CN103319744B - A kind of sthptic sponge and preparation method thereof - Google Patents
A kind of sthptic sponge and preparation method thereof Download PDFInfo
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- CN103319744B CN103319744B CN201310166946.0A CN201310166946A CN103319744B CN 103319744 B CN103319744 B CN 103319744B CN 201310166946 A CN201310166946 A CN 201310166946A CN 103319744 B CN103319744 B CN 103319744B
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Abstract
The invention belongs to sthptic sponge field, relate to a kind of sthptic sponge and application thereof.In order to solve the problem of sthptic sponge water absorption difference in prior art, the technical scheme is that and various modified starches of the prior art are mixed with sodium hydroxide, modified starch and ethanol, and finally prepare the sthptic sponge of high-hydroscopicity through steps such as crosslinking, etherificates.This sthptic sponge soaking effect is excellent, safety, stable, is a kind of biocompatibility, can be directly used for the sthptic sponge of blood wound surface.
Description
Technical field
The present invention relates to sponge of a kind of hemostasis and preparation method thereof, particularly to a kind of biocompatibility, can be direct
For there being sthptic sponge of blood wound surface and preparation method thereof.
Background technology
Hemorrhage is the phenomenon being easiest in accident and medical procedure occur, the life security of substantial amounts of hemorrhage entail dangers to people,
It is thus desirable to stop blooding in time for hemorrhage wound surface.
Along with the development of medical science, hemostatic material is of a great variety, for biocompatibility, and conventional biocompatible hemostatic
Material has: the gelatin class hemostatic materials such as absorbability gelfoam, collagen protein sponge；Oxidized cellulose, oxidation regeneration fiber
Element class hemostatic material；The natural biological polysaccharide hemostatic materials etc. such as chitosan/chitin kind, starch polysaccharide.
Present disclosure relates to the hemostatic material of starch polysaccharide, and the patent application that this field is relevant is as follows:
CN200710141944.0 denaturated starch absorbable hemostatic material and preparation method thereof, CN200710199682.3
Biocompatibility modified starch sponges, CN200810032631.6 biocompatible hemostatic, anti, promoting healing, surgery are closed
Modified starch material, modified starch that CN200810033239.3 is biocompatibility pre-gelatinized and preparation method thereof,
CN200810009706.9 denaturated starch absorbable hemostatic material and preparation method thereof, CN200910045995.2 bio-compatible
Property hemostasis and promote knitting material and preparation method thereof.
Above 6 patent applications, described content is roughly the same, for same applicant or inventor.In above-mentioned patent
Disclose partial denaturation starch purposes in terms of hemostasis, and propose several specific modified starch, as cationic starch,
Epichlorohydrin cross-linked starch, carboxymethyl starch, hetastarch, the modified starch of pre-gelatinized, the hydroxypropyl two starch phosphorus of pre-gelatinized
Acid esters, acrylic acid-carboxymethyl starch graft copolymer etc., but its specific nature and detailed applications are not illustrated.
Applicant has carried out systematic study to above-mentioned all kinds of modified starches, finds that the modified starch in above-mentioned patent application is inhaled
Water multiplying power is low, unstable properties, it is impossible to enough meet the demand of clinical hemostasis.Applicant experimental studies have found that through being repeated several times,
Modified starch of the prior art is made sthptic sponge after series of physical chemical treatment, it is possible to be greatly improved
Its water absorption, has fabulous application prospect.Simultaneously applicant also by testing sieve have selected preferred preparation raw material proportioning and
Technological parameter, its preparation is more stable, safety, more benefits industrialized production.
Summary of the invention
It is an object of the present invention to provide a kind of new sthptic sponge, this material good water absorption, safety, stable performance,
Overcome modified starch water absorption in prior art low, the shortcomings such as preparation is unstable.
Further object is that the preparation method that described sthptic sponge is provided, it is an object of the invention to by with
Lower technical scheme realizes:
A kind of preparation method of sthptic sponge, it is characterised in that: comprise the following steps:
1) sodium hydroxide, modified starch and ethanol are put in reactor, and mix and blend make it all dissolve；
2) in reactor, add cross-linking agent, react 50-120min；
3) in reactor, it is passed through nitrogen, is subsequently adding etherifying agent and reacts, be again passed through nitrogen, seal reactor,
Heating Water, stirring；
4) with diluted acid, above-mentioned reactant is neutralized to pH6.0-8.0；
5) sucking filtration, washing, it is dried, lyophilizing under low temperature, obtains sthptic sponge.
Preferably, the modified starch used in the 1st step is pre-gelatinized starch, denaturated starch by acid, dextrin, Oxytarch, ester
Change one or more the combination in starch, etherification starch, crosslinked starch, graft starch, composite modified starch.
Preferably, in step 1, the amount ratio of sodium hydroxide, modified starch and ethanol three is (1-5g): (30-60g):
(200-500ml)。
Preferably, one or more groups during cross-linking agent is polyvinyl alcohol, acrylic aldehyde, formaldehyde, sodium trimetaphosphate in step 2
Close.
Preferably, the time being passed through nitrogen in step 3 for the first time is 5-15min.
Preferably, the time being passed through nitrogen in step 3 for the second time is 5-15min.
Preferably, in step 3, etherifying agent is oxirane, 2-diethyl aminoethyl chlorine, diisopropyl aminoethyl chlorine or two
The chloro-2 hydroxypropyl ammonia diethyl tertiary amines of ethylamino-ethyl bromine, 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride, 3-, N-(2,3-epoxies
Propyl group) diethylamide, N-(2,3-glycidyl) dibutylamine, one in N-(2,3-glycidyl)-methylphenylamine or
Multiple combination.
Preferably, one or more combinations during the diluted acid in step 4 is hydrochloric acid, sulphuric acid, phosphoric acid, citric acid, acetic acid.
Preferably, in step 4, pH value is 6.5-7.5.
Preferably, in step 5, washing uses reagent to be ethanol.
Preferably, the amount ratio of sodium hydroxide, modified starch, ethanol, cross-linking agent and etherifying agent is: (1-5g): (30-
60g)∶(200-500ml)∶(3-8ml)∶(2-6ml)。
Preferably, in step 1 ethanol be concentration be the ethanol of 85%.
Preferably, in step 3, Heating Water temperature is 40-70 DEG C.
Preferably, in step 3, mixing time is 2-5h.
A kind of preparation method of sthptic sponge, it is characterised in that: comprise the following steps:
1) 2g sodium hydroxide, 50g modified starch and 300ml85% ethanol are put in reactor, and
Mix and blend also makes it all dissolve；
2) in reactor, add cross-linking agent, react 30-120min；
3) in reactor, it is passed through nitrogen 5-15min, is subsequently adding 3ml etherifying agent and reacts, be again passed through nitrogen 5-
15min, seals reactor, Heating Water to (30-70) DEG C, stirring reaction 2-5 hour；
4) with diluted acid, above-mentioned reactant is neutralized to pH6.5-7.5；
5) sucking filtration, with ethanol wash, is dried, lyophilizing under low temperature, obtains sthptic sponge.
The purposes of the sthptic sponge that another Technical Design of the present invention is prepared by the method for the present invention:
For preparing people, mammal, birds, reptile have the hemostatic material of blood wound surface.
Blood wound surface is had or for surgery hands for preparing body surface, in-vivo tissue organ and body cavity inner tissue or organ
Hemostatic material under art, emergency care of trauma, laryngoscope, endoscope, chamber mirror.
For preparing the material promoting organization healing.
Preferably, described tissue include sub-dermal soft tissue, muscular tissue, osseous tissue, cerebral tissue, nervous tissue, liver, kidney,
Spleen.
In the material that preparation prevents its hetero-organization or the organ of the tissue of wound or organ and surrounding from sticking together.
Applicant, after having carried out the test of a series of conditional filtering, finds that the method for the present invention has the following characteristics that
1. modified starch, cross-linking agent, the kind of etherifying agent are had no requirement by the method for the present invention, in prior art often
This method is may be used to, its water absorbent rate of the sthptic sponge prepared and suction with the modified starch seen, cross-linking agent, etherifying agent
Water speed is all far above degeneration sponge of the prior art, such as, compared with matched group, water absorbent rate averagely improves more than 20%,
Rate of water absorption improves more than 1 times, has obvious performance advantage.
2. understanding through data analysis, the proportioning of sodium hydroxide, modified starch and ethanol is to water absorbent rate and water suction speed
Rate has critically important impact, when the proportioning of sodium hydroxide, modified starch and ethanol is 2g: 50g: 300ml, water absorbent rate and
Rate of water absorption reaches peak, and unrelated with the selection of modified starch and cross-linking agent, etherifying agent.
Beneficial effects of the present invention: the present invention by carrying out some physical chemistry process, significantly to existing modified starch
Improve its water absorbing properties, and filtered out preferred preparation raw material proportioning and technological parameter by great many of experiments so that system
The standby sthptic sponge obtained is better than like product of the prior art on water absorbing properties, has broad application prospects.This
Prepared by bright sthptic sponge convenient, preparation is more stable, safety, more benefits industrialized production.
Detailed description of the invention
Being further described in detail the present invention below in conjunction with detailed description of the invention, the embodiment be given is only for explaining
The bright present invention rather than in order to limit the scope of the present invention.
Embodiment 1 sthptic sponge of the present invention preferred substance consumption and the screening test of step parameter
In reaction, selection and the consumption thereof of each material see table
Table 1.
Above-mentioned 1-45 kind combinations of reactants 1 is respectively intended to prepare sthptic sponge 1-45 by the following method:
Method 1: sodium hydroxide, modified starch and ethanol are put in reactor, and mix and blend make its CL；
In reactor, add cross-linking agent, react 50min；
In reactor, it is passed through nitrogen 5min, is subsequently adding etherifying agent and reacts, be again passed through nitrogen 5min, seal anti-
Answer device, Heating Water to 40 DEG C, stirring reaction 2 hours；
With diluted acid, above-mentioned reactant is neutralized to pH6.5；
Sucking filtration, with ethanol wash, is dried ,-45 DEG C, vacuum be lyophilization 15 hours under 15 handkerchiefs, obtain hemostasis sea
Continuous.
Above-mentioned 46-90 kind combinations of reactants 2 is respectively intended to prepare sthptic sponge 46-90 by the following method:
Method 2: sodium hydroxide, modified starch and ethanol are put in reactor, and mix and blend make its CL；
In reactor, add cross-linking agent, react 120min；
In reactor, it is passed through nitrogen 15min, is subsequently adding etherifying agent and reacts, be again passed through nitrogen 15min, seal
Reactor, Heating Water to 70 DEG C, stirring reaction 5 hours；
With diluted acid, above-mentioned reactant is neutralized to pH7.5；
Sucking filtration, with ethanol wash, is dried ,-45 DEG C, vacuum be lyophilization 15 hours under 15 handkerchiefs, obtain hemostasis sea
Continuous.
Embodiment 2 matched group experimental design
According to the method for the embodiment 1,3,4,5 of patent cn200710199682.3, prepare sthptic sponge A respectively,
C, D, E, as a control group.
The water absorbent rate of embodiment 3 sthptic sponge and the detection of rate of water absorption
Multiplying power that sponge sucks in water uses centrifugal determination, will about 0.025g sponge as in 2ml water, balance 10min, then
Putting in centrifuge, under 500rpm rotating speed, take out after centrifugal 10 minutes, calculating residual liquid amount of weighing, each sample test is gone for 6 times
Meansigma methods.
The rate of water absorption of sponge is observed by Germany's Dataphysics company OCA40Micro video contact angle measuring instrument.
Experimental result: the hemostasis that the 90 kinds of hemostatic starchs prepared by embodiment 1 method and embodiment 2 matched group are obtained
Sponge A, its water absorbent rate of C, D, E and rate of water absorption contrast are as shown in the table:
Table 2
Interpretation:
Following conclusion can be drawn by above experimental data:
1. modified starch, cross-linking agent, the kind of etherifying agent are had no requirement by the method for the present invention, in prior art often
This method is may be used to, its water absorbent rate of the sthptic sponge prepared and suction with the modified starch seen, cross-linking agent, etherifying agent
Water speed is all far above modified starch of the prior art, such as, compared with matched group, water absorbent rate averagely improves more than 20%,
Rate of water absorption improves more than 1 times, has obvious performance advantage.
2. understanding through data analysis, the proportioning of sodium hydroxide, modified starch and ethanol is to water absorbent rate and water suction speed
Rate has critically important impact, when the proportioning of sodium hydroxide, modified starch and ethanol is 2g: 50g: 300ml, water absorbent rate and
Rate of water absorption reaches peak, and unrelated with the selection of modified starch and cross-linking agent, etherifying agent.
The embodiment 4 modified starch sthptic sponge haemostatic effect to liver Hemorrhage Model
Test method:
Cutting liver placenta percreta area 1.5cm × 2.5cm in pig liver surface scalpel, Wound depth is 0.25cm,
Making hemorrhage wound surface, the sthptic sponge of employing has: sthptic sponge 1-90, and the sthptic sponge that matched group uses has sthptic sponge A, C,
D, E.
Respectively above-mentioned wound surface is stopped blooding.After hemorrhage, immediately sthptic sponge is placed on wound and with outside medical
Section's glove or hemostatic gauze press on sponge, blocking blood flow, glove or gauze are unclamped gently after 1～2min, observe hemostasis
Whether effect, glove and gauze adhesion sponge and sludged blood, cause the most hemorrhage when opening.Without by modified starch sea after hemostasis
Silk floss is taken away or is removed, but does suitably infiltration with normal saline and rinse.
Result of the test:
Sthptic sponge 1-90 haemostatic effect is fine, and easy to use.All sthptic sponges are sucked blood and and blood after meeting blood immediately
Liquid forms the sponge-sludged blood colloid of viscosity, all can efficiently control the hemorrhage of liver wound surface, and stop blooding within 1 minute
Sponge A, C, D, the E time more than 1.5 minutes just can control hemorrhage.Sthptic sponge 1-90 closely glues with liver wound tissue
Attached, promote blood coagulation, sludged blood does not sticks together with the gauze dressing of pressing, does not results in the most hemorrhage.
Claims (8)
1. the preparation method of a sthptic sponge, it is characterised in that: comprise the following steps:
1) sodium hydroxide, modified starch and ethanol are put in reactor, and mix and blend make it all dissolve；
2) in reactor, add cross-linking agent, react 50-120min；
3) in reactor, it is passed through nitrogen, is subsequently adding etherifying agent and reacts, be again passed through nitrogen, seal reactor, water-bath
Heating, stirring；
4) with diluted acid, above-mentioned reactant is neutralized to pH6.5-7.5；
5) sucking filtration, washing, it is dried, lyophilizing under low temperature, obtains sthptic sponge；
1st) modified starch used in step is pre-gelatinized starch, denaturated starch by acid, dextrin, Oxytarch, esterification starch, etherificate
One or more combination in starch, crosslinked starch, graft starch, composite modified starch；
Step 1) in sodium hydroxide, the amount ratio of modified starch and ethanol three be (1-5g): (30-60g): (200-500mL)；
Step 2) in cross-linking agent be in polyvinyl alcohol, acrylic aldehyde, formaldehyde, sodium trimetaphosphate one or more combination；
Step 3) in be passed through for the first time time of nitrogen be 5-15min；
Step 3) in second time to be passed through time of nitrogen be 5-15min；
Step 3) in etherifying agent be oxirane, 2-diethyl aminoethyl chlorine, diisopropyl aminoethyl chlorine, diethyl aminoethyl
The chloro-2 hydroxypropyl ammonia diethyl tertiary amines of bromine, 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride, 3-, N-(2,3-glycidyl) diethyl
One or more combinations in amine, N-(2,3-glycidyl) dibutylamine, N-(2,3-glycidyl)-methylphenylamine；
Step 4) in diluted acid be in hydrochloric acid, sulphuric acid, phosphoric acid, citric acid, acetic acid one or more combination；
Step 5) in washing use reagent be ethanol；
The amount ratio of sodium hydroxide, modified starch, ethanol, cross-linking agent and etherifying agent is: (1-5g): (30-60g): (200-
500mL)∶(3-8mL)∶(2-6mL)；
Step 1) in ethanol be concentration be the ethanol of 85%；
Step 3) in water bath heating temperature be 40-70 DEG C；
Step 3) in mixing time be 2-5h.
2. the preparation method of a sthptic sponge, it is characterised in that: comprise the following steps:
1) 2g sodium hydroxide, 50g modified starch and 300mL85% ethanol are put in reactor, and mix and blend make it complete
Portion dissolves；
2) in reactor, add cross-linking agent, react 30-120min；
3) in reactor, it is passed through nitrogen 5-15min, is subsequently adding 3mL etherifying agent and reacts, be again passed through nitrogen 5-
15min, seals reactor, heating in water bath to (30-70) DEG C, stirring reaction 2-5 hour；
4) with diluted acid, above-mentioned reactant is neutralized to pH6.5-7.5；
5) sucking filtration, with ethanol wash, is dried, lyophilizing under low temperature, obtains sthptic sponge.
3. the sthptic sponge that any one of claim 1-2 method prepares.
4. the purposes of the sthptic sponge of claim 3, its feature exists: be used for preparing people, mammal, birds, reptile have
The hemostatic material of blood wound surface.
5. the purposes of the sthptic sponge of claim 3, its feature exists: be used for preparing body surface, in-vivo tissue organ has blood to create
Face or the hemostatic material under surgical operation, emergency care of trauma, laryngoscope, endoscope, chamber mirror.
6. the purposes of the sthptic sponge of claim 3, it is characterised in that: for preparing the material promoting organization healing.
7. the purposes of the sthptic sponge of claim 6, it is characterised in that: described tissue includes sub-dermal soft tissue, muscular tissue, bone
Tissue, cerebral tissue, nervous tissue, liver,kidney,spleen.
8. the purposes of the sthptic sponge of claim 3, it is characterised in that: for preparing the tissue or organ and surrounding preventing wound
Its hetero-organization or the material that sticks together of organ in.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101455857A (en) * | 2007-12-11 | 2009-06-17 | 美国淀粉医疗公司 | Biocompatibility modified starch sponges |
| CN102600495A (en) * | 2011-01-19 | 2012-07-25 | 北京博恩康生物科技有限公司 | Absorbable hemostatic composition and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101455857A (en) * | 2007-12-11 | 2009-06-17 | 美国淀粉医疗公司 | Biocompatibility modified starch sponges |
| CN102600495A (en) * | 2011-01-19 | 2012-07-25 | 北京博恩康生物科技有限公司 | Absorbable hemostatic composition and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 响应面法优化交联羧甲基玉米淀粉制备工艺的研究;周睿等;《粮食加工》;20081231(第06期);第48-51、72页 * |
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Effective date of registration: 20150409 Address after: 225300 Jiangsu city of Taizhou province China pharmaceutical Road East, Xinyang City Road on the north side (G34 building) Applicant after: Jiangsu Deweilan Medical Instrument Co., Ltd. Applicant after: Zhou Xiao Address before: 225300 Jiangsu city of Taizhou province China pharmaceutical Road East, Xinyang City Road on the north side (G34 building) Applicant before: Jiangsu Deweilan Medical Instrument Co., Ltd. Applicant before: Liu Bozhi Applicant before: Zhou Xiao |
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Address after: 225300 Taizhou City, Jiangsu Province, China Medicine Chengkou Tai Road East, Xinyang Road North (G34) Workshop Area, First to Fourth Floors Co-patentee after: Zhou Xiao Patentee after: Jiangsu Deweilan medical equipment Limited by Share Ltd Address before: 225300 Jiangsu city of Taizhou province China pharmaceutical Road East, Xinyang City Road on the north side (G34 building) Co-patentee before: Zhou Xiao Patentee before: Jiangsu Deweilan Medical Instrument Co., Ltd. |
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