CN116421771A - Novel porous starch hemostatic powder and preparation method and application thereof - Google Patents
Novel porous starch hemostatic powder and preparation method and application thereof Download PDFInfo
- Publication number
- CN116421771A CN116421771A CN202310374825.9A CN202310374825A CN116421771A CN 116421771 A CN116421771 A CN 116421771A CN 202310374825 A CN202310374825 A CN 202310374825A CN 116421771 A CN116421771 A CN 116421771A
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- starch
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- porous starch
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Abstract
The invention discloses novel porous starch hemostatic powder and a preparation method and application thereof, and belongs to the technical field of biomedical materials. The novel porous starch hemostatic powder disclosed by the invention comprises the following components in parts by weight: 80-100 parts of porous starch styptic powder, 1-5 parts of modified konjac glucomannan, 1-3 parts of poly L-lysine and 1-3 parts of modified collagen; the preparation method of the novel porous starch hemostatic powder comprises ball milling treatment, emulsification treatment, ultrasonic acid hydrolysis, ultrasonic enzyme hydrolysis, modification treatment and composite treatment. The invention has excellent water absorption performance, hydrogel performance, hemostatic performance, blood coagulation performance and the like through the synergistic effects of polysaccharide and polypeptide compounding, blending modification, ball milling modification, ultrasonic acid enzyme, nano material modification and the like, and can be applied to the fields of hemostasis and blood coagulation.
Description
Technical Field
The invention belongs to the technical field of biomedical materials, and particularly relates to novel porous starch hemostatic powder and a preparation method and application thereof.
Background
In daily life, bleeding is often caused by sudden accidents, natural disasters, operations, first aid, war and the like. Although the human body can stop bleeding by a physiological hemostasis mechanism, the coagulation time of the human body is long, and under the condition of massive bleeding, the physiological hemostasis effect is almost negligible, and if the physiological hemostasis effect cannot be timely and effectively controlled, the life health of wounded persons, even life safety, can be seriously threatened. The research and development of hemostatic materials have been the focus of attention at home and abroad, and particularly effective and safe hemostatic materials are important points in the hot spots.
In recent years, with the rapid development of biomedicine, materials science and bioengineering, biological hemostatic materials have shown great potential. Various types of hemostatic materials have been developed, and the current hemostatic materials mainly include gelatins, collagens, oxidized celluloses, regenerated oxidized celluloses, starches and the like. The starch has the advantages of excellent hemostatic performance, wide sources, good biocompatibility, lower preparation cost, easy degradation and absorption in human body, less stress reaction and the like, so that the starch is widely applied to hemostasis.
Starch is a plant polysaccharide which has the most extensive application, low price and no cytotoxicity, has good biocompatibility, is nontoxic and nonirritating, is not easy to cause anaphylactic reaction of organisms, can be degraded into monosaccharide in vivo by amylase in body fluid, and can be degraded and absorbed in vivo. Starch contains a large number of hydroxyl groups and there are many modified products such as gelatinized starch, porous starch, crosslinked starch, etc. The porous starch can increase the viscosity of blood by absorbing water in the blood, gather a large amount of red blood cells, platelets, coagulation factors and the like on the surface of starch particles, and achieve the hemostatic effect by means of the blood coagulation mechanism, so that the porous starch becomes one of excellent hemostatic materials.
Porous starch is a modified starch, also known as microporous starch. The porous starch carrier is prepared by subjecting natural starch to enzymatic hydrolysis treatment or other treatment at a temperature lower than gelatinization temperature. However, the existing porous starch preparation method is easy to appear, after micropores are formed on the surfaces of starch particles, the structure is unstable, the adhesiveness is poor, the starch is easy to collapse after water absorption, the hemostatic effect of the starch is affected, and the application of the starch is further limited.
Disclosure of Invention
The invention aims to solve the technical problems that porous starch microporous particles in the prior art are unstable in structure and poor in adhesiveness and are easy to collapse after absorbing water, and provides novel porous starch hemostatic powder and a preparation method and application thereof.
The technical scheme adopted by the invention for solving the problems is as follows:
the invention provides novel porous starch hemostatic powder which comprises the following raw materials in parts by weight: 80-100 parts of porous starch styptic powder, 1-5 parts of modified konjaku gum, 1-3 parts of poly L-lysine and 1-3 parts of modified collagen.
Further, the modified konjac glucomannan is prepared by blending 10-15 parts of konjac glucomannan, 1-2 parts of chitosan and 1-2 parts of sodium hyaluronate; the modified collagen is prepared by blending and modifying 10-15 parts of gelatin, 3-5 parts of silk fibroin, 1-3 parts of alginic acid, 2-4 parts of carboxymethyl cellulose and 1-2 parts of bioactive glass.
The preparation method of the novel porous starch hemostatic powder comprises the following steps:
s1, starch pretreatment
S11, ball milling treatment
Firstly, passing starch through a 200-target standard test sieve, and then, according to the starch: absolute ethyl alcohol: adding zirconia balls into a ball milling tank according to the weight ratio of 1:1:1, and fixing the ball milling tank on a planetary ball mill with the rotating speed of 300-500 r/min for ball milling for 30-60 min; finally taking out the mixture after ball milling, and placing the mixture in an oven at 40-60 ℃ for drying for 2 hours.
Further, the starch is prepared from tapioca starch: corn starch is 1:2-3 weight ratio.
S12, emulsifying treatment
Firstly mixing the starch treated by the S11 with pure water according to the weight ratio of 1:10-20, adjusting the pH to 9-10 after magnetically stirring for 2-4 h, and continuously stirring for 1-2 h.
Further, the milk mixing is to adjust the concentration of the starch emulsion to 30% -50%.
Further, the magnetic stirring speed is 300-500 rpm.
S2, ultrasonic acid enzyme modification treatment
S21, ultrasonic acid hydrolysis
Firstly mixing the starch suspension treated by the S12 with an acidic solution, and then placing the mixture under the condition of 300-500W of power for ultrasonic treatment for 1-2 hours, and then regulating the pH value to 5-6 by using an inorganic salt solution.
Further, the starch suspension is mixed with an acidic solution according to the starch suspension: the acid solution is 20-30: mixing at a volume ratio of 1.
Further, the acidic solution is any one or combination of hydrochloric acid and sulfuric acid with the concentration of 1-4 mol/L.
Further, the inorganic salt solution is any one or a combination of more than one of sodium chloride, potassium chloride, calcium chloride, sodium carbonate and sodium bicarbonate with the concentration of 1-2 mol/L.
S22, ultrasonic enzyme hydrolysis
(1) Firstly, placing acidolysis solution treated by S21 under the condition of 200-300W of power for ultrasonic treatment for 1-2 hours, then placing the acidolysis solution in a water bath kettle at 50-60 ℃ for preheating for 10-20 minutes, and finally adding alpha-amylase for enzymolysis;
(2) And (3) placing the alpha-amylase enzymolysis liquid into a water bath kettle at 40-60 ℃ for preheating for 20-30 min after ultrasonic treatment for 1-2 h under the condition of 200-300W of power, and finally adding saccharifying enzyme for enzymolysis.
Further, the addition amount of the alpha-amylase is 0.1 to 0.5 weight percent of acidolysis solution, and the enzymolysis is carried out for 2 to 6 hours; the addition amount of the saccharifying enzyme is 0.4-0.8wt% of alpha-amylase enzymatic hydrolysate, and the enzymatic hydrolysis is carried out for 4-6 hours.
S3, modification treatment
S31, placing the enzyme solution treated in the step S22 under the ultrasonic condition with the power of 300-500W, adding the pore-forming agent, and stirring to uniformly disperse the pore-forming agent in the enzymolysis liquid to obtain a dispersion liquid.
And S32, sequentially adding nano calcium bentonite and medical polyvinyl alcohol into the dispersion liquid treated in the step S31, and stirring and mixing to obtain a blend liquid.
S33, firstly adding 1-3% of hydrochloric acid or sulfuric acid and 60-70% of ethanol solution into the blending solution processed by the S32 to remove the pore-forming agent, wherein the addition amount of the blending solution is 0.1-0.5 wt%, and then carrying out centrifugal separation treatment on the blending solution, wherein the centrifugal speed is 3000-4000 rpm, the time is 20-30 min, and the steps are repeated for 3-5 times.
S34, washing the product treated in the step S33 for 3 times, drying at 60 ℃ for 6-8 hours, and finally crushing and sieving with a 200-target standard test sieve to obtain the porous starch hemostatic powder.
Further, the addition amount of the pore-foaming agent is 0.05 to 0.1 weight percent of enzymolysis liquid; the pore-foaming agent is a mixed solution of hydrogen peroxide solution with the weight percent of 1-3 and sodium bicarbonate solution with the weight percent of 0.5-1; the volume ratio of the hydrogen peroxide solution to the sodium bicarbonate solution is 2:1.
Further, the addition of the nano calcium bentonite and the medical polyvinyl alcohol is 1-3wt% of dispersion liquid, the particle size of the nano calcium bentonite is 10-50 nm, and the particle size of the medical polyvinyl alcohol is 1-3 mu m.
S4, compounding treatment
S41, compounding porous starch hemostatic powder, modified konjaku gum, poly-L-lysine and modified collagen according to parts by weight.
S42, grinding, sieving, packaging and sterilizing the compound processed in the step S41.
Further, the screening material is a 300-target quasi-inspection screening; the sterilization refers to Co60 irradiation sterilization, and the irradiation dose is 1-6 KGy.
The novel porous starch hemostatic powder can be applied to the field of hemostasis and coagulation.
The beneficial effects of the invention are as follows:
1. the invention adopts polysaccharides (starch and konjac gum) and polypeptides (poly-L-lysine and collagen) for compounding, which not only overcomes the defect of the traditional single component, but also realizes the function of improving the hemostatic powder. Meanwhile, in order to further improve the function of the hemostatic powder composite hydrogel, the konjac glucomannan, chitosan and sodium hyaluronate are blended to generate a synergistic effect, so that the stability and adhesiveness of the hemostatic powder in forming the composite hydrogel in wounds are improved; the gelatin, silk fibroin, alginic acid, carboxymethyl cellulose and bioactive glass are used for blending and modifying collagen, and different materials form complementation and interaction, so that the structural integrity, stability and adhesiveness of the hemostatic powder are improved, and especially the hemostatic performance and the blood flow resistance are improved.
2. According to the invention, corn starch and tapioca starch are used as raw materials, the particle shapes of the corn starch and tapioca starch are round, and the round and round are mixed, so that uniform mixing is facilitated, and meanwhile, the use of irregular-shape incompressible bleeding wounds is facilitated. The amylose content of the cassava starch is relatively low, which is favorable for forming a porous structure and enhancing the adsorption capacity; the jade forest starch has relatively low branched chain content, is favorable for stable structure, enhances the flushing resistance and forms complementary advantages. Therefore, the high stability structure and adhesiveness of the blood meal are further ensured by proper proportioning of the corn starch and the tapioca starch.
3. The invention adopts ball milling pretreatment, on one hand, the specific surface area and the reactivity of starch can be improved, and the production time is reduced; on the other hand, the collision between the starch and the zirconia balls can break the macromolecular chains of the starch, reduce the ordered structure of the crystallization area of the starch, and enable the starch particles to form cracks and holes, so that the water absorption capacity is stronger. Meanwhile, the invention also adopts ultrasonic to assist the acid enzyme hydrolysis, improves the hydrolysis efficiency of the starch, and simultaneously improves the water absorption performance and pore-forming quality of the starch.
4. The invention adopts pore-forming agent, nano calcium bentonite and medical polyvinyl alcohol for modification, wherein, the mixture of hydrogen peroxide solution and sodium bicarbonate solution is adoptedThe liquid is used as pore-forming agent, so that the surface and the internal structure of the hemostatic powder have a plurality of microporous structures with different apertures, the specific surface area is larger, and the liquid absorbing capacity and the hemostatic capacity are improved. The nanometer calcium bentonite has the function of an ion cross-linking agent, can generate chemical bonds among hemostatic powder particles, is mutually connected to form a three-dimensional reticular microporous structure, enhances the water absorption of the hemostatic powder particles, can polymerize with medical polyvinyl alcohol and the like, absorbs liquid to quickly form hydrogel, and simultaneously contains Ca 2+ Ions also accelerate activation of endogenous coagulation factors, further optimizing hemostatic performance. Furthermore, the medical polyvinyl alcohol can quickly form the network hydrogel with better adhesiveness after absorbing water, and can increase the concentration of blood coagulation factors and platelets, thereby playing a role in blood coagulation, improving the hemostatic effect and reducing the time required by hemostasis. In addition, nanometer calcium bentonite can be embedded into the micropore of the hemostatic powder, and medical polyvinyl alcohol is embedded into the micropore surface of the hemostatic powder, when the hemostatic powder forms hydrogel during imbibition, the double structure can ensure that absorbed liquid is locked in the micropore, the structure is not washed away and collapsed after excessive imbibition, the original structure is lost, and the good original structure can be maintained while a large amount of imbibition is realized.
Drawings
Fig. 1 is a scanning electron microscope picture of the novel porous starch styptic powder prepared in example 1.
Detailed Description
Example 1
The novel porous starch hemostatic powder comprises the following raw materials in parts by weight: 90 parts of porous starch styptic powder, 3 parts of modified konjak gum, 2 parts of poly-L-lysine and 2 parts of modified collagen. Wherein, the modified konjak gum is prepared by blending and modifying 13 parts of konjak gum, 2 parts of chitosan and 2 parts of sodium hyaluronate; the modified collagen is prepared by blending and modifying 12 parts of gelatin, 4 parts of silk fibroin, 2 parts of alginic acid, 3 parts of carboxymethyl cellulose and 2 parts of bioactive glass.
The preparation method of the novel porous starch hemostatic powder comprises the following steps:
s1, starch pretreatment
S11, ball milling treatment
Firstly, passing tapioca starch and corn starch in a weight ratio of 1:2 through a 200-target standard test sieve, and then, according to starch: absolute ethyl alcohol: adding zirconia balls into a ball milling tank according to the weight ratio of 1:1:1, and fixing the ball milling tank on a planetary ball mill with the rotating speed of 400r/min for ball milling for 40min; finally, taking out the mixture after ball milling, and placing the mixture in a baking oven at 50 ℃ for 2 hours.
S12, emulsifying treatment
Mixing the starch treated by the step S11 with pure water according to the weight ratio of 1:15, adjusting the concentration of the starch emulsion to 40%, magnetically stirring for 3 hours at the stirring speed of 400rpm, adjusting the pH to 9 by using a sodium hydroxide solution, and continuously stirring for 1.5 hours.
S2, ultrasonic acid enzyme modification treatment
S21, ultrasonic acid hydrolysis
Firstly, treating the starch suspension treated by the step S12 according to the starch suspension: 3mol/L hydrochloric acid solution 25:1 volume ratio, and after being placed under the condition of 400W power for ultrasonic treatment for 1.5 hours, the pH value is regulated to 5.5 by using 1.5mol/L sodium chloride solution.
S22, ultrasonic enzyme hydrolysis
(1) Firstly, placing acidolysis solution treated by S21 into a water bath at 55 ℃ for preheating for 15min after ultrasonic treatment for 1.5h under the condition of 250W of power, and finally adding 0.3wt% of alpha-amylase of the acidolysis solution for enzymolysis for 4h;
(2) And (3) placing the alpha-amylase enzymatic hydrolysate into a water bath kettle at 50 ℃ for preheating for 25min after ultrasonic treatment for 1.5h under the condition of 250W of power, and finally adding 0.6wt% of saccharifying enzyme of the alpha-amylase enzymatic hydrolysate for enzymolysis for 5h.
S3, modification treatment
S31, placing the enzyme solution treated in the step S22 under the ultrasonic condition with the power of 400W, adding 0.08wt% of enzymolysis solution, mixing the solution of hydrogen peroxide solution and sodium bicarbonate solution with the volume ratio of 2:1 and 2wt% with the pore-forming agent, and stirring to uniformly disperse the pore-forming agent in the enzymolysis solution to obtain a dispersion liquid.
S32, sequentially adding 30nm nano calcium bentonite of 2wt% of the dispersion liquid and 2 mu m medical polyvinyl alcohol of 2wt% of the dispersion liquid into the dispersion liquid treated in the step S31, and stirring and mixing to obtain a blend liquid.
S33, firstly adding 2% hydrochloric acid and 65% ethanol solution into the blend solution processed in the S32 to remove the pore-forming agent, wherein the addition amounts of the blend solution are 0.3wt%, and then carrying out centrifugal separation treatment on the blend solution, wherein the centrifugal speed is 3500rpm and the time is 25min, and repeating the steps for 4 times.
S34, washing the product treated in the step S33 for 3 times, drying at 60 ℃ for 7 hours, and finally crushing and sieving with a 200-target standard test sieve to obtain the porous starch hemostatic powder.
S4, compounding treatment
S41, compounding 90 parts of porous starch hemostatic powder, 3 parts of modified konjak gum, 2 parts of poly-L-lysine and 2 parts of modified collagen.
S42, sequentially grinding the compound processed in the step S41, sieving with a 300-target standard inspection sieve, packaging, and sterilizing by Co60 irradiation with the irradiation dose of 4KGy.
Example 2
The novel porous starch hemostatic powder comprises the following raw materials in parts by weight: 80 parts of porous starch styptic powder, 1 part of modified konjak gum, 1 part of poly L-lysine and 1 part of modified collagen. Wherein, the modified konjac gum is prepared by blending 10 parts of konjac gum, 1 part of chitosan and 1 part of sodium hyaluronate; the modified collagen is prepared by blending 10 parts of gelatin, 3 parts of silk fibroin, 1 part of alginic acid, 2 parts of carboxymethyl cellulose and 1 part of bioactive glass.
The preparation method of the novel porous starch hemostatic powder comprises the following steps:
s1, starch pretreatment
S11, ball milling treatment
Firstly, passing tapioca starch and corn starch in a weight ratio of 1:2 through a 200-target standard test sieve, and then, according to starch: absolute ethyl alcohol: adding zirconia balls into a ball milling tank according to the weight ratio of 1:1:1, and fixing the ball milling tank on a planetary ball mill with the rotating speed of 300r/min for ball milling for 30min; finally, taking out the mixture after ball milling, and placing the mixture in a baking oven at 40 ℃ for 2 hours.
S12, emulsifying treatment
Mixing the starch treated by the step S11 with pure water according to the weight ratio of 1:10, adjusting the concentration of the starch emulsion to 30%, magnetically stirring for 2 hours at the stirring speed of 300rpm, adjusting the pH to 9 by using a sodium hydroxide solution, and continuously stirring for 1 hour.
S2, ultrasonic acid enzyme modification treatment
S21, ultrasonic acid hydrolysis
Firstly, treating the starch suspension treated by the step S12 according to the starch suspension: 1mol/L hydrochloric acid solution is 20:1 volume ratio, and placing the mixture under the condition of 300W power for ultrasonic treatment for 1h, and then regulating the pH value to 5 by using 1mol/L potassium chloride solution.
S22, ultrasonic enzyme hydrolysis
(1) The acidolysis solution treated by S21 is firstly placed under the condition of 200W for ultrasonic treatment for 1h, then placed in a water bath kettle at 50 ℃ for preheating for 10min, and finally added with 0.1wt% of alpha-amylase for enzymolysis for 2h.
(2) And (3) placing the alpha-amylase enzymolysis liquid into a water bath kettle at 40 ℃ for preheating for 20min after ultrasonic treatment for 1h under the condition of 200W of power, and finally adding 0.4wt% of saccharifying enzyme of the alpha-amylase enzymolysis liquid for enzymolysis for 4h.
S3, modification treatment
S31, placing the enzyme solution treated in the step S22 under the ultrasonic condition with the power of 300W, adding 0.05wt% of enzymolysis solution, mixing the solution of hydrogen peroxide solution and sodium bicarbonate solution with the volume ratio of 2:1 and 1wt% with the pore-forming agent, and stirring to uniformly disperse the pore-forming agent in the enzymolysis solution to obtain a dispersion liquid.
S32, sequentially adding 10nm nano calcium bentonite of 1wt% of the dispersion liquid and 1 mu m medical polyvinyl alcohol of 1wt% of the dispersion liquid into the dispersion liquid treated in the step S31, and stirring and mixing to obtain a blend liquid.
S33, firstly adding 1% sulfuric acid and 60% ethanol solution into the blend solution processed in the S32 to remove the pore-forming agent, wherein the addition amounts of the blend solution are 0.1wt%, and then carrying out centrifugal separation treatment on the blend solution, wherein the centrifugal speed is 3000rpm, the time is 20min, and repeating the steps for 3 times.
S34, washing the product treated in the step S33 for 3 times, drying at 60 ℃ for 6 hours, and finally crushing and sieving with a 200-target standard test sieve to obtain the porous starch hemostatic powder.
S4, compounding treatment
S41, carrying out composite treatment on 80 parts by weight of porous starch hemostatic powder, 1 part by weight of modified konjak gum, 1 part by weight of poly-L-lysine and 1 part by weight of modified collagen.
S42, sequentially grinding the compound processed in the step S41, sieving with a 300-target standard inspection sieve, packaging, and sterilizing by Co60 irradiation with the irradiation dose of 1KGy.
Example 3
The novel porous starch hemostatic powder comprises the following raw materials in parts by weight: 100 parts of porous starch styptic powder, 5 parts of modified konjak gum, 3 parts of poly L-lysine and 3 parts of modified collagen. Wherein, the modified konjac gum is prepared by blending 15 parts of konjac gum, 2 parts of chitosan and 2 parts of sodium hyaluronate; the modified collagen is prepared by blending 15 parts of gelatin, 5 parts of silk fibroin, 3 parts of alginic acid, 4 parts of carboxymethyl cellulose and 2 parts of bioactive glass.
The preparation method of the novel porous starch hemostatic powder comprises the following steps:
s1, starch pretreatment
S11, ball milling treatment
Firstly, passing tapioca starch and corn starch in a weight ratio of 1:3 through a 200-target standard test sieve, and then, according to starch: absolute ethyl alcohol: adding zirconia balls into a ball milling tank according to the weight ratio of 1:1:1, and fixing the ball milling tank on a planetary ball mill with the rotating speed of 500r/min for ball milling for 60min; finally taking out the mixture after ball milling, and placing the mixture in an oven at 60 ℃ for drying for 2 hours.
S12, emulsifying treatment
Mixing the starch treated by the step S11 with pure water according to the weight ratio of 1:20, adjusting the concentration of the starch emulsion to 50%, magnetically stirring for 4 hours at the stirring speed of 500rpm, adjusting the pH to 10 by using a sodium hydroxide solution, and continuously stirring for 2 hours.
S2, ultrasonic acid enzyme modification treatment
S21, ultrasonic acid hydrolysis
Firstly, treating the starch suspension treated by the step S12 according to the starch suspension: the 4mol/L sulfuric acid solution is 30:1 volume ratio, and placing the mixture under the condition of power of 500W for ultrasonic treatment for 2 hours, and then regulating the pH value to 6 by using 2mol/L calcium chloride solution.
S22, ultrasonic enzyme hydrolysis
(1) The acidolysis solution treated by S21 is firstly placed under the condition of 300W for ultrasonic treatment for 2 hours, then placed in a water bath kettle at 60 ℃ for preheating for 20 minutes, and finally added with 0.5 weight percent of alpha-amylase for enzymolysis for 6 hours.
(2) And (3) placing the alpha-amylase enzymolysis liquid into a water bath kettle at 60 ℃ for preheating for 30min after ultrasonic treatment for 2h under the condition of 300W of power, and finally adding 0.8wt% of saccharifying enzyme of the alpha-amylase enzymolysis liquid for enzymolysis for 6h.
S3, modification treatment
S31, placing the enzyme solution treated in the step S22 under an ultrasonic condition with the power of 500W, adding 0.1wt% of enzymolysis solution, and mixing the mixed solution of hydrogen peroxide solution and sodium bicarbonate solution with the volume ratio of 2:1 and 3wt% to obtain a pore-foaming agent, and stirring to uniformly disperse the pore-foaming agent in the enzymolysis solution to obtain a dispersion.
S32, sequentially adding 50nm nano calcium bentonite of 3wt% of the dispersion liquid and 3 mu m medical polyvinyl alcohol of 3wt% of the dispersion liquid into the dispersion liquid treated in the step S31, and stirring and mixing to obtain a blend liquid.
S33, adding 3% hydrochloric acid and 70% ethanol solution into the blend solution processed in the S32 to remove the pore-forming agent, wherein the addition amounts of the blend solution are 0.5wt%, and then carrying out centrifugal separation treatment on the blend solution, wherein the centrifugal speed is 4000rpm, the time is 30min, and repeating the steps for 5 times.
S34, washing the product treated in the step S33 for 3 times, drying at 60 ℃ for 8 hours, and finally crushing and sieving with a 200-target standard test sieve to obtain the porous starch hemostatic powder.
S4, compounding treatment
S41, compounding 100 parts of porous starch hemostatic powder, 5 parts of modified konjak gum, 3 parts of poly-L-lysine and 3 parts of modified collagen.
S42, sequentially grinding the compound processed in the step S41, sieving with a 300-target standard inspection sieve, packaging, and sterilizing by Co60 irradiation with the irradiation dose of 6KGy.
Comparative example 1
Comparative example 1 the preparation conditions were the same as in example 1 except that the novel porous starch styptic powder component was only 90 parts of the porous starch styptic powder.
Comparative example 2
Comparative example 2 the preparation conditions were the same as in example 1 except that the step of ball milling treatment of S11 was not performed.
Comparative example 3
Comparative example 3 the preparation conditions were the same as in example 1 except that no ultrasonic auxiliary treatment was performed in step S2.
Comparative example 4
Comparative example 4 the preparation conditions were the same as in example 1 except that no porogen was added in step S31.
Comparative example 5
Comparative example 5 the preparation conditions were the same as in example 1 except that no nano-calcium bentonite was added in step S32.
Comparative example 6
Comparative example 6 the preparation conditions were the same as in example 1 except that no medical polyvinyl alcohol was added in the step S32.
Comparative example 7
The compound hemostatic powder currently on the market was used as a control.
Hemostatic powder Performance test of examples and comparative examples
The hemostatic powder of the example and the comparative example is respectively added into purified water, and after the hemostatic powder is saturated by water absorption and swelling, the water absorption swelling ratio, the water absorption capacity, the water absorption rate for 3min, the average gel forming time and the hydrogel adhesiveness of the hemostatic powder are calculated by statistics.
A bleeding wound surface of 2.0X2.0 cm was formed on the leg of a small laboratory rabbit having a body weight of about 2kg, and the hemostatic powders of examples and comparative examples were applied to the bleeding wound surface, respectively, and the average hemostatic time was recorded.
The average clotting time was recorded by adding equal amounts of the hemostatic powders of examples and comparative examples to the blood of rabbits of the same concentration.
The performance of examples 1 to 3 and comparative examples 1 to 7 was tested and the results are shown in Table 1.
Table 1 performance test
From the results in Table 1, it is understood that the novel porous starch hemostatic powder of the present invention has excellent water absorption property, hydrogel property, hemostatic property and blood coagulation property, and has good stability, adhesiveness and blood-flushing resistance. As can be seen from the results of comparative examples 1 to 6, the components and steps of the present invention interact and coordinate to increase the efficacy, and any one of them is omitted. From the average hemostatic time, it was found that each of examples 1 to 3 can achieve effective hemostasis for about 30 seconds, each of comparative examples 1 to 6 can achieve effective hemostasis for about 60 seconds, and commercially available comparative example 7 requires about 180 seconds to achieve effective hemostasis. This fully demonstrates the excellent hemostatic properties of the novel porous starch hemostatic powder of the present invention. Similarly, comparative analysis resulted in other properties of the novel porous starch hemostatic powder of the present invention.
Meanwhile, in order to further illustrate the structural stability of the novel porous starch hemostatic powder, a scanning electron microscope test microstructure is also provided. From the results shown in fig. 1, the novel porous starch styptic powder has complete structure and high stability, and provides powerful guarantee for maintaining good original structure after a large amount of liquid is absorbed. Meanwhile, a large number of microporous structures with different apertures are formed on the surface of the microstructure, the pore-forming quality is high, the specific surface area is larger, and a good foundation is laid for improving the liquid absorbing capacity and the hemostatic capacity. In addition, nanometer calcium bentonite is embedded in the micropores, medical polyvinyl alcohol particles are embedded on the surfaces of the micropores, and when in liquid suction, the double structure can enable absorbed liquid to be locked in the micropores, so that the original structure is not lost due to the fact that the structure is washed away and collapsed after excessive liquid suction.
Therefore, the novel porous starch hemostatic powder prepared by the invention has excellent water absorption performance, hydrogel performance, hemostatic performance and blood coagulation performance, so that the novel porous starch hemostatic powder can be applied to the fields of hemostasis and blood coagulation.
It is to be understood that the foregoing description is only of the preferred embodiments of the invention, and is not intended to limit the scope of the invention, but is to be accorded the full scope of the principles, structures and structures disclosed herein.
Claims (10)
1. A novel porous starch hemostatic powder, which is characterized in that: the raw materials of the composite material comprise the following components in parts by weight: 80-100 parts of porous starch styptic powder, 1-5 parts of modified konjaku gum, 1-3 parts of poly L-lysine and 1-3 parts of modified collagen.
2. The novel porous starch styptic powder according to claim 1, wherein: the modified konjak gum is prepared by blending 10-15 parts of konjak gum, 1-2 parts of chitosan and 1-2 parts of sodium hyaluronate; the modified collagen is prepared by blending and modifying 10-15 parts of gelatin, 3-5 parts of silk fibroin, 1-3 parts of alginic acid, 2-4 parts of carboxymethyl cellulose and 1-2 parts of bioactive glass.
3. The method for preparing novel porous starch styptic powder according to claim 1, wherein: the method comprises the following steps:
s1, starch pretreatment
S11, ball milling treatment
Firstly, passing starch through a 200-target standard test sieve, and then, according to the starch: absolute ethyl alcohol: adding zirconia balls into a ball milling tank according to the weight ratio of 1:1:1, and fixing the ball milling tank on a planetary ball mill with the rotating speed of 300-500 r/min for ball milling for 30-60 min; finally taking out the mixture after ball milling, and placing the mixture in an oven at 40-60 ℃ for drying for 2 hours;
s12, emulsifying treatment
Firstly mixing the starch treated by the step S11 with pure water according to the weight ratio of 1:10-20, stirring magnetically for 2-4 h, then adjusting the pH to 9-10 by using sodium hydroxide solution, and continuing stirring for 1-2 h;
s2, ultrasonic acid enzyme modification treatment
S21, ultrasonic acid hydrolysis
Firstly mixing the starch suspension treated by the step S12 with an acidic solution, placing the mixture under the condition of 300-500W of power for ultrasonic treatment for 1-2 hours, and then regulating the pH value to 5-6 by using an inorganic salt solution;
s22, ultrasonic enzyme hydrolysis
(1) Firstly, placing acidolysis solution treated by S21 under the condition of 200-300W of power for ultrasonic treatment for 1-2 hours, then placing the acidolysis solution in a water bath kettle at 50-60 ℃ for preheating for 10-20 minutes, and finally adding alpha-amylase for enzymolysis;
(2) Placing the alpha-amylase enzymolysis liquid into a water bath kettle with the temperature of 40-60 ℃ for preheating for 20-30 min after ultrasonic treatment for 1-2 h under the power of 200-300W, and finally adding saccharifying enzyme for enzymolysis;
s3, modification treatment
S31, placing the enzyme solution treated in the S22 under an ultrasonic condition with the power of 300-500W, adding a pore-forming agent, and stirring to uniformly disperse the pore-forming agent in the enzymolysis solution to obtain a dispersion liquid;
s32, sequentially adding nano calcium bentonite and medical polyvinyl alcohol into the dispersion liquid treated in the step S31, and stirring and mixing to obtain a blend liquid;
s33, firstly adding 1-3% of hydrochloric acid or sulfuric acid and 60-70% of ethanol solution into the blending solution processed in the S32 to remove the pore-forming agent, wherein the addition amount of the blending solution is 0.1-0.5 wt%, and then carrying out centrifugal separation treatment on the blending solution, wherein the centrifugal speed is 3000-4000 rpm, the time is 20-30 min, and the steps are repeated for 3-5 times;
s34, washing the product treated in the step S33 for 3 times, drying at 60 ℃ for 6-8 hours, and finally crushing and sieving with a 200-target standard test sieve to obtain porous starch hemostatic powder;
s4, compounding treatment
S41, compounding porous starch hemostatic powder, modified konjac glucomannan, poly-L-lysine and modified collagen according to parts by weight;
s42, grinding, sieving, packaging and sterilizing the compound processed in the step S41.
4. The method for preparing novel porous starch styptic powder according to claim 3, wherein: in the step S11, the starch is prepared from tapioca starch: corn starch is 1:2-3 weight ratio.
5. The method for preparing novel porous starch styptic powder according to claim 3, wherein: in the step S12, the concentration of the starch emulsion is regulated to be 30-50%; the magnetic stirring speed is 300-500 rpm.
6. The method for preparing novel porous starch styptic powder according to claim 3, wherein: in the step S21, the starch suspension is mixed with an acid solution according to the following steps: the acid solution is 20-30: mixing at a volume ratio of 1; the acid solution is any one or combination of hydrochloric acid and sulfuric acid with the concentration of 1-4 mol/L; the inorganic salt solution is any one or a combination of more of sodium chloride, potassium chloride, calcium chloride, sodium carbonate and sodium bicarbonate with the concentration of 1-2 mol/L.
7. The method for preparing novel porous starch styptic powder according to claim 3, wherein: in the step S22, the addition amount of the alpha-amylase is 0.1-0.5 wt% of acidolysis solution, and enzymolysis is carried out for 2-6 h; the addition amount of the saccharifying enzyme is 0.4-0.8wt% of alpha-amylase enzymatic hydrolysate, and the enzymatic hydrolysis is carried out for 4-6 hours.
8. The method for preparing novel porous starch styptic powder according to claim 3, wherein: in the step S31, the addition amount of the pore-foaming agent is 0.05-0.1wt% of enzymolysis liquid; the pore-foaming agent is a mixed solution of hydrogen peroxide solution with the weight percent of 1-3 and sodium bicarbonate solution with the weight percent of 0.5-1; the volume ratio of the hydrogen peroxide solution to the sodium bicarbonate solution is 2:1.
9. The method for preparing novel porous starch styptic powder according to claim 3, wherein: in the step S32, the addition of the nano calcium bentonite and the medical polyvinyl alcohol is 1-3wt% of dispersion liquid, the particle size of the nano calcium bentonite is 10-50 nm, and the particle size of the medical polyvinyl alcohol is 1-3 mu m.
10. The novel porous starch styptic powder according to claims 1-9 can be applied in the field of hemostasis and coagulation.
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