CN102423503B - Preparation method of high-efficiency silicon oxide hemostasis material - Google Patents
Preparation method of high-efficiency silicon oxide hemostasis material Download PDFInfo
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- CN102423503B CN102423503B CN201110442310.5A CN201110442310A CN102423503B CN 102423503 B CN102423503 B CN 102423503B CN 201110442310 A CN201110442310 A CN 201110442310A CN 102423503 B CN102423503 B CN 102423503B
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 239000000463 material Substances 0.000 title claims abstract description 66
- 229910052814 silicon oxide Inorganic materials 0.000 title claims abstract description 29
- 230000023597 hemostasis Effects 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims description 10
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910001424 calcium ion Inorganic materials 0.000 claims abstract description 27
- 210000002381 plasma Anatomy 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 230000008569 process Effects 0.000 claims abstract description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 31
- 235000012239 silicon dioxide Nutrition 0.000 claims description 29
- 230000002439 hemostatic effect Effects 0.000 claims description 25
- 238000001179 sorption measurement Methods 0.000 claims description 17
- 239000002210 silicon-based material Substances 0.000 claims description 16
- 230000004913 activation Effects 0.000 claims description 14
- 238000010521 absorption reaction Methods 0.000 claims description 11
- 238000004440 column chromatography Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 11
- 206010052428 Wound Diseases 0.000 abstract description 4
- 208000027418 Wounds and injury Diseases 0.000 abstract description 4
- 230000000202 analgesic effect Effects 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 238000001727 in vivo Methods 0.000 abstract description 2
- 239000012567 medical material Substances 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 abstract description 2
- 230000003213 activating effect Effects 0.000 abstract 1
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 230000003115 biocidal effect Effects 0.000 abstract 1
- 239000002775 capsule Substances 0.000 abstract 1
- 230000000025 haemostatic effect Effects 0.000 description 11
- 230000023555 blood coagulation Effects 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 239000000203 mixture Substances 0.000 description 8
- 210000004369 blood Anatomy 0.000 description 7
- 239000008280 blood Substances 0.000 description 7
- 229910021536 Zeolite Inorganic materials 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000010457 zeolite Substances 0.000 description 6
- 239000002808 molecular sieve Substances 0.000 description 5
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000013335 mesoporous material Substances 0.000 description 4
- 206010053567 Coagulopathies Diseases 0.000 description 3
- 229940030225 antihemorrhagics Drugs 0.000 description 3
- 230000035602 clotting Effects 0.000 description 3
- 230000015271 coagulation Effects 0.000 description 3
- 238000005345 coagulation Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- FYGHSUNMUKGBRK-UHFFFAOYSA-N 1,2,3-trimethylbenzene Chemical compound CC1=CC=CC(C)=C1C FYGHSUNMUKGBRK-UHFFFAOYSA-N 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- 108090000190 Thrombin Proteins 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- 235000011148 calcium chloride Nutrition 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000000235 small-angle X-ray scattering Methods 0.000 description 2
- 239000008279 sol Substances 0.000 description 2
- 229960004072 thrombin Drugs 0.000 description 2
- 241000459479 Capsula Species 0.000 description 1
- 241001269238 Data Species 0.000 description 1
- 102000010911 Enzyme Precursors Human genes 0.000 description 1
- 108010062466 Enzyme Precursors Proteins 0.000 description 1
- 208000007536 Thrombosis Diseases 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 210000000709 aorta Anatomy 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 210000000987 immune system Anatomy 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000000338 in vitro Methods 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 210000000653 nervous system Anatomy 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 210000000952 spleen Anatomy 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to a high-efficiency silicon oxide hemostasis material. The hemostasis material is prepared from silicon oxide adsorbing a large number of calcium ions and materials activating blood plasma. The invention has the advantages of moderate reaction conditions, convenient and feasible operation process, and low cost and easy acquisition of raw materials; and the prepared hemostasis material product has an excellent hemostasis effect. By using silicon oxide as the hemostasis material, the biocompatibility of the hemostasis material can be obviously improved, thereby showing the good prospect of the silicon oxide hemostasis material in the in-vivo application; because of the specific pore properties, the mesoporous silicon oxide material can adsorb antibiotic, analgesic and the like, thereby being beneficial to the treatment of wounds; and the material provided by the invention can be used for hemostasis in different medical situations, and can be prepared into wound plasters, transfusion plasters, self-adhesive dressings, cores of tablets and capsules, operation kits, first-aid kits and the like when being combined with other medical materials and medical appliances.
Description
Technical field
The invention belongs to field of biomedical materials, specifically, is a kind of preparation method of high-efficiency silicon oxide hemostasis material.
Technical background
Emergency haemostatic is an emerging research field in the world.Emergency haemostatic is developed mainly for the outer damaging the spleen and stomach emergency that The blood streamed down.(3 minutes) just can control the emergency as aorta is bled so in a short period of time, for further medical treatment tries to gain time precious to one.The eighties in 20th century, Francis X.Hursey was not intended to find that zeolite molecular sieve has good anastalsis and in 1989, applied for patent.At the beginning of 2002, Z-Medica company sets up, the novel hemostatic material of special Development and Production commodity Quikclot by name, this material is synthetic zeolite (the A type zeolite with 75%, LTA structure) the composite type zeolite hemostatic material mixing as binding agent for substrate and 25% clay, use at present the novel hemostatic material Quikclot that zeolite molecular sieve material is main body to be approved listing by U.S. FDA, no matter in laboratory (especially in field operations battlefield) still in practice, its haemostatic effect and improve survival rate two aspects and be all better than traditional hemostatic material.Due to Quikclot hemostatic material, to have thermal discharge high, Hui Dui wound tissue burn.Thereby exploitation has the low hemostatic material of good haemostatic effect side effect simultaneously, it is the target that research worker is consistent.
We have developed a series of molecular sieve hemostatic material on this basis, and (number of patent application is respectively 200810063282.4,200810122044.6,200810122045.0,200910095272.3,200910095273.8 etc.), but because aluminium element has very large harm to nervous system and immune system, thereby limited this application of class hemostatic material in human body.But earth silicon material does not exist this class problem, thereby the haemostatic effect of raising silica material seems very necessary.China Patent No. CN100345597C disclosed mesopore molecular sieve hemostatic material and preparation method thereof, but they just emphasize simple mesoporous material (main component is silicon dioxide and other oxides), but due to the processing not having through other, haemostatic effect is relatively poor.
Due to absorption calcium ion, the earth silicon material after adsorption activation blood plasma is similar to traditional zeolite molecular sieve again, meets that blood can absorb rapidly, swelling, through effect promotion thrombins such as physics, chemistry, biology, activates and sticks platelet, promotion thrombosis.There is in some aspects more superior character, to guarantee that it can be used as novel hemostatic material simultaneously.Because the absorption calcium ion again earth silicon material after adsorption activation blood plasma can discharge calcium ion, thereby acceleration coagulation process, simultaneously because earth silicon material has activated coagulation process, can produce the thrombin of more various activation, and these thrombins can only keep active at silica containing inorganic surfaces in this case, when this material touches blood, it is the thrombin proenzyme in can direct activation blood, thereby accelerate greatly coagulation process, play the effect of quick-acting haemostatic powder.Utilize its mesoporous silicon oxide to have the features such as larger aperture, pore volume, adsorbable antibiotics or analgesic, to obtain better curative effect simultaneously.The biocompatibility of more main silicon dioxide hemostatic material is better, and while being applied to human body, side effect is low.
Research shows, by silicon dioxide, adsorbs calcium ion, then adsorption activation blood plasma can improve the haemostatic effect of silicon dioxide greatly.So far, there are no earth silicon material is adsorbed to calcium ion, then adsorption activation blood plasma is for the domestic and international patent document report of medical applications.
Summary of the invention
Object of the present invention, just for the deficiencies in the prior art part, proposes a kind of preparation method that improves earth silicon material haemostatic effect.
In the preparation method of a kind of high-efficiency silicon oxide hemostasis material that the present invention proposes, silicon dioxide has following features: the Powdered silicon dioxide and the mesoporous silicon oxide that are less than 100um.Mesoporous silicon oxide in the present invention is self-assembly property and the template action of utilizing surfactant, through sol-gel process, synthesize, the present invention has simultaneously done corresponding improvement on this basis, obtained the mesoporous material of a large amount of absorption calcium ions, and and then adsorption activation blood plasma, obtained having the mesoporous silicon oxide hemostatic material of efficient haemostatic effect.But silicon dioxide of the present invention is not limited to this, the Powdered silicon dioxide that every other granular size is less than 100um is all applicable to the present invention as commercialization SiO 2 powder, column chromatography silicon dioxide.
Concrete technical scheme of the present invention is as follows:
The present invention is a kind of high-efficiency silicon oxide hemostasis material, and hemostatic material is that silicon dioxide has adsorbed a large amount of calcium ions, and adsorption activation the material of blood plasma.
Concrete steps of the present invention are as follows:
1) solution of the raw material of hemostatic material and calcium ions is carried out to calcium ion absorption;
2) by the silicon dioxide adsorption activation blood plasma after calcium ion absorption, then vacuum drying, preservation, obtain high-efficiency silicon oxide hemostasis material.
The raw material of hemostatic material of the present invention is mesoporous silicon oxide, mesoporous silicon oxide synthesizes by sol-gal process, mesoporous material synthetic specific as follows: structure directing agent is dissolved in the deionized water that contains medium, stirring obtains uniform solution, then add inorganic precursors TEOS, continue stirring and obtain stable colloidal sol; By the colloidal sol obtaining hydro-thermal regular hour at a certain temperature, burin-in process; Then after cool to room temperature, filter, wash, be dried.Finally roasting at a certain temperature, removes structure directing agent.The sintering temperature of the mesoporous silicon oxide after synthetic is 250 ℃～450 ℃, and roasting time is 3h～6h.
The raw material of hemostatic material of the present invention can be also the Powdered silicon dioxide that is less than 100um.
The Powdered silicon dioxide of the 100um of being less than of the present invention is commercialization SiO 2 powder or column chromatography silicon dioxide.
Calcium ion concentration of the present invention is 0.1M～5M, and calcium ion adsorption time is 1h～3h, and the adsorption temp of calcium ion is 10 ℃～100 ℃.
Earth silicon material after calcium ion absorption of the present invention and the ratio of blood plasma are 1: 0.2～5, the ratio of the earth silicon material after the amount of deionized water adding during blood plasma absorption and calcium ion absorption is 1:, 1～6, the adsorption activation time is 10～30min, and vacuum drying temperature is 20 ℃～38 ℃.
Tool of the present invention has the following advantages:
1, reaction condition is gentle, easy to operation, and raw material is cheap and easy to get; The hemostatic material product haemostatic effect obtaining is fabulous;
2, by using silicon dioxide as hemostatic material, can obviously improve the biocompatibility of hemostatic material, represent the good prospect of application in vivo of silicon dioxide hemostatic material;
3, the distinctive porous of Metaporous silicon dioxide material, can adsorption antibacterial element and analgesic etc., contribute to the treatment of wound, material of the present invention can be for the hemostasis of different medical applications, with other medical materials, medical apparatus and instruments combination, can be made into adhesive bandage, infusion patch, sticking dressing, Tablet and Capsula core material, operation bag, first-aid kit etc.
Accompanying drawing explanation
Fig. 1 is the blood coagulation design sketch of the coagulant material of FDU-12 Metaporous silicon dioxide material in the present invention;
Fig. 2 serves as reasons and take the transmission electron microscope picture of F127 as the synthetic mesoporous FDU-12 Metaporous silicon dioxide material of structure directing agent water;
Fig. 3 serves as reasons and take the SAXS collection of illustrative plates of F127 as the synthetic mesoporous FDU-12 Metaporous silicon dioxide material of structure directing agent water;
Fig. 4 is the external blood coagulation design sketch of commercialization silicon dioxide and column chromatography earth silicon material.
The specific embodiment
The invention is further illustrated by the following examples:
1.0g EO106PO70EO106 (F127), 1.2g trimethylbenzene and 2.5g KCl are dissolved in the HCl solution that 100ml concentration is 2M, and stirring adds 4.32g TEOS after half an hour, and mixture is strong agitation 24h under 14 ℃ of conditions.Mixed solution is transferred in water heating kettle at 120 ℃ of hydro-thermal 24h.Then filtration washing, obtains product at 60 ℃ after dry, then at 350 ℃ roasting 6h.After cooling room temperature, obtain the mesoporous FDU-12 material of three-dimensional cubic phase.Its blood coagulation effect is poor, sees the close oblique line of Fig. 1, and error line is obtained by three groups of experimental datas.FDU-12 material has good order mesoporous structure, sees the TEM of Fig. 2 FDU-12, and the SAXS figure of FDU-12 material is shown in Fig. 3.
By the CaCl2 solution room temperature mix and blend 3h of 2.0g FDU-12 material and 40ml 5M, then filter deionized water wash 5 times, 60 ℃ of mesoporous materials that obtain adsorbing calcium ion after dry.Its blood coagulation effect is poor, sees the closeer oblique line of Fig. 1.
Embodiment 3
The FDU-12 material that 1.0g is adsorbed to calcium ion mixes with 3ml deionized water, then adds respectively the porcine blood plasma of 1ml.Mix, stir 15min, 25 ℃ of vacuum dryings then, obtain the Metaporous silicon dioxide material of adsorption activation blood plasma, and its blood coagulation effect is very good, sees that Fig. 1 dredges oblique line.
Embodiment 4
Respectively by the CaCl2 solution room temperature mix and blend 3h of the commercialization earth silicon material of 2.0g, column chromatography silicon dioxide (100 order～200 order) and 40ml 5M, then filter, deionized water wash 5 times, 60 ℃ of earth silicon materials that obtain adsorbing calcium ion after dry.Its blood coagulation effect is poor sees the real block diagram of Fig. 4.
The commercialization SiO 2 powder and the column chromatography earth silicon material that respectively 1.0g are adsorbed to calcium ion mix with 1ml deionized water, then add respectively the porcine blood plasma of 1ml.Mix, stir 15min, 25 ℃ of vacuum dryings then, obtain the earth silicon material of adsorption activation blood plasma, and its blood coagulation effect is very good, sees the empty block diagram of Fig. 4.
External blood coagulation experiment is carried out at 25 ℃, and pig whole blood is in advance 25 ℃ of constant temperature water bath half an hour.During experiment in vitro, first determine nature clotting time, get the 0.2M CaCl of different volumes
2solution, then adds the whole blood of 2ml constant temperature, makes nature clotting time in 10min left and right.The external blood coagulation experimental procedure of hemostatic material is as follows: the material of getting 0.1g joins in the centrifuge tube of 10ml, then adds a certain amount of 0.2M CaCl
2, finally add the whole blood of 2ml constant temperature, start to clock simultaneously, time during whole blood coagulation is designated as clotting time.For commercialization earth silicon material and column chromatography earth silicon material, the quantity of material of getting is 0.2g.
Claims (5)
1. a high-efficiency silicon oxide hemostasis material, is characterized in that, described hemostatic material is the absorption calcium ion earth silicon material after adsorption activation blood plasma again, and described silicon dioxide is selected from Powdered silicon dioxide and the mesoporous silicon oxide that is less than 100um.
2. a preparation method for high-efficiency silicon oxide hemostasis material as claimed in claim 1, is characterized in that, concrete steps are as follows:
1) solution of the raw material of hemostatic material and calcium ions is carried out to calcium ion absorption, the raw material of described hemostatic material is selected from Powdered silicon dioxide and the mesoporous silicon oxide that is less than 100um;
2) by the silicon dioxide adsorption activation blood plasma after calcium ion absorption, then vacuum drying, preservation, obtain high-efficiency silicon oxide hemostasis material.
3. the preparation method of high-efficiency silicon oxide hemostasis material according to claim 2, it is characterized in that, the raw material of described hemostatic material is mesoporous silicon oxide, described mesoporous silicon oxide synthesizes by sol-gal process, the sintering temperature of the mesoporous silicon oxide after synthetic is 250 ℃～450 ℃, and roasting time is 3h～6h.
4. the preparation method of high-efficiency silicon oxide hemostasis material according to claim 2, is characterized in that, the described Powdered silicon dioxide that is less than 100um is commercialization SiO 2 powder or column chromatography silicon dioxide.
5. according to the preparation method of the high-efficiency silicon oxide hemostasis material described in claim 2 or 3 or 4, it is characterized in that, described calcium ion concentration is 0.1M～5M, and calcium ion adsorption time is 1h～3h, and the adsorption temp of calcium ion is 10 ℃～100 ℃.
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| CN104018234B (en) * | 2014-06-04 | 2017-06-30 | 东华大学 | A kind of preparation method of the composite nano-fiber membrane for being capable of quick-acting haemostatic powder |
| CN106913546B (en) * | 2015-12-28 | 2021-06-22 | 山东新时代药业有限公司 | Fast-dissolving minodronic acid tablet and preparation method thereof |
| CN108379648A (en) * | 2018-03-03 | 2018-08-10 | 青岛大学 | A kind of preparation method of original position inductive formation fibrin ferment load regenerated oxycellulose as styptic material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4822349A (en) * | 1984-04-25 | 1989-04-18 | Hursey Francis X | Method of treating wounds |
| CN1727011A (en) * | 2005-06-16 | 2006-02-01 | 复旦大学 | Hemostatic material of new type pore-borne molecular sieve and preparation method |
| CN101708183A (en) * | 2009-11-10 | 2010-05-19 | 浙江大学 | Method for improving haemostatic effect of external-use zeolite haemostatic |
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| US20030195284A1 (en) * | 2002-04-10 | 2003-10-16 | Paik Syng L. | Low bio-burden elastic bandage |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4822349A (en) * | 1984-04-25 | 1989-04-18 | Hursey Francis X | Method of treating wounds |
| CN1727011A (en) * | 2005-06-16 | 2006-02-01 | 复旦大学 | Hemostatic material of new type pore-borne molecular sieve and preparation method |
| CN101708183A (en) * | 2009-11-10 | 2010-05-19 | 浙江大学 | Method for improving haemostatic effect of external-use zeolite haemostatic |
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