CN107198791A - The method that electrostatic spraying prepares cross linked porous starch hemostatic microsphere - Google Patents
The method that electrostatic spraying prepares cross linked porous starch hemostatic microsphere Download PDFInfo
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- CN107198791A CN107198791A CN201710376254.7A CN201710376254A CN107198791A CN 107198791 A CN107198791 A CN 107198791A CN 201710376254 A CN201710376254 A CN 201710376254A CN 107198791 A CN107198791 A CN 107198791A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/001—Use of materials characterised by their function or physical properties
- A61L24/0036—Porous materials, e.g. foams or sponges
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/001—Use of materials characterised by their function or physical properties
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/001—Use of materials characterised by their function or physical properties
- A61L24/0015—Medicaments; Biocides
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/04—Surgical adhesives or cements; Adhesives for colostomy devices containing macromolecular materials
- A61L24/08—Polysaccharides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/20—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
- A61L2300/23—Carbohydrates
- A61L2300/232—Monosaccharides, disaccharides, polysaccharides, lipopolysaccharides
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/418—Agents promoting blood coagulation, blood-clotting agents, embolising agents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2303/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2303/02—Starch; Degradation products thereof, e.g. dextrin
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Surgery (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Medicinal Preparation (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention provides a kind of method that electrostatic spraying prepares cross linked porous starch hemostatic microsphere, it comprises the following steps：Amidin is sprayed in solidification liquid by the method for electrostatic spraying, solidification regeneration shaping is carried out, by supercritical CO2It is dried to obtain the cross linked porous spherex；Wherein, the voltage of the electrostatic spraying is 3~20kV, includes sodium hydroxide in the amidin, and the mass fraction of starch and sodium hydroxide is respectively 5~20% and 2~3%；Microsphere diameter is 100~800 microns, and microsphere surface is dense layer surface (thickness is about 0.1~0.5 μm), internal to contain the abundant hole that size is 2~3 μm, specific surface area (1~50m of microballoon2/g).The present invention has the advantages that：Crosslinked starch porous microsphere can be easily prepared, simple to operate, condition is easily controllable, granular size is more uniform；Obtained crosslinked starch porous microsphere, porosity is high, and specific surface area is big, and coagulating effectiveness can be produced rapidly as styptic.
Description
Technical field
The present invention relates to a kind of method that electrostatic spraying prepares cross linked porous starch hemostatic microsphere, belong to natural polymer material
Expect technical field.
Background technology
Starch is a kind of polysaccharide that nature is widely present, and is exactly the main component of human food since ancient times.In the energy
Today that in short supply, environment goes from bad to worse, starch has very important strategic position and huge for saving the energy, environmental protection etc.
Big potentiality to be exploited.Spherex is as a kind of Biodegradable material, with degradation speed controllability, biocompatibility, nothing
The features such as between poison, non-immunogenicity and bin stability and medicine mutually without influence, spherex has as pharmaceutical carrier
Absorbed, target by cell through tissue space, being sustained, efficiently, multipath is the advantages of be administered, in adsorbent, styptic, medicine
Extensive use in terms of carrier and embedding medium.
The preparation method of current spherex mainly has：Physical, chemical method, enzymatic isolation method, reverse microemulsion method etc..Physics
Method be under mechanical force by starch crush be microballoon, thus obtained microsphere particle diameter is big, particle diameter distribution is uneven.Chemical method is starch
Hydrolysis obtains microballoon in acid condition, and the method hydrolysis time length, side reaction is more, product yield is low and microballoon one-tenth porosity is low.Enzyme
Solution is ative starch under glucoamylase and alpha-amylase effect hydrolysis obtains porous-starch microballoon, the method influence factor compared with
It is many, such as：PH value and ative starch granular size can influence the aperture density and depth of microballoon, so as to be caused to sustained drug release effect
Influence.Inverted emulsion method is that starch forms water-in-oil emulsion under emulsifying agent effect, and crosslinking obtains spherex, party's legal system
The toxic solvents such as the toluene and benzotrichloride that are used during standby can be polluted the biological nature of starch.
The content of the invention
The present invention is directed to the deficiency of prior art, it is proposed that a kind of simple to operate, condition is easily controllable, uniform particle sizes friendships
Join the preparation method of starch porous microsphere.
The present invention is achieved by the following technical solutions：
The invention provides a kind of method that electrostatic spraying prepares cross linked porous spherex, it comprises the following steps：
Amidin is sprayed in solidification liquid by the method for electrostatic spraying, solidification regeneration shaping is carried out, through overdrying
It is dry to obtain the cross linked porous spherex；Wherein, the voltage of the electrostatic spraying is 3~20kV, in the amidin
Include sodium hydroxide, and the mass fraction of starch and sodium hydroxide is respectively 5~20% and 2~3%.
Because starch solution relatively glues, strand highly tangles, and voltage can not overcome the surface of starch solution when being less than 3kV
Power and viscoelastic power, it is impossible to obtain size for micron and following microballoon；Electrostatic spraying is readily obtained fiber when voltage is higher than 20kV
Shape material.If starch concentration is higher than the scope, solution viscosity is too big, it is impossible to EFI；The concentration of sodium hydroxide is less than described
Scope, then can not be completely dissolved starch；Starch concentration is less than the scope, or the concentration of sodium hydroxide is higher than the model
Enclose, then EFI is unstable, microballoon size pattern is uneven.
Preferably, the amidin is in the sodium hydrate aqueous solution that pH value is 10~13 by starch dissolution
In be prepared from.
Preferably, also include in the amidin in water soluble surfactant active and water-soluble polymer
One or two.
Preferably, the solidification liquid be sodium metaphosphate, calcium chloride, water, ethanol and epoxychloropropane mixing it is molten
Liquid, wherein, sodium metaphosphate and calcium chloride are in terms of mass parts, and water, ethanol and epoxychloropropane are in terms of parts by volume, sodium metaphosphate, chlorine
It is (1~3) to change calcium, epoxychloropropane, water, the ratio of ethanol:(1~7):(1~7)：(20~80):(20~80).
The proportioning of solidification liquid each component is in order that the starch drop quick solidification that EFI enters solidification liquid is molded.Deviate suitable
When proportioning will influence formation and the performance of microballoon.
Preferably, the feeding rate of the electrostatic spraying is 1~80 μ L/min.
, can be with the size of Effective Regulation microballoon by adjusting feeding rate.Feeding speed is excessive easily to make obtained microballoon
Excessive and cause haemostatic effect poor, feeding speed is too small, and the efficiency reduction and energy expenditure that can make to prepare microballoon are more, cost
Increase.
Preferably, the method for the drying is supercritical carbon dioxide seasoning.
A kind of purposes such as the cross linked porous spherex of preceding method preparation in hemostatic material.
Compared with prior art, the present invention has following beneficial effect：
1st, crosslinked starch porous microsphere can be easily prepared, simple to operate, condition is easily controllable, granular size is more equal
It is even.
2nd, crosslinked starch porous microsphere made from the above method of the present invention, porosity is up to 80%, and specific surface area is up to
50m2/ g, coagulating effectiveness can be produced rapidly as styptic, as little as 50s of external clotting time.
Brief description of the drawings
By reading the detailed description made with reference to the following drawings to non-limiting example, further feature of the invention,
Objects and advantages will become more apparent upon：
Fig. 1 (amplifies 50 for the surface topography scanning electron microscope (SEM) photograph of crosslinked starch porous microsphere made from embodiments of the invention 1
Times)；
Fig. 2 (amplifies for the surface topography scanning electron microscope (SEM) photograph of crosslinked starch porous microsphere made from embodiments of the invention 1
500 times)；
Fig. 3 is the scanning electron microscope (SEM) photograph of crosslinked starch porous microsphere internal structure made from embodiments of the invention 1；
Fig. 4 is the external procoagulant activity figure of crosslinked starch porous microsphere made from embodiments of the invention 3.
Embodiment
Embodiment 1
2.4g starch dissolutions are taken in 20ml, 2% sodium hydrate aqueous solution, with 80 μ in 14.00kV high-voltage electrostatic fields
L/min flow velocity is sprayed in coagulating bath, and the composition of coagulating bath is：Water 96ml, ethanol 96ml, epoxychloropropane 8ml, calcium chloride
6g, sodium trimetaphosphate 2g, magnetic agitation 4h wash drying, obtain the cross linked porous spherexs of 2.82g, as shown in Figure 1,2 and 3.
Fig. 1 scanning electron microscope (SEM) photographs show that cross linked porous starch hemostatic microsphere outward appearance is in cobblestone-appearance, and surface compact is smooth；Fig. 2
It is core shell structure to show the microballoon；Fig. 3 is then the internal structure of microballoon, shows three-dimensional netted honeycomb.Therefore it is described micro-
Ball is the structure with the porous core of fine and close shell.
Embodiment 2
2.4g starch is taken, the surfactant 0.1g of Tween 80 are dissolved in 20ml, 2% sodium hydrate aqueous solution,
Sprayed in 14.00kV high-voltage electrostatic fields with 80 μ l/min flow velocity in coagulating bath, the composition of coagulating bath is：Water 96ml, ethanol
96ml, epoxychloropropane 8ml, calcium chloride 6g, sodium trimetaphosphate 2g, magnetic agitation 4h wash drying, obtain the porous friendships of 2.32g
Join spherex.
Embodiment 3
2.4g starch, sodium alginate 2g, and gelatin 1g is taken to be dissolved in 20ml, 2% sodium hydrate aqueous solution,
Sprayed in 14.00kV high-voltage electrostatic fields with 15 μ l/min flow velocity in coagulating bath, the composition of coagulating bath is：Water 96ml, ethanol
96ml, epoxychloropropane 8ml, calcium chloride 6g, sodium trimetaphosphate 1g, magnetic agitation 4h wash drying, obtain 2.54g starch-sea
Calcium alginate-gelatin cross-blend porous microsphere.
Embodiment 4
1.4g starch dissolutions are taken in 20ml, 3.0% sodium hydrate aqueous solution, with 35 in 8.00kV high-voltage electrostatic fields
μ l/min flow velocity is sprayed in coagulating bath, and the composition of coagulating bath is：Water 90ml, ethanol 98ml, epoxychloropropane 12ml, chlorination
Calcium 1g, sodium trimetaphosphate 1g, magnetic agitation 2.5h wash drying, obtain the cross linked porous spherexs of 1.55g.
Embodiment 5
3.0g starch and gelatin 0.5g are taken, is dissolved in 20ml, 2.5% sodium hydrate aqueous solution, in 12.00kV high pressures
Sprayed in electrostatic field with 80 μ l/min flow velocity in coagulating bath, the composition of coagulating bath is：Water 95ml, alcohol 95 ml, epoxy chlorine
Propane 10ml, calcium chloride 8g, sodium trimetaphosphate 0.5g, magnetic agitation 4h wash drying, obtain 2.87g starch-gelatins porous micro-
Ball.
Embodiment 6
Porous-starch hemostatic microsphere made from 10mg starch granules and above-described embodiment is taken respectively in 2ml disposable plastic
Guan Zhong, draws 1ml, 37 DEG C of anticoagulated bloods and is added thereto, then adds into blood 100 μ l, 0.1M CaCl2Start meter after solution
When, often cross 10s and tilt plastic tube once, timing, gained time are stopped when plastic tube is tilted into 90 ° of blood not in flowing
As the clotting time, each sample, which is repeated 5 times, takes its average value.External rush blood coagulation figure is as shown in Figure 4.Data are listed in table 1.
The physical property and external clotting time of the starch granules of table 1 and spherex
The as shown by data of table 1 is compared with dense non-porous starch granules, the external blood coagulation of starch porous microsphere prepared by the present invention
Time substantially shortens, and is only its 30~60%.Consider biocompatibility, the absorption of human body of starch, porous-starch is micro-
Spherical shell turns into safe and efficient hemostatic material.
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (6)
1. a kind of method that electrostatic spraying prepares cross linked porous starch hemostatic microsphere, it is characterised in that comprise the following steps：
Amidin is sprayed in solidification liquid by the method for electrostatic spraying, solidification regeneration shaping is carried out, by overcritical
CO2It is dried to obtain the cross linked porous spherex；Wherein, the voltage of the electrostatic spraying is 3~20kV, and the starch is water-soluble
Include sodium hydroxide in liquid, and the mass fraction of starch and sodium hydroxide is respectively 5~20% and 2~3%.
2. the method that electrostatic spraying as claimed in claim 1 prepares cross linked porous starch hemostatic microsphere, it is characterised in that described
Solidification liquid is the mixed solution of sodium metaphosphate, calcium chloride, water, ethanol and epoxychloropropane, wherein, sodium metaphosphate and calcium chloride with
Mass parts meter, water, ethanol and epoxychloropropane are in terms of parts by volume, sodium metaphosphate, calcium chloride, epoxychloropropane, water, the ratio of ethanol
Example is (1~3):(1~7):(1~7)：(20~80):(20~80).
3. the method that electrostatic spraying as claimed in claim 1 prepares cross linked porous starch hemostatic microsphere, it is characterised in that described
Amidin is to be prepared from starch dissolution in pH value is 10~13 sodium hydrate aqueous solution.
4. the method that electrostatic spraying as claimed in claim 1 or 2 prepares cross linked porous starch hemostatic microsphere, it is characterised in that
Also include one or both of water soluble surfactant active and water-soluble polymer in the amidin.
5. the method that electrostatic spraying as claimed in claim 1 prepares cross linked porous starch hemostatic microsphere, it is characterised in that described
The feeding rate of electrostatic spraying is 1~80 μ L/min.
6. a kind of purposes of cross linked porous starch hemostatic microsphere prepared by method as claimed in claim 1 in hemostatic material.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110404114A (en) * | 2019-07-23 | 2019-11-05 | 广东省医疗器械研究所 | One kind having surface crater degradable macromolecule microballoon and the preparation method and application thereof |
| CN110538344A (en) * | 2019-10-09 | 2019-12-06 | 北京诺康达医药科技股份有限公司 | Medical degradable hemostatic material and preparation method thereof |
| CN110665049A (en) * | 2019-10-25 | 2020-01-10 | 石家庄亿生堂医用品有限公司 | Method for preparing hemostatic starch microspheres by ultrasonic |
| CN112617179A (en) * | 2020-11-13 | 2021-04-09 | 华南理工大学 | High-resistance single-particle starch microsphere, and preparation method and application based on electrostatic spraying method |
| CN112843324A (en) * | 2021-01-13 | 2021-05-28 | 山东省药学科学院 | Preparation method of rapidly degradable hemostatic powder |
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| CN101653714A (en) * | 2009-09-10 | 2010-02-24 | 复旦大学 | Fibroin nanosphere prepared by electrostatic spraying technology as well as preparation method and preparation device thereof |
| CN102406956A (en) * | 2011-03-09 | 2012-04-11 | 天津爱勒易医药材料有限公司 | Starch hemostatic microsphere and preparation method thereof |
| CN104311870A (en) * | 2014-11-07 | 2015-01-28 | 石家庄亿生堂医用品有限公司 | Medical hemostatic polysaccharide starch microsphere and preparation method thereof |
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| CN101205304A (en) * | 2007-12-10 | 2008-06-25 | 中国农业大学 | Starch microspheres and method for preparing the same |
| CN101653714A (en) * | 2009-09-10 | 2010-02-24 | 复旦大学 | Fibroin nanosphere prepared by electrostatic spraying technology as well as preparation method and preparation device thereof |
| CN102406956A (en) * | 2011-03-09 | 2012-04-11 | 天津爱勒易医药材料有限公司 | Starch hemostatic microsphere and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110404114A (en) * | 2019-07-23 | 2019-11-05 | 广东省医疗器械研究所 | One kind having surface crater degradable macromolecule microballoon and the preparation method and application thereof |
| CN110404114B (en) * | 2019-07-23 | 2021-06-22 | 广东省医疗器械研究所 | Degradable polymer microsphere with surface pits and preparation method and application thereof |
| CN110538344A (en) * | 2019-10-09 | 2019-12-06 | 北京诺康达医药科技股份有限公司 | Medical degradable hemostatic material and preparation method thereof |
| CN110665049A (en) * | 2019-10-25 | 2020-01-10 | 石家庄亿生堂医用品有限公司 | Method for preparing hemostatic starch microspheres by ultrasonic |
| CN110665049B (en) * | 2019-10-25 | 2022-02-01 | 石家庄亿生堂医用品有限公司 | Method for preparing hemostatic starch microspheres by ultrasonic |
| CN112617179A (en) * | 2020-11-13 | 2021-04-09 | 华南理工大学 | High-resistance single-particle starch microsphere, and preparation method and application based on electrostatic spraying method |
| CN112617179B (en) * | 2020-11-13 | 2022-07-26 | 华南理工大学 | High-resistance single-particle starch microsphere, and preparation method and application based on electrostatic spraying method |
| CN112843324A (en) * | 2021-01-13 | 2021-05-28 | 山东省药学科学院 | Preparation method of rapidly degradable hemostatic powder |
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Application publication date: 20170926 |