CN105233326A - Preparation method and preparation of absorbable micropore vacuum polysaccharide particles - Google Patents
Preparation method and preparation of absorbable micropore vacuum polysaccharide particles Download PDFInfo
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Abstract
The invention discloses a preparation method and preparation of absorbable micropore vacuum polysaccharide particles. The preparation method comprises the steps that plant starch is added to an extrusion mechanism for extrusion and gelatinization, after soybean oil, span 80 and polysorbate 80 are added for emulsification, perforating, crosslinking and desolvation are carried out, pigments and pyrogen are removed, drying, screening, packaging and sterilization are carried out, and the micropore vacuum polysaccharide particles are obtained. Packaging is carried out under the aseptic conditions, and cobalt 60 is used for sterilization. Micropore vacuum polysaccharide particles of 20 micrometers and 50 micrometers are used for preparing external-use hemostasis medicine, and the micropore vacuum polysaccharide particles of 51 micrometers to 100 micrometers are used for preparing intraoperative hemostasis medicine. The absorbable micropore vacuum polysaccharide particles are free of toxins, stimulation, immunogenicity, apyrogeneity and mutagenesis effects, and can be degraded and absorbed by human tissue and body fluid. Metabolite is CO2 and H2O. The absorbable micropore vacuum polysaccharide particles are directly used for bleeding wound surfaces, have the advantages of being good in biocompatibility and water absorption performance, short in hemostasis time and the like, are completely absorbed within 72 hours, and are free of adhesion.
Description
Technical field
The present invention relates to field of medicaments, specifically a kind of preparation method of absorbable micropore vacuum polysaccharide particle sphere and purposes.
Background technology
At present, the hemostatic material on medical market is various in style, comprises traditional cotton prepared material, biological medical polymer material, synthetic protein dressing, mineral material, liquid type material, metal species dressing etc.Along with the high speed development of modern science and technology, the research of medical hemostatic dressing achieves progress quickly, and various Medical dressing continues to bring out, and performance is also more and more excellent.Natural activity high-molecular biologic hemostatic material is owing to having very high biological function and biocompatibility; at protection wound, accelerate, in wound healing, there is powerful advantage; therefore from the existing animal and plant of nature, the extensive concern that absorbable natural polymer hemostatic material causes various countries' medical circle and industrial circle is extracted in recent years; many large-scale medical companies are devoted to research and develop novel hemostatic material, but the bibliographical information extracting macromolecule polysaccharidase hemostatic material from natural plants potato starch is very few.The micropore polysaccharide hemostatic microsphere of domestic use, a kind of hemostatic material developed by Medafor company of the U.S., expensive, increase the weight of the financial burden of patient.Therefore, a kind of hemostasis of research rapidly, avirulence, no antigen, low price, the macromolecule polysaccharidase class hemostasia products with independent intellectual property right be domestic scholars must faced by problem.
Developed various new hemostatic material both at home and abroad, applying more general bleeding-stopping dressing has traditional gelfoam, alginate, collagen protein and the collagen-based composite recently occurred, chitosan and zeolite etc.Zoopery and clinical practice all achieve certain effect, but different hemostatic materials, have different clotting mechanisms, and all there is certain defect in above material.
Wherein the absorption rate of gelfoam is comparatively slow, and general needs more than 4 weeks, therefore can increase the infection risk of wound, affect wound healing.Collagen protein sponge is from the collagen extract of animal tissue, although it has excellent anthemorrhagic performance, is foreign protein eventually, easily occurs rejection, easily cause patient allergy to react, and causes infecting humanized and animality disease, as hepatitis etc.; Clinical signs is that patient allergy is reacted, wound healing is slow and wound easy infection complication, therefore Clinical practice is very limited.And albumin glue not easily stores and transports, use inconvenience etc.
The production development of natural biological polysaccharide is rapid, and its product mainly comprises the extract chitin, chitosan etc. of plant polysaccharide and Shrimp waste.It has excellent biocompatibility, nontoxic, nonirritant, not easily causes body anaphylaxis, can not cause simultaneously and infects or infect humanized and zoonosis, safe and reliable.But the general dissolubility of such material is poor, material is easily crisp, and mechanical strength is low, generally need add acid dissolve in the course of processing, acts on human body and easily causes side reaction, the side reaction such as easily cause surrounding tissue hyperemia, red and swollen phenomenon, shed tears.
The domestic bibliographical information had in polysaccharide hemostasis.Chitosan is made into powder by modified form and structural change by some documents, and add certain calcium again, zinc ion makes a kind of novel chitosan styptic powder, chitosan is not extract from plant amylum; The absorbability polysaccharide sthptic sponge that some Literature Discussions are made through special process by the plant polysaccharide of purification is on the impact of wound healing; Have document disclose a kind of with potato raw starch for raw material makes the method for polysaccharide styptic powder, i.e. expanded, hydrolysis, emulsifying, refine, dry, product becomes many micropores state; The medicinal ingredient of the hemostatic micro-granules that some documents relate to is the spheroidal particle of the surface band micropore that the micropore polysaccharide extracted from potato starch is formed after crosslinked, forms through gelatinizing, emulsifying and paraffin oil dispersion, epichlorohydrin cross-linked, ethyl acetate separatory, washes of absolute alcohol dehydration, oven drying.The polysaccharide styptic powder related to is for surface is with micropore, and inside is without the granule of vacuum, all different from of the present invention.
The one of external invention derives from plant amylum hemostatic material micropore polysaccharide hemostatic microsphere, it is a kind of absorbable hemostasia material (US Patent No. 6060461) for AristaTM of Medafor company of U.S. research and development in 2002,2006 by U.S. FDA certification, and its effective ingredient is micropore polysaccharide.When it acts on hemorrhage wound surface, the moisture in the rapid absorbing blood of micropore polysaccharide molecular energy, and effective ingredient in blood is assembled at particle surface, form gelatinous mixture, reach the effect of at once stopping blooding; The intrinsic coagulation factor is activated simultaneously, is partially formed sludged blood, can completes blood coagulation in tens of second.Because it is from plant amylum, can be monosaccharide by the amylase degrades in body fluid in human body, can digests and assimilates in vivo.This hemostasis is only physical process, not containing the disease that any animal is potential in material, without immunoreation, without anaphylaxis, without any side effects to wound healing, is a kind of outstanding topical hemostatic agent.But it be crack is not micropore that microstructure shows its microsphere surface, inside is also without vacuum, and when being applied to the hemorrhage wound surface hemostasis of large area soft tissue, because its adhesiveness, absorbency are strong not, haemostatic effect is restricted, and can be washed away when amount of bleeding is more by blood flow.The micropore vacuum polysaccharide microsphere absorbable hemostatic powder that the present invention relates to, for surface has micropore inside to be vacuum, is the hemostatic material that current uniquely energy and same kind of products at abroad compare favourably.
Summary of the invention
The object of the present invention is to provide preparation method and the purposes of a kind of good biocompatibility, good water absorption, bleeding stopping period short, absorbable micropore vacuum polysaccharide particle sphere, to solve the problem proposed in above-mentioned background technology.
For achieving the above object, the invention provides following technical scheme:
A preparation method for absorbable micropore vacuum polysaccharide particle sphere, comprises the following steps:
(1) expanded, gelatinizing: plant amylum is added in extruder, carry out expanded, gelatinizing process, in extrusion process, extruder extrusion friction produces heat, and pressure controls the condition of high temperature at 175 ~ 185 DEG C in 3 ~ 5MPa, temperature, and plant amylum is expanded.Plant amylum absorbs these heats and is subject to strong shearing, hydrogen bond rupture between strand, and strand is moved, and causes starch granules portion disintegrates, and gelatinizing occurs.Extruded by the aperture on extruder, the temperature of outlet controls, at 120 DEG C, then to take in drying containers.Namely spherex that is expanded, gelatinizing is obtained.After the method process, its gelatinization degree can reach more than 98%, and traditional heating gelatinization rate is only 80 ~ 85%, and easy to operate, equipment simple, be heated evenly, industrialization easily produces.
(2) emulsifying, perforation, crosslinked: to get soybean oil, sorbester p17 and Tween 80, mixing, in 60 ~ 80 DEG C of thermostat water baths, abundant stirring 30 ~ 60 minutes, wherein sorbester p17 and Tween 80 mass ratio are 0.8 ~ 1.2: 1, then be slowly injected in the spherex of expanded, gelatinizing, Keep agitation.Soybean oil is 5 ~ 10: 1 with the volume mass ratio of spherex, and the unit of volume mass ratio is ml/g, and the blended emulsifier of sorbester p17, Tween 80 composition and the mass ratio of spherex are 0.5 ~ 2: 1.By the spherex after emulsifying, be mixed with the emulsion that percentage by weight is 30 ~ 40%, then enzyme liquid puncture pore is added, in enzyme in enzyme liquid and emulsion, the mass ratio of spherex is 0.08 ~ 0.12: 1, temperature controls at 60 DEG C, and the pH value of solution maintains 4 ~ 6.5, reacts 24 hours, with the HCl solution of 0.5 ~ 1.0mol/L, the pH value of solution is adjusted to 4 ~ 5.5, obtains the spherical modified starch acid solution of micropore vacuum.Strengthen its structure with cross-linking agents process, strengthen porous microsphere mechanical strength, namely obtain the micropore vacuum starch milk white liquid of excellent performance, the mass ratio of cross-linking agent and the spherical modified starch acid solution of micropore vacuum is 1 ~ 2: 1.
(3) desolvation process: by above-mentioned product stratification, abandon the supernatant, take off a layer milky white liquid, add after ethyl acetate or petroleum ether fully stir, separatory, the quality adding ethyl acetate or petroleum ether is 10 times of lower floor's milky white liquid; Stratification again, takes off a layer milky white liquid, and add the washes of absolute alcohol of lower floor's milky white liquid 5 times of quality, then stir, then vacuum filtration is to moisture pump, obtains micropore vacuum modified starch particle sphere pressed powder.
(4) pigment and pyrogen is removed: pour in distilling flask by gained micropore vacuum modified starch particle sphere pressed powder again, be placed in magnetic stirring apparatus heating plate, add in the distilled water of 3 ~ 5 times, Keep agitation, stratification, abandon the supernatant, then by lower floor's milky white liquid repeated washing 3 ~ 5 times.In the white emulsion after washing, add distilled water again dissolve, by micropore vacuum modified starch particle sphere pressed powder: active carbon=1: the mass ratio of 5 adds active carbon, to remove pigment and pyrogen.After 10 ~ 12h, with the filter element filtering of 5 ~ 20 μm, remove active carbon.Obtain micropore vacuum polysaccharide particle sphere emulsion.
(5) dry, screening, packaging, sterilizing: the micropore vacuum polysaccharide particle sphere emulsion of above-mentioned gained is carried out spraying dry at 120 DEG C, sieve through 20 μm of micro-meshes with 100 μm, obtain the micropore vacuum polysaccharide particle sphere of 20 ~ 100 μm.Aseptically pack, then use Co 60 sterilizing.
As the further scheme of the present invention: the middle pressure of starch in extrusion process of step (1) is 4MPa, temperature is 180 DEG C.
As the further scheme of the present invention: enzyme is perforation agent.
As the further scheme of the present invention: cross-linking agent is sodium trimetaphosphate.
As the further scheme of the present invention: sorbester p17 and Tween 80 mass ratio are 1: 1.
As the further scheme of the present invention: in the enzyme in enzyme liquid and emulsion, the mass ratio of spherex is 0.1: 1.
As the further scheme of the present invention: the granularity of active carbon is 20 ~ 40 orders.
As the further scheme of the present invention: again sieve with the micro-mesh of 50 μm in step (5), obtain the micropore vacuum polysaccharide particle sphere of 20 ~ 50 μm, 51 ~ 100 μm two kinds of specifications, and the micropore vacuum polysaccharide particle sphere uniformity coefficient of two kinds of specifications reaches more than 95%.
As the further scheme of the present invention: plant amylum adopts one or more the mixture in potato starch, wheaten starch, sweet potato starch, tapioca, corn starch.
Described absorbable micropore vacuum polysaccharide particle sphere is for the preparation of haemostatic medicament.
Main uses of the present invention: 1. save oneself in war wound, wound scene; Save oneself in the scene of 2. flood-fighting, earthquake relief work and fire fighter's wound hemorrhage; 3. on emergency tender, in first-aid kit and for subsequent use in family; 4. stop blooding in various surgical operation art; 5. the micropore vacuum polysaccharide particle sphere of 20 ~ 50 μm is for the preparation of hemostatic for external use thing, and the micropore vacuum polysaccharide particle sphere of 51 ~ 100 μm is for the preparation of haemostatic medicament in art.
Compared with prior art, the invention has the beneficial effects as follows:
The preparation method of a kind of absorbable micropore vacuum polysaccharide particle sphere that the present invention relates to and purposes.Micropore vacuum polysaccharide particle sphere is from potato plants starch, extract the spherical white particle powder of micropore vacuum polysaccharide, and there is micropore on surface, and inside is vacuum, and stereoeffect is netted.The diameter of micropore vacuum polysaccharide particle sphere is 20 ~ 100 μm, and molecular weight is 30000 ~ 100000, and water absorbent rate is 100 ~ 150 times, and bleeding stopping period is 5 ~ 20s.Have avirulence, nonirritant, without immunogenicity, apyrogenetity, without mutagenic effect, can be absorbed by tissue, degraded by body fluid, metabolite is CO
2and H
2o.Directly apply to hemorrhage wound surface, there is the features such as good biocompatibility, good water absorption, bleeding stopping period be short, within 72 hours, be completely absorbed, the phenomenon of adhesion can not be produced.Because micropore vacuum polysaccharide particle sphere derives from plant amylum, particularly potato starch, not containing any animal derived, humanized's albumen, without immunoreation, without anaphylaxis, be a kind of novel desirable hemostatic material.
Detailed description of the invention
Below in conjunction with the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, a kind of preparation method of absorbable micropore vacuum polysaccharide particle sphere, comprises the following steps:
(1) expanded, gelatinizing: added by potato starch in extruder, carries out expanded, gelatinizing process, and in extrusion process, extruder extrusion friction produces heat, and pressure controls the condition of high temperature at 175 DEG C in 3MPa, temperature, starch swelling.Starch absorbs these heats and is subject to strong shearing, hydrogen bond rupture between strand, and strand is moved, and causes starch granules portion disintegrates, and gelatinizing occurs.Extruded by the aperture on extruder, the temperature of outlet controls, at 120 DEG C, then to take in drying containers.Namely spherex that is expanded, gelatinizing is obtained.After the method process, its gelatinization degree can reach more than 98%, and traditional heating gelatinization rate is only 80 ~ 85%, and easy to operate, equipment simple, be heated evenly, industrialization easily produces.
(2) emulsifying, perforation, crosslinked: get soybean oil, sorbester p17 and Tween 80, mixing, in 60 DEG C of thermostat water baths, abundant stirring 30 minutes, wherein sorbester p17 and Tween 80 mass ratio are 0.8: 1, are then slowly injected in the spherex of expanded, gelatinizing, Keep agitation.Soybean oil is 5: 1 with the volume mass ratio of spherex, and the unit of volume mass ratio is ml/g, and the blended emulsifier of sorbester p17, Tween 80 composition and the mass ratio of spherex are 0.5: 1.By the spherex after emulsifying, be mixed with the emulsion that percentage by weight is 30%, then enzyme liquid puncture pore is added, in enzyme in enzyme liquid and emulsion, the mass ratio of spherex is 0.08: 1, temperature controls at 60 DEG C, and the pH value of solution maintains 6.5, reacts 24 hours, with the HCl solution of 0.5mol/L, the pH value of solution is adjusted to 4, obtains the spherical modified starch acid solution of micropore vacuum.Strengthen its structure by sodium trimetaphosphate crosslinking Treatment, strengthen porous microsphere mechanical strength, namely obtain the micropore vacuum starch milk white liquid of excellent performance, the mass ratio of sodium trimetaphosphate and the spherical modified starch acid solution of micropore vacuum is 1: 1.
(3) desolvation process: by above-mentioned product stratification, abandon the supernatant, take off a layer milky white liquid, add after ethyl acetate or petroleum ether fully stir, separatory, the quality adding ethyl acetate or petroleum ether is 10 times of lower floor's milky white liquid; Stratification again, takes off a layer milky white liquid, and add the washes of absolute alcohol of lower floor's milky white liquid 5 times of quality, then stir, then vacuum filtration is to moisture pump, obtains micropore vacuum modified starch particle sphere pressed powder.
(4) pigment and pyrogen is removed: pour in distilling flask by gained micropore vacuum modified starch particle sphere pressed powder again, be placed in magnetic stirring apparatus heating plate, add in the distilled water of 3 times, Keep agitation, stratification, abandon the supernatant, then by lower floor's milky white liquid repeated washing 3 times.In the white emulsion after washing, add distilled water again dissolve, by micropore vacuum modified starch particle sphere pressed powder: active carbon=1: the mass ratio of 5 adds active carbon, to remove pigment and pyrogen.After 10h, with the filter element filtering of 5 ~ 20 μm, remove active carbon.Obtain micropore vacuum polysaccharide particle sphere emulsion.
(5) dry, screening, packaging, sterilizing: the micropore vacuum polysaccharide particle sphere emulsion of above-mentioned gained is carried out spraying dry at 120 DEG C, sieve through 20 μm of micro-meshes with 100 μm, obtain the micropore vacuum polysaccharide particle sphere of 20 ~ 100 μm.Aseptically pack, then use Co 60 sterilizing.The particle diameter of the micropore vacuum polysaccharide particle sphere of preparation is 20 ~ 100 μm; There is micropore on surface, inside is vacuum, and stereoeffect is netted.
Embodiment 2
In the embodiment of the present invention, a kind of preparation method of absorbable micropore vacuum polysaccharide particle sphere, comprises the following steps:
(1) expanded, gelatinizing: added by potato starch in extruder, carries out expanded, gelatinizing process, and in extrusion process, extruder extrusion friction produces heat, and pressure controls the condition of high temperature at 185 DEG C in 5MPa, temperature, starch swelling.Starch absorbs these heats and is subject to strong shearing, hydrogen bond rupture between strand, and strand is moved, and causes starch granules portion disintegrates, and gelatinizing occurs.Extruded by the aperture on extruder, the temperature of outlet controls, at 120 DEG C, then to take in drying containers.Namely spherex that is expanded, gelatinizing is obtained.After the method process, its gelatinization degree can reach more than 98%, and traditional heating gelatinization rate is only 80 ~ 85%, and easy to operate, equipment simple, be heated evenly, industrialization easily produces.
(2) emulsifying, perforation, crosslinked: get soybean oil, sorbester p17 and Tween 80, mixing, in 80 DEG C of thermostat water baths, abundant stirring 60 minutes, wherein sorbester p17 and Tween 80 mass ratio are 1.2: 1, are then slowly injected in the spherex of expanded, gelatinizing, Keep agitation.Soybean oil is 10: 1 with the volume mass ratio of spherex, and the unit of volume mass ratio is ml/g, and the blended emulsifier of sorbester p17, Tween 80 composition and the mass ratio of spherex are 2: 1.By the spherex after emulsifying, be mixed with the emulsion that percentage by weight is 40%, then enzyme liquid puncture pore is added, in enzyme in enzyme liquid and emulsion, the mass ratio of spherex is 0.12: 1, temperature controls at 60 DEG C, and the pH value of solution maintains 5.5, reacts 24 hours, with the HCl solution of 1.0mol/L, the pH value of solution is adjusted to 4.3, obtains the spherical modified starch acid solution of micropore vacuum.Strengthen its structure by sodium trimetaphosphate crosslinking Treatment, strengthen porous microsphere mechanical strength, namely obtain the micropore vacuum starch milk white liquid of excellent performance, the mass ratio of sodium trimetaphosphate and the spherical modified starch acid solution of micropore vacuum is 2: 1.
(3) desolvation process: by above-mentioned product stratification, abandon the supernatant, take off a layer milky white liquid, add after ethyl acetate or petroleum ether fully stir, separatory, the quality adding ethyl acetate or petroleum ether is 10 times of lower floor's milky white liquid; Stratification again, takes off a layer milky white liquid, and add the washes of absolute alcohol of lower floor's milky white liquid 5 times of quality, then stir, then vacuum filtration is to moisture pump, obtains micropore vacuum modified starch particle sphere pressed powder.
(4) pigment and pyrogen is removed: pour in distilling flask by gained micropore vacuum modified starch particle sphere pressed powder again, be placed in magnetic stirring apparatus heating plate, add in the distilled water of 5 times, Keep agitation, stratification, abandon the supernatant, then by lower floor's milky white liquid repeated washing 5 times.In the white emulsion after washing, add distilled water again dissolve, by micropore vacuum modified starch particle sphere pressed powder: active carbon=1: the mass ratio of 5 adds active carbon, to remove pigment and pyrogen.After 12h, with the filter element filtering of 5 ~ 20 μm, remove active carbon.Obtain micropore vacuum polysaccharide particle sphere emulsion.
(5) dry, screening, packaging, sterilizing: the micropore vacuum polysaccharide particle sphere emulsion of above-mentioned gained is carried out spraying dry at 120 DEG C, sieve through 20 μm of micro-meshes with 100 μm, obtain the micropore vacuum polysaccharide particle sphere of 20 ~ 100 μm.Aseptically pack, then use Co 60 sterilizing.The particle diameter of the micropore vacuum polysaccharide particle sphere of preparation is 20 ~ 100 μm; There is micropore on surface, inside is vacuum, and stereoeffect is netted.
Embodiment 3
In the embodiment of the present invention, a kind of preparation method of absorbable micropore vacuum polysaccharide particle sphere, comprises the following steps:
(1) expanded, gelatinizing: added by potato starch in extruder, carries out expanded, gelatinizing process, and in extrusion process, extruder extrusion friction produces heat, and pressure controls the condition of high temperature at 180 DEG C in 4MPa, temperature, starch swelling.Starch absorbs these heats and is subject to strong shearing, hydrogen bond rupture between strand, and strand is moved, and causes starch granules portion disintegrates, and gelatinizing occurs.Extruded by the aperture on extruder, the temperature of outlet controls, at 120 DEG C, then to take in drying containers.Namely spherex that is expanded, gelatinizing is obtained.After the method process, its gelatinization degree can reach more than 98%, and traditional heating gelatinization rate is only 80 ~ 85%, and easy to operate, equipment simple, be heated evenly, industrialization easily produces.
(2) emulsifying, perforation, crosslinked: get soybean oil, sorbester p17 and Tween 80, mixing, in 70 DEG C of thermostat water baths, abundant stirring 45 minutes, wherein sorbester p17 and Tween 80 mass ratio are 1: 1, are then slowly injected in the spherex of expanded, gelatinizing, Keep agitation.Soybean oil is 7.5: 1 with the volume mass ratio of spherex, and the unit of volume mass ratio is ml/g, and the blended emulsifier of sorbester p17, Tween 80 composition and the mass ratio of spherex are 1: 1.By the spherex after emulsifying, be mixed with the emulsion that percentage by weight is 35%, then enzyme liquid puncture pore is added, in enzyme in enzyme liquid and emulsion, the mass ratio of spherex is 0.1: 1, temperature controls at 60 DEG C, and the pH value of solution maintains 5, reacts 24 hours, with the HCl solution of 0.7mol/L, the pH value of solution is adjusted to 4.1, obtains the spherical modified starch acid solution of micropore vacuum.Strengthen its structure by sodium trimetaphosphate crosslinking Treatment, strengthen porous microsphere mechanical strength, namely obtain the micropore vacuum starch milk white liquid of excellent performance, the mass ratio of sodium trimetaphosphate and the spherical modified starch acid solution of micropore vacuum is 1.5: 1.
(3) desolvation process: by above-mentioned product stratification, abandon the supernatant, take off a layer milky white liquid, add after ethyl acetate or petroleum ether fully stir, separatory, the quality adding ethyl acetate or petroleum ether is 10 times of lower floor's milky white liquid; Stratification again, takes off a layer milky white liquid, and add the washes of absolute alcohol of lower floor's milky white liquid 5 times of quality, then stir, then vacuum filtration is to moisture pump, obtains micropore vacuum modified starch particle sphere pressed powder.
(4) pigment and pyrogen is removed: pour in distilling flask by gained micropore vacuum modified starch particle sphere pressed powder again, be placed in magnetic stirring apparatus heating plate, add in the distilled water of 4 times, Keep agitation, stratification, abandon the supernatant, then by lower floor's milky white liquid repeated washing 4 times.In the white emulsion after washing, add distilled water again dissolve, by micropore vacuum modified starch particle sphere pressed powder: active carbon=1: the mass ratio of 5 adds active carbon, to remove pigment and pyrogen.After 11h, with the filter element filtering of 5 ~ 20 μm, remove active carbon.Obtain micropore vacuum polysaccharide particle sphere emulsion.
(5) dry, screening, packaging, sterilizing: the micropore vacuum polysaccharide particle sphere emulsion of above-mentioned gained is carried out spraying dry at 120 DEG C, sieve through 20 μm of micro-meshes with 100 μm, obtain the micropore vacuum polysaccharide particle sphere of 20 ~ 100 μm.Aseptically pack, then use Co 60 sterilizing.The particle diameter of the micropore vacuum polysaccharide particle sphere of preparation is 20 ~ 100 μm; There is micropore on surface, inside is vacuum, and stereoeffect is netted.
Main uses of the present invention: saving oneself in the scene being 1. adapted to the army military training wound hemorrhage wounded, saves oneself in the scene of the hemorrhage wounded of Battlefield trauma injuries, save oneself in the scene of flood-fighting, earthquake relief work and fire fighter's wound hemorrhage, on emergency tender, in first-aid kit and for subsequent use in family; 2. stop blooding in various surgical operation art.During use, hemorrhage wound surface is without any need for process, to be sprayed directly on by hemostatic micro-granules ball on hemorrhage wound surface and it to be covered completely.This hemostatic micro-granules ball is not by the restriction of wound surface size, shape and the depth, easy to use, and hemostasis rapidly.3. 20 ~ 50 μm of micropore vacuum poly particle spheres are used for external hemostasis, and 51 ~ 100 μm of micropore vacuum polysaccharide particle sphere Rhizoma Atractylodis Macrocephalae stop blood.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or basic feature, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.
In addition, be to be understood that, although this description is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of description is only for clarity sake, those skilled in the art should by description integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (10)
1. a preparation method for absorbable micropore vacuum polysaccharide particle sphere, is characterized in that, comprise the following steps:
(1) expanded, gelatinizing: plant amylum is added in extruder, carry out expanded, gelatinizing process, in extrusion process, extruder extrusion friction produces heat, and pressure controls under the state of 175 ~ 185 DEG C in 3 ~ 5MPa, temperature, and plant amylum is expanded, gelatinizing; Extruded by the aperture on extruder, the temperature of outlet controls, at 120 DEG C, then to take in drying containers; Namely spherex that is expanded, gelatinizing is obtained;
(2) emulsifying, perforation, crosslinked: to get soybean oil, sorbester p17 and Tween 80, mixing, in 60 ~ 80 DEG C of thermostat water baths, abundant stirring 30 ~ 60 minutes, wherein sorbester p17 and Tween 80 mass ratio are 0.8 ~ 1.2: 1, then be slowly injected in the spherex of expanded, gelatinizing, Keep agitation; Soybean oil is 5 ~ 10: 1 with the volume mass ratio of spherex, and the unit of volume mass ratio is ml/g, and the blended emulsifier of sorbester p17, Tween 80 composition and the mass ratio of spherex are 0.5 ~ 2: 1; By the spherex after emulsifying, be mixed with the emulsion that percentage by weight is 30 ~ 40%, then enzyme liquid puncture pore is added, in enzyme in enzyme liquid and emulsion, the mass ratio of spherex is 0.08 ~ 0.12: 1, temperature controls at 60 DEG C, and the pH value of solution maintains 4 ~ 6.5, reacts 24 hours, with the HCl solution of 0.5 ~ 1.0mol/L, the pH value of solution is adjusted to 4 ~ 5.5, obtains the spherical modified starch acid solution of micropore vacuum; Use cross-linking agents process, namely obtain micropore vacuum starch milk white liquid, the mass ratio of cross-linking agent and the spherical modified starch acid solution of micropore vacuum is 1 ~ 2: 1;
(3) desolvation process: by above-mentioned micropore vacuum starch milk white liquid stratification, abandon the supernatant, take off a layer milky white liquid, add after ethyl acetate or petroleum ether fully stir, separatory, the quality adding ethyl acetate or petroleum ether is 10 times of lower floor's milky white liquid; Stratification again, takes off a layer milky white liquid, and add the washes of absolute alcohol of lower floor's milky white liquid 5 times of quality, then stir, then vacuum filtration is to moisture pump, obtains micropore vacuum modified starch particle sphere pressed powder;
(4) pigment and pyrogen is removed: pour in distilling flask by gained micropore vacuum modified starch particle sphere pressed powder again, be placed in magnetic stirring apparatus heating plate, add in the distilled water of 3 ~ 5 times, Keep agitation, stratification, abandon the supernatant, then by lower floor's milky white liquid repeated washing 3 ~ 5 times; In the white emulsion after washing, add distilled water again dissolve, by micropore vacuum modified starch particle sphere pressed powder: active carbon=1: the mass ratio of 5 adds active carbon, to remove pigment and pyrogen; After 10 ~ 12h, with the filter element filtering of 5 ~ 20 μm, remove active carbon; Obtain micropore vacuum polysaccharide particle sphere emulsion;
(5) dry, screening, packaging, sterilizing: the micropore vacuum polysaccharide particle sphere emulsion of above-mentioned gained is carried out spraying dry at 120 DEG C, sieve through 20 μm of micro-meshes with 100 μm, obtain the micropore vacuum polysaccharide particle sphere of 20 ~ 100 μm; Aseptically pack, then use Co 60 sterilizing.
2. the preparation method of absorbable micropore vacuum polysaccharide particle sphere according to claim 1, is characterized in that, the middle pressure of starch in extrusion process of step (1) is 4MPa, temperature is 180 DEG C.
3. the preparation method of absorbable micropore vacuum polysaccharide particle sphere according to claim 1, is characterized in that, enzyme is perforation agent, and in the enzyme in enzyme liquid and emulsion, the mass ratio of spherex is 0.1: 1.
4. the preparation method of absorbable micropore vacuum polysaccharide particle sphere according to claim 1, it is characterized in that, cross-linking agent is sodium trimetaphosphate.
5. the preparation method of absorbable micropore vacuum polysaccharide particle sphere according to claim 1, it is characterized in that, sorbester p17 and Tween 80 mass ratio are 1: 1.
6. the preparation method of absorbable micropore vacuum polysaccharide particle sphere according to claim 1, it is characterized in that, plant amylum adopts one or more the mixture in potato starch, wheaten starch, sweet potato starch, tapioca, corn starch.
7. the preparation method of absorbable micropore vacuum polysaccharide particle sphere according to claim 1, it is characterized in that, the granularity of active carbon is 20 ~ 40 orders.
8. the preparation method of absorbable micropore vacuum polysaccharide particle sphere according to claim 1, it is characterized in that, again sieve with the micro-mesh of 50 μm in step (5), obtain the micropore vacuum polysaccharide particle sphere of 20 ~ 50 μm, 51 ~ 100 μm two kinds of specifications.
9., according to the purposes of the arbitrary described absorbable micropore vacuum polysaccharide particle sphere of claim 1-8, it is characterized in that, for the preparation of haemostatic medicament.
10. the purposes of absorbable micropore vacuum polysaccharide particle sphere according to claim 9, it is characterized in that, the micropore vacuum polysaccharide particle sphere of 20 ~ 50 μm is for the preparation of hemostatic for external use thing, and the micropore vacuum polysaccharide particle sphere of 51 ~ 100 μm is for the preparation of haemostatic medicament in art.
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| CN107456579A (en) * | 2016-12-20 | 2017-12-12 | 史跃 | A kind of preparation method of micropore polysaccharide drug bearing microsphere |
| CN109908396A (en) * | 2019-01-08 | 2019-06-21 | 中国人民解放军军事科学院军事医学研究院 | A kind of calcium ion-exchanged porous-starch hemostatic material and its preparation method and application |
| CN113974126A (en) * | 2021-11-05 | 2022-01-28 | 山东岱岳制盐有限公司 | Preparation method of zinc-rich refined salt |
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| CN107456579A (en) * | 2016-12-20 | 2017-12-12 | 史跃 | A kind of preparation method of micropore polysaccharide drug bearing microsphere |
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| CN113974126B (en) * | 2021-11-05 | 2023-12-22 | 山东岱岳制盐有限公司 | Preparation method of zinc-rich refined salt |
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