CN1065771C - Method for radio-grafting medical high molecular aquagel membrane - Google Patents
Method for radio-grafting medical high molecular aquagel membrane Download PDFInfo
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- CN1065771C CN1065771C CN98124925A CN98124925A CN1065771C CN 1065771 C CN1065771 C CN 1065771C CN 98124925 A CN98124925 A CN 98124925A CN 98124925 A CN98124925 A CN 98124925A CN 1065771 C CN1065771 C CN 1065771C
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Abstract
The present invention belongs to the biomedical material field of a high molecular polymer. Polyethylene oxide, polyvinyl alcohol and water are used as raw materials, a water gel membrane is prepared by the technical steps of membrane casting, hot and cold cyclic treatment, radiation processing, etc. The method has the advantages of simple preparing technology, raw material saving and cost reduction. The product has favorable performance and excellent hydrophilicity, permeability and tissue compatibility.
Description
The invention belongs to the high molecular polymer field of biomedical materials, be specifically related to a kind of radiation grafting technology of medical macromolecular materials aquagel membrane.
In the clinical medicine to various processing such as wound, burns than the large area skin wound, general applying biological material as from body, allogeneic or dermatoheteroplasty with the protection wound surface, reduce and infect, quicken more and.Yet these biological material sources are limited, and adopt the Corii Sus domestica transplanting can make receptor produce intensive rejection.Sensitizer only stays collagen fiber in the xenogenesis skin and will remove, and needs very complicated technique process.At present, use high molecular polymer in the world through crosslinking with radiation, promptly use the β electron beam irradiation processing of cobalt-60 and electron accelerator, can prepare the medical aquogel material that serves many purposes, as artificial skin wound dressing, drug sustained release system, cardiac valve, sensor, artificial intraocular lenses and contact lens etc.Because the medical aquogel material has good hydrophilicity, pliability, permeability and histocompatibility, and radiation synthesis can finish simultaneously with sterilization, so accepted by clinical medicine as a kind of medical material.
Macromolecular material commonly used has polyvinyl alcohol, polyethylene glycol oxide, polyvinyl pyrrolidone, poly-ethylacrylic acid hydroxyl ethyl ester, polyacrylamide etc., and can be used as raw material and make medical supplies, be nontoxic to body.Adopt different macromolecular materials, its processing technique difference, the performance of product and result of use also have suitable difference.By people Radiat.Phys.Chem.vol 46.NO.2 pp.169-174 such as Japanese Yoshii F, the chemical acetal method of 1995 usefulness that provide strengthens the radiation pre-treating technology of hydrogel mechanical strength, and this technology is complicated; The mechanical strength that people J.of controlled Releaset 18 (1992) 95-100 such as U.S. Peppas N.A and Scoff J.E provide the freeze-thaw cycle technology to strengthen hydrogel, however need-20 ℃-25 ℃ circulations 5 times; People Rodiat.Phys.Chem.Vol 42 such as Poland RosiakJ.M and Olejniczak J., No.4-6, pp 903-906, the hydrogel product thickness of describing in 1993 is the 3-4 millimeter.
The object of the present invention is to provide a kind of technology easy, save raw material, the radiation grafting new technology of the medical high molecular aquagel membrane that reduces cost, this technology can make properties of product more excellent, can have fabulous hydrophilic, permeability and histocompatibility.
Technical scheme of the present invention is as follows:
The present invention uses polyethylene glycol oxide and polyvinyl alcohol, at high temperature form the homogeneous aqueous solution, in cold cycling, form the physics coagulation between the high molecular polymer chain, again through the crosslinking electron beam irradiation grafting, the polymer of two kinds of different in kinds is connected together, forms the special graft of performance.
Technical process is as follows:
Block diagram is represented:
1, batching: selecting polyethylene glycol oxide and polyvinyl alcohol for use is raw material.
Polyethylene glycol oxide 6-24%, polyvinyl alcohol 2-12%, water 70-90%.
The said mixture aqueous solution is through heating for dissolving, and it is water-soluble to make it to become a kind of homogeneous mixture
Liquid.
2, mold: pour the said mixture aqueous solution Flat bottom container of all size into, mold thickness is 1.5
-2mm makes it cooling and solidifies.
3, cold cycling treatment: the said mixture aqueous solution is connected container puts in the refrigerator, temperature 0-5 ℃, the time
Between 24-36 hour, take out then, put room temperature 22-27 ℃, time 12-24 hour, so advance
2 cold cycling treatment of row are to form the physical crosslinking between the high molecular polymer chain.
4, RADIATION PROCESSING: it is crosslinked to adopt cobalt-60 and electron accelerator to carry out irradiation grafting.
(1) it is crosslinked its sample utilization electron accelerator to be carried out irradiation grafting; Condition: close rate is
20kGy/ time, room temperature is 22-27 ℃, and dosage is 40-60kGy.
(2) crosslinked with cobalt 60 irradiation graftings; Close rate is 10kGy/H, and dosage is 40-60kGy.
5, under aseptic condition, take out through the sample of irradiation grafting after crosslinked, put into 0-5 ℃ of ice above-mentioned
Case is preserved standby.
The invention has the advantages that:
Improve complicated radiation pre-treating technology in the present hydrogel preparation, made preparation technology easy, saved raw material, reduced cost, made properties of product more excellent, reduced sample thickness, increased mechanical strength.Overcome the conventional medical gauze, shortcoming such as biological dressing adhesion wound such as Corii Sus domestica and tissue rejection reaction.This aquagel membrane possesses fabulous hydrophilic, pliability, and permeability and histocompatibility are the desirable wound dressings of handling various skin injurys, can partly or entirely replace traditional husky cloth dressing and heterogenous skin and transplant.
The present invention has following accompanying drawing:
The gel fraction of Fig. 1 radiation grafting polyethylene glycol oxide hydrogel
The swelling degree of Fig. 2 radiation grafting polyethylene glycol oxide hydrogel
The tensile strength of Fig. 3 radiation grafting polyethylene glycol oxide hydrogel
The elongation at break of Fig. 4 radiation grafting polyethylene glycol oxide hydrogel
Embodiment 1: the preparation of polyethylene glycol oxide and polyvinyl alcohol radiation graft copolymer hydrogel wound dressing.
(1) electron beam β electron radiation grafting:
1, take by weighing polyethylene glycol oxide 28 grams, polyvinyl alcohol 12 grams are put into 160 gram deionized waters, heating
Dissolving.
2, pour in the culture dish polyethylene glycol oxide and the polyvinyl alcohol mixture solution of uniform dissolution into solution
Thickness is 2mm, and cooling is solidified.
3, the culture dish sample is put 24h in 4 ℃ of refrigerators, taken out then and put room temperature (25 ℃) 12h, so
4, the sample application electron accelerator β electronics after the cold cycling treatment is carried out the crosslinking with radiation grafting.
Radiation condition: electric current 10mA, accelerator energy 1.7MeV, close rate 20kGy/ time, 25 ℃ of room temperatures,
Dosage 40kGy.
5, the aseptic 4 ℃ of refrigerators of the hydrogel sample of radiation preparation are preserved standby.
(2) Co-60 gamma-radiation grafting:
1, preparation method is identical with electron radiation 1-3 step before the grafting of Co-60 gamma-radiation.
2, with the radiation of culture dish sample application Co-60 gamma-rays, radiation condition: close rate 10kGy/ hour, 4 hours time, dosage 40kGy, 25 ℃.
3, it is standby that the hydrogel sample of radiation preparation is put 4 ℃ of aseptic preservations of refrigerator.The physicochemical property index test of polyethylene glycol oxide and polyvinyl alcohol radiation graft copolymer hydrogel wound dressing
(1) the hydrogel gel fraction is measured
1, hydrogel sample is cut into 1 * 2cm fritter, totally 3, put into small beaker, put vacuum drying 24 hours
2, weigh rustless steel mesh bag weight be 0.5334 the gram
3, exsiccant water-setting blob of viscose is put into the rustless steel mesh bag respectively, the average of weighing is 0.5495 gram,
Put into the uncrosslinked colloidal sol of water heating for dissolving then
4, above-mentioned rustless steel mesh bag is put into methanol solution 1 hour, take out drying at room temperature, placed vacuum desiccator then interior 24 hours, be weighed as 0.5439 gram after the drying.
5, calculate:
Gel fraction (%)=65.2
(2) the hydrogel swelling degree is measured
Swelling degree (%)=1892.6
Annotate: 1, dried hydrogel weight is weighed after 24 hours in the vacuum desiccator for 3 parts of the hydrogel sample same form are placed;
2, exsiccant hydrogel sample being put into the distilled water immersion weighed after 24 hours.
(3) hydrogel tensile strength and elongation at break are measured
1, be that the cutter of ASTMD-1822-L is cut into the dumbbell shaped sample, dumbbell with hydrogel sample model
The sample intermediate width is 0.3cm, and each hydrogel sample is cut into 6 dumbbell shaped samples to be tested, uses
Calibrator is measured sample thickness (millimeter).
2, sample to be tested is used Changchun and produced stretching-machine measurement tensile strength, speed is 100 millimeters/minute.
3, measure the middle 1 centimetre of maximum elongation degree when being stretched to fracture of dumbbell shaped sample simultaneously.
4, calculate:
Tensile strength (MPa)=4.5
Elongation at break (%)=900
(4) hydrogel physicochemical property measurement result
The physicochemical property of the polyethylene glycol oxide hydrogel that the crosslinking with radiation grafting forms is shown in Fig. 1,2,3,4.Symbol is the physicochemical property of leg-of-mutton curve polyethylene glycol oxide (PEO) the hydrogel sample that to represent weight ratio be 20% grafting polyvinyl alcohol (PVA).The result shows:
1, the gel fraction of grafted polyethylene glycol oxide hydrogel increases with the increase of radiation dose, extremely
Being tending towards saturated behind the 80KGY, is 63.4% (Fig. 1) during the 40KGY radiation.
2, the hydrogel swelling degree increases with radiation dose and reduces, grafted polyethylene glycol oxide hydrogel swollen
Expansibility is 1310.1% when the 40KGY radiation, (Fig. 2).
3, the tensile strength of hydrogel reduces with the increase of radiation dose, and is grafted when the 40KGY radiation
The tensile strength of polyethylene glycol oxide hydrogel is up to 4.8MPa, (Fig. 3).
4, the elongation at break of hydrogel reduces with the radiation dose increase, when the 40KGY radiation, and grafting
The elongation at break of polyethylene glycol oxide hydrogel be 537%, (Fig. 4).
By the physicochemical property test result of above-mentioned hydrogel wound dressing as seen, radiation grafting the polyethylene glycol oxide hydrogel of polyvinyl alcohol gel fraction, swelling degree and elongation at break with appropriateness, especially has ideal mechanical strength, be the ideal wound dressing of handling various skin injurys, can partly or entirely replace traditional gauze dressing and heterogenous skin and transplant.
Claims (4)
1, a kind of method for radio-grafting of medical high molecular aquagel membrane is characterized in that: processing step is:
A, batching:
Polyethylene glycol oxide 6-24% weight (%)
Polyvinyl alcohol 2-12% weight (%)
Water 70-90% weight (%)
B, casting film: above-mentioned raw materials is mixed, heating for dissolving, making becomes the homogeneous mixture aqueous solution, will
Above-mentioned solution is poured Cheng Mo in the Flat bottom container of all size into, and make it cooling and solidify,
C, cold cycling treatment, the film that casting is good places circular treatment under the hot and cold different temperatures,
D, RADIATION PROCESSING:
Use electron accelerator to carry out the crosslinking with radiation grafting, close rate is 20kGy/ time, dosage 40-
60kGy, temperature 22-27 ℃,
E, sterilization 0-5 ℃ of preservation in back.
2, method according to claim 1 is characterized in that: the thickness of casting film is 1.5-2.0mm.
3, method according to claim 1 is characterized in that: cold cycling treatment low temperature is 0-5 ℃, and time 24-36 hour, the heat temperature was 22-27 ℃, and the time is 12-24 hour.
4, method according to claim 1 is characterized in that: irradiation processing uses cobalt-60 irradiation grafting crosslinked, and close rate is 10kGy/ hour, and dosage is 40-60kGy.
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| Application Number | Priority Date | Filing Date | Title |
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| CN98124925A CN1065771C (en) | 1998-11-17 | 1998-11-17 | Method for radio-grafting medical high molecular aquagel membrane |
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| Application Number | Priority Date | Filing Date | Title |
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| CN98124925A CN1065771C (en) | 1998-11-17 | 1998-11-17 | Method for radio-grafting medical high molecular aquagel membrane |
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| CN1065771C true CN1065771C (en) | 2001-05-16 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1093552C (en) * | 1998-12-30 | 2002-10-30 | 北京科技大学 | Preparation of hemicrystalline polyvinyl alcohol hydrogel |
| CN100390220C (en) * | 2005-08-26 | 2008-05-28 | 江苏恩华药业股份有限公司 | A hydrogel preparation method |
| CN101161696B (en) * | 2007-09-27 | 2010-06-02 | 北京师范大学 | Hydrogel and method for preparing same |
| CN101293110B (en) * | 2008-05-28 | 2013-10-23 | 苏州大学 | Medical hydrogel wound dressing and preparation method thereof |
| CN101518481B (en) * | 2009-03-20 | 2011-04-27 | 都本立 | Medical moisturized eye paste and method for preparing same |
| CN102634042A (en) * | 2012-04-20 | 2012-08-15 | 浙江大学 | PVA (polyvinyl alcohol) composite aquagel with bioactivity and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1067251A (en) * | 1991-05-25 | 1992-12-23 | 上海科学技术大学 | The synthetic method of chemicals slow-release type hydrogel film |
| CN1096307A (en) * | 1993-06-12 | 1994-12-14 | 中国药品生物制品检定所 | The preparation method of composite aquogel |
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1998
- 1998-11-17 CN CN98124925A patent/CN1065771C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1067251A (en) * | 1991-05-25 | 1992-12-23 | 上海科学技术大学 | The synthetic method of chemicals slow-release type hydrogel film |
| CN1096307A (en) * | 1993-06-12 | 1994-12-14 | 中国药品生物制品检定所 | The preparation method of composite aquogel |
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