 1, which is characterized in that described in step (1)
The concentration of silk fibroin water solution is 15g/L~30g/L；In the mixed liquor concentration of riboflavin be 0.1mmol/L~
0.5mmol/L。
3. the preparation method of fibroin albumen hemostatic material according to claim 1, which is characterized in that described in step (3)
The depth of mixed liquor in transparent mould is 10mm~30mm.
4. the preparation method of fibroin albumen hemostatic material according to claim 1, which is characterized in that ultraviolet in step (4)
The parameter of light irradiation are as follows: the distance of ultraviolet light is 10cm~20cm；The time of ultraviolet light is 5min~30min.
5. the preparation method of fibroin albumen hemostatic material according to claim 1, which is characterized in that the purple in step (4)
The ultraviolet light that outer light is power 50W~500W, the ultraviolet lamp of 350~400nm of wavelength issues.
6. the preparation method of fibroin albumen hemostatic material according to claim 1, which is characterized in that dry in step (5)
Environment be 20~30 DEG C of temperature, relative humidity 10~50% constant-temperature constant-humidity environment.
7. the preparation method of fibroin albumen hemostatic material according to claim 1, which is characterized in that described in step (6)
The partial size of powder is 0.1~1mm.
8. the preparation method of fibroin albumen hemostatic material according to claim 1, which is characterized in that fibroin in step (1)
The preparation of protein solution includes the following steps: using Cocoon shell as raw material, obtains fibroin albumen by degumming, dissolution, dialysis
Solution is added deionized water in silk fibroin protein solution and obtains silk fibroin water solution.
9. a kind of fibroin albumen hemostatic material that the preparation method using as described in claim 1-8 any one is prepared.
10. fibroin albumen hemostatic material according to claim 9, which is characterized in that the fibroin albumen hemostatic material
Multiplying power of sucking blood is 7.5~11.5, and the clotting time is 55~80s.
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