CN103319615B - A kind of hemostatic starch and preparation method thereof - Google Patents
A kind of hemostatic starch and preparation method thereof Download PDFInfo
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- CN103319615B CN103319615B CN201310166876.9A CN201310166876A CN103319615B CN 103319615 B CN103319615 B CN 103319615B CN 201310166876 A CN201310166876 A CN 201310166876A CN 103319615 B CN103319615 B CN 103319615B
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- 229920002472 Starch Polymers 0.000 title claims abstract description 87
- 235000019698 starch Nutrition 0.000 title claims abstract description 87
- 239000008107 starch Substances 0.000 title claims abstract description 85
- 230000002439 hemostatic Effects 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 58
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 45
- 229920000881 Modified starch Polymers 0.000 claims abstract description 42
- 235000019426 modified starch Nutrition 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000004368 Modified starch Substances 0.000 claims abstract description 38
- 210000004369 Blood Anatomy 0.000 claims abstract description 13
- 239000008280 blood Substances 0.000 claims abstract description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 32
- 239000000203 mixture Substances 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 20
- 239000003795 chemical substances by application Substances 0.000 claims description 16
- 239000003431 cross linking reagent Substances 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
- 210000001519 tissues Anatomy 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 11
- -1 diisopropyl aminoethyl chlorine Chemical compound 0.000 claims description 8
- 239000000376 reactant Substances 0.000 claims description 8
- 210000000056 organs Anatomy 0.000 claims description 7
- 210000004185 Liver Anatomy 0.000 claims description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 230000035876 healing Effects 0.000 claims description 3
- 230000001737 promoting Effects 0.000 claims description 3
- CSPHGSFZFWKVDL-UHFFFAOYSA-M (3-chloro-2-hydroxypropyl)-trimethylazanium;chloride Chemical compound [Cl-].C[N+](C)(C)CC(O)CCl CSPHGSFZFWKVDL-UHFFFAOYSA-M 0.000 claims description 2
- 241000271566 Aves Species 0.000 claims description 2
- 229920001353 Dextrin Polymers 0.000 claims description 2
- 239000004375 Dextrin Substances 0.000 claims description 2
- JQVDAXLFBXTEQA-UHFFFAOYSA-N Dibutylamine Chemical compound CCCCNCCCC JQVDAXLFBXTEQA-UHFFFAOYSA-N 0.000 claims description 2
- 206010022114 Injury Diseases 0.000 claims description 2
- 210000003734 Kidney Anatomy 0.000 claims description 2
- 241000270322 Lepidosauria Species 0.000 claims description 2
- 241000124008 Mammalia Species 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- UGTZMIPZNRIWHX-UHFFFAOYSA-K Sodium trimetaphosphate Chemical compound [Na+].[Na+].[Na+].[O-]P1(=O)OP([O-])(=O)OP([O-])(=O)O1 UGTZMIPZNRIWHX-UHFFFAOYSA-K 0.000 claims description 2
- 210000000952 Spleen Anatomy 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
- HGINCPLSRVDWNT-UHFFFAOYSA-N acrylaldehyde Chemical compound C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 230000002490 cerebral Effects 0.000 claims description 2
- 239000003153 chemical reaction reagent Substances 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims description 2
- 235000019425 dextrin Nutrition 0.000 claims description 2
- 238000001727 in vivo Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 230000003387 muscular Effects 0.000 claims description 2
- 125000000466 oxiranyl group Chemical group 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 210000004872 soft tissue Anatomy 0.000 claims description 2
- 239000001117 sulphuric acid Substances 0.000 claims description 2
- 235000011149 sulphuric acid Nutrition 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims 2
- 150000001412 amines Chemical class 0.000 claims 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims 1
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims 1
- 238000005886 esterification reaction Methods 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 11
- 230000023597 hemostasis Effects 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 3
- 238000004132 cross linking Methods 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 239000002250 absorbent Substances 0.000 description 11
- 230000002745 absorbent Effects 0.000 description 11
- 206010018987 Haemorrhage Diseases 0.000 description 9
- 239000008236 heating water Substances 0.000 description 5
- 239000008187 granular material Substances 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 3
- 150000004676 glycans Polymers 0.000 description 3
- 229920001282 polysaccharide Polymers 0.000 description 3
- 239000005017 polysaccharide Substances 0.000 description 3
- 150000004804 polysaccharides Polymers 0.000 description 3
- 230000002522 swelling Effects 0.000 description 3
- CWSZBVAUYPTXTG-UHFFFAOYSA-N 5-[6-[[3,4-dihydroxy-6-(hydroxymethyl)-5-methoxyoxan-2-yl]oxymethyl]-3,4-dihydroxy-5-[4-hydroxy-3-(2-hydroxyethoxy)-6-(hydroxymethyl)-5-methoxyoxan-2-yl]oxyoxan-2-yl]oxy-6-(hydroxymethyl)-2-methyloxane-3,4-diol Chemical compound O1C(CO)C(OC)C(O)C(O)C1OCC1C(OC2C(C(O)C(OC)C(CO)O2)OCCO)C(O)C(O)C(OC2C(OC(C)C(O)C2O)CO)O1 CWSZBVAUYPTXTG-UHFFFAOYSA-N 0.000 description 2
- 229940027278 Hetastarch Drugs 0.000 description 2
- 229920001612 Hydroxyethyl starch Polymers 0.000 description 2
- 238000007405 data analysis Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 229920000159 gelatin Polymers 0.000 description 2
- 235000019322 gelatine Nutrition 0.000 description 2
- 230000000025 haemostatic Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000001356 surgical procedure Methods 0.000 description 2
- 229920002101 Chitin Polymers 0.000 description 1
- DJHJJVWPFGHIPH-OODMECLYSA-N Chitin Chemical compound O[C@@H]1C(NC(=O)C)[C@H](O)OC(CO)[C@H]1COC[C@H]1C(NC(C)=O)[C@@H](O)[C@H](COC[C@H]2C([C@@H](O)[C@H](O)C(CO)O2)NC(C)=O)C(CO)O1 DJHJJVWPFGHIPH-OODMECLYSA-N 0.000 description 1
- 229920001661 Chitosan Polymers 0.000 description 1
- 102000008186 Collagen Human genes 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- 239000001828 Gelatine Substances 0.000 description 1
- 206010019677 Hepatic haemorrhage Diseases 0.000 description 1
- 229920002201 Oxidized cellulose Polymers 0.000 description 1
- 206010062936 Placenta accreta Diseases 0.000 description 1
- 241000282898 Sus scrofa Species 0.000 description 1
- ANOBYBYXJXCGBS-UHFFFAOYSA-L Tin(II) fluoride Chemical compound F[Sn]F ANOBYBYXJXCGBS-UHFFFAOYSA-L 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking Effects 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 230000023555 blood coagulation Effects 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- UZBQIPPOMKBLAS-UHFFFAOYSA-N diethylazanide Chemical compound CC[N-]CC UZBQIPPOMKBLAS-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- BRLQWZUYTZBJKN-UHFFFAOYSA-N epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 description 1
- 238000006266 etherification reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229920000578 graft polymer Polymers 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000009940 knitting Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229940107304 oxidized cellulose Drugs 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Abstract
The invention belongs to field of hemostasi starch, relate to a kind of hemostatic starch and application thereof.In order to solve the problem of hemostatic starch 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 hemostatic starch of high-hydroscopicity through steps such as crosslinking, etherificates.This hemostatic starch soaking effect is excellent, safety, stable, is a kind of biocompatibility, can be directly used for the hemostatic starch of blood wound surface.
Description
Technical field
The present invention relates to starch of a kind of hemostasis and preparation method thereof, particularly to a kind of biocompatibility, can be direct
For there being hemostatic starch 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 gelatine starch, collagen protein starch；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 starch, CN200810032631.6 biocompatibility is only
The modified starch material that blood, anti, promoting healing, surgery are closed, the change that CN200810033239.3 is biocompatibility pre-gelatinized
Property starch and preparation method thereof, CN200810009706.9 denaturated starch absorbable hemostatic material and preparation method thereof,
CN200910045995.2 biocompatible hemostatic and promotion 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 hemostatic starch 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 hemostatic starch, 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 hemostatic starch is provided, it is an object of the invention to by with
Lower technical scheme realizes:
A kind of preparation method of hemostatic starch, 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, obtains hemostatic starch.
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 hemostatic starch, 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 making
It all 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 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, obtains hemostatic starch.
The purposes of the hemostatic starch 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 hemostatic starch 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.
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 hemostatic starch obtained is better than like product of the prior art on water absorbing properties, has broad application prospects.This
Prepared by bright hemostatic starch 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 hemostatic starch 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 is respectively intended to prepare by the following method hemostatic starch 1-45:
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, obtains hemostatic starch.
Above-mentioned 46-90 kind combinations of reactants 2 is respectively intended to prepare hemostatic starch 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, obtains hemostatic starch.
Embodiment 2 matched group experimental design
According to the method for the embodiment 1,3,4,5 of patent cn200710199682.3, prepare hemostatic starch A respectively,
C, D, E, as a control group, specifically comprise the following steps that
By 2g pre-gelatinized hydroxypropyl PASELLI EASYGEL 51# as in 30ml water, it is stirred continuously, makes starch granules the most molten
Swollen and be dispersed in water, form uniform suspension, then sucking filtration, with ethanol wash, be dried, obtain hemostatic starch A.
By 2g carboxymethyl starch 66# as in 30ml water, it is stirred continuously, makes starch granules the most swelling and be scattered in water
In, form uniform suspension, be subsequently poured in container, then sucking filtration, with ethanol wash, be dried, obtain hemostatic starch C.
By 3g crosslinked carboxymethyl fecula 66#+As in 30ml water, it is stirred continuously, makes starch granules the most swelling and disperse
Yu Shuizhong, forms uniform suspension, is subsequently poured in container, then sucking filtration, with ethanol wash, is dried, obtains hemostatic starch
D。
By 3g hetastarch 88# modified starch as in 30ml water, it is stirred continuously, makes starch granules the most swelling and divide
Dissipate in water, form uniform suspension, then sucking filtration, with ethanol wash, be dried, obtain hemostatic starch E.
The water absorbent rate of embodiment 3 hemostatic starch and the detection of rate of water absorption
Starch water absorbent rate uses centrifugal determination, will about 0.025g starch as in 2ml water, balance l0min, 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 starch 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
Starch 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 hemostatic starch 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 hemostatic starch 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 hemostatic starch of employing has: hemostatic starch 1-90, and the hemostatic starch that matched group uses has hemostatic starch A, C,
D, E.
Respectively above-mentioned wound surface is stopped blooding.After hemorrhage, immediately hemostatic starch is placed on wound and with outside medical
Section's glove or hemostatic gauze press on starch, blocking blood flow, glove or gauze are unclamped gently after 1～2min, observe hemostasis
Whether effect, glove and gauze adhesion starch and sludged blood, cause the most hemorrhage when opening.Without modified starch is formed sediment after hemostasis
Powder is taken away or is removed, but does suitably infiltration with normal saline and rinse.
Result of the test:
Hemostatic starch 1-90 haemostatic effect is fine, and easy to use.All hemostatic starchs are sucked blood and and blood after meeting blood immediately
Liquid forms the starch-sludged blood colloid of viscosity, all can efficiently control the hemorrhage of liver wound surface, and stop blooding within 1 minute
Starch A, C, D, the E time more than 1.5 minutes just can control hemorrhage.Hemostatic starch 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 (12)
1. the preparation method of a hemostatic starch, 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, obtains hemostatic starch；
Step 1) in use modified starch be 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；
In step 1, the amount ratio of sodium hydroxide, modified starch and ethanol three is (1-5g): (30-60g): (200-500ml)；
One or more combinations during cross-linking agent is polyvinyl alcohol, acrylic aldehyde, formaldehyde, sodium trimetaphosphate in step 2；
The time being passed through nitrogen in step 3 for the first time is 5-15min；
The time being passed through nitrogen in step 3 for the second time is 5-15min；
In step 3, etherifying agent is oxirane, 2-diethyl aminoethyl chlorine, diisopropyl aminoethyl chlorine or 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；
Diluted acid in step 4 is one or more combinations in hydrochloric acid, sulphuric acid, phosphoric acid, citric acid, acetic acid；
In step 5, washing uses reagent to be ethanol.
2. preparation method as claimed in claim 1, it is characterised in that: sodium hydroxide, modified starch, ethanol, cross-linking agent and ether
The amount ratio of agent is: (1-5g): (30-60g): (200-500ml): (3-8ml): (2-6ml).
3. preparation method as claimed in claim 1, it is characterised in that: in step 1 ethanol be concentration be the ethanol of 85%.
4. preparation method as claimed in claim 1, it is characterised in that: in step 3, water bath heating temperature is 40-70 DEG C.
5. preparation method as claimed in claim 1, it is characterised in that: in step 3, mixing time is 2-5h.
6. the preparation method of a hemostatic starch, it is characterised in that: comprise the following steps:
1) 2g sodium hydroxide, 50g modified starch and 300ml 85% 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, obtains hemostatic starch.
7. the hemostatic starch that method described in any one of claim 1-6 prepares.
8. the purposes of the hemostatic starch of claim 7, its feature exists: be used for preparing people, mammal, birds, reptile have
The hemostatic material of blood wound surface.
9. the purposes of the hemostatic starch of claim 7, 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.
10. the purposes of the hemostatic starch of claim 7, it is characterised in that: for preparing the material promoting organization healing.
The purposes of the hemostatic starch of 11. claim 10, it is characterised in that: described tissue include sub-dermal soft tissue, muscular tissue,
Osseous tissue, cerebral tissue, nervous tissue, liver,kidney,spleen.
The purposes of the hemostatic starch of 12. claim 7, it is characterised in that: for preparing the tissue preventing wound or organ and week
In the material that its hetero-organization enclosed or organ stick together.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310166876.9A CN103319615B (en) | 2013-05-08 | A kind of hemostatic starch and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310166876.9A CN103319615B (en) | 2013-05-08 | A kind of hemostatic starch and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103319615A CN103319615A (en) | 2013-09-25 |
| CN103319615B true CN103319615B (en) | 2016-11-30 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4117222A (en) * | 1976-07-31 | 1978-09-26 | Hoechst Aktiengesellschaft | Process for the manufacture of absorbent, modified starch ethers and their use |
| CN101361986A (en) * | 2007-08-09 | 2009-02-11 | 美国淀粉医疗公司 | Modified starch absorbable hemostasia material and preparation method thereof |
| CN101559235A (en) * | 2009-05-21 | 2009-10-21 | 官培龙 | Compound microporous starch powder hemostat and preparation method thereof |
| CN102740862A (en) * | 2009-12-04 | 2012-10-17 | 美格乐控股公司 | Microspheres of hydrolysed starch with endogenous, charged ligands |
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4117222A (en) * | 1976-07-31 | 1978-09-26 | Hoechst Aktiengesellschaft | Process for the manufacture of absorbent, modified starch ethers and their use |
| CN101361986A (en) * | 2007-08-09 | 2009-02-11 | 美国淀粉医疗公司 | Modified starch absorbable hemostasia material and preparation method thereof |
| CN101559235A (en) * | 2009-05-21 | 2009-10-21 | 官培龙 | Compound microporous starch powder hemostat and preparation method thereof |
| CN102740862A (en) * | 2009-12-04 | 2012-10-17 | 美格乐控股公司 | Microspheres of hydrolysed starch with endogenous, charged ligands |
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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. |