CN101337086A - Hydrogel dressing and preparation method thereof - Google Patents
Hydrogel dressing and preparation method thereof Download PDFInfo
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- CN101337086A CN101337086A CNA200710043427XA CN200710043427A CN101337086A CN 101337086 A CN101337086 A CN 101337086A CN A200710043427X A CNA200710043427X A CN A200710043427XA CN 200710043427 A CN200710043427 A CN 200710043427A CN 101337086 A CN101337086 A CN 101337086A
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Abstract
The invention discloses hydrogel dressing which is composed of an upper layer and a lower layer. The lower-layer hydrogel is prepared by utilizing freeze thawing radiation method, and the upper-layer hydrogel is prepared by utilizing the radiation method; both the layers of hydrogel contain water-soluble polymer, and solvent for the residual; wherein, the lower-layer hydrogel contains polyvinyl alcohol. The invention also discloses a hydrogel-dressing preparation method which comprises the following steps: after the deaeration treatment of the water-soluble polymer solution containing polyvinyl alcohol, the hydrogel is prepared by utilizing circulating frozen thawing method; the water-soluble polymer solution after the deaeration treatment is positioned on the hydrogel, and then irradiation is performed under the high-energy rays. The hydrogel dressing has not only excellent strength and toughness, but also high transparence and wound fluid absorption ability. Meanwhile, the hydrogel dressing requires no additional chemical cross-linking agent or initiating agent, medical adhesive, and no reinforcing layer, such as fiber fabrics and woven fabrics, the two layers can be bonded firmly, and the preparation and the disinfection can be finished synchronously.
Description
Technical field
The present invention relates to a kind of aerogel dressing and preparation method thereof.
Background technology
Since Britain scientist George doctor Winter in 1962 found that moist environment helps wound healing, various new-type dressing had obtained broad development, and aerogel dressing is exactly wherein very important a kind of.Studies show that in a large number aerogel dressing has obviously alleviating pain of air permeable humidity retaining, softness, and more can not destroy the advantages such as wound tissue that healed during change dressings, promoting aspect the wound healing special advantages is being arranged.
Chemical crosslink technique, circulating frozen melt method and radiation method is a hydrogel preparation method commonly used at present.Polyacrylic acid hydrogel by chemical crosslinking preparation when nineteen eighty-three by Geistlich﹠amp; Sons Co. commercialization.But the hydrogel of chemical crosslink technique preparation is remaining unreacted monomer, cross-linking agent and initiator etc. usually, needs complicated purification process to use.Freeze-thaw method is a kind of very effective method of being reported the earliest by Peppas for preparing polyvinyl alcohol (PVA) hydrogel.The hydrogel that this method makes has advantages such as good springiness and mechanical strength be big, but this swelling behavior degree is less and opaque, influences in the therapeutic process observation to wound.Crinis Carbonisatus such as scientist in Poland Rosiak in 1989 understand that radiation method prepares hydrogel wound dressing.Radiation method causes the crosslinked aerogel dressing that makes by high-energy radiation, and its process need not added harmful substances such as any chemical cross-linking agent and initiator, and product is pure, does not need extra purification process; Radiation can at room temperature be carried out, the reaction condition gentleness, and can be by control properties of product such as control radiation dose, close rates; Gel formation can carry out simultaneously with sterilization; Simple to operate, cost is low.The hydrogel that this method makes has swellbility preferably, but mechanical strength is less, and application is restricted.
For solving the low problem of hydrogel intensity that radiation method makes, Many researchers is devoted to develop the composite water gel dressing, and these dressing are composited by several parts such as ventilated membrane, non-woven fabrics or fabric, hydrogel, medical adhesives usually.Disclose a kind of polyvinyl alcohol, polyvinyl pyrrolidone and/or polyethylene glycol oxide hydrogel wound dressing of containing as CN1273128A, this dressing just is to use non-woven fabrics as supporting layer, adopts radiation method to prepare hydrogel; CN1044405 discloses and a kind ofly can absorb wound fluid, and can be with water transport to airborne binder, and it is to be the aerogel dressing of skeleton with fabric or non-woven fabrics; CN1616116A discloses a kind of preparation method that contains the aerogel dressing of radiation sensitive agent and be suitable for the suitability for industrialized production operation, this hydrogel is made up of components such as polyvinylpyrrolidone, polyvinyl alcohol, radiation sensitive agent, plasticizer, pH regulator agent, water, preparation method be with non-woven fabrics as supporting layer, adopt irradiation method to prepare hydrogel layer; CN1095916 and CN2292547 etc. adopt above mentality of designing.Though these hydrogels have strengthened the intensity of hydrogel to a certain extent, enhancement Layers such as employed fabric or non-woven fabrics are opaque materials, are unfavorable for observing the wound healing situation; Simultaneously since the hydrophilic of fabric and non-woven fabrics a little less than, and the sticking effect between the gel is less, if use medical adhesive then to make the preparation process complexity, has reduced the pliability of aerogel dressing simultaneously.
Summary of the invention
The objective of the invention is for intensity that solves existing hydrogel and the problem that swellability can not get both, and provide that a kind of intensity height, transparency are good, good permeability and absorb the strong aerogel dressing of wound sepage ability.
The objective of the invention is to be realized by following technical proposal: aerogel dressing of the present invention is by two-layer composition up and down, and the lower layer of water gel adopts the preparation of freeze thawing radiation method, and the upper water gel adopts the radiation method preparation; All for containing water-soluble polymer, surplus is a solvent to two-layer hydrogel; Wherein, the lower layer of water gel contains polyvinyl alcohol.
Wherein, that the thickness of the hydrogel layer of the hydrogel layer of described employing freeze-thaw method preparation and/or the preparation of employing radiation method is preferable is 0.2～5mm, and that better is 0.3～3mm, and that best is 0.4～2mm.
Wherein, described water-soluble polymer is preferable is in the synthetic polymer one or more, perhaps the mixture of one or more synthetic polymers and one or more natural polymers.What described synthetic polymer was preferable is as polyvinyl alcohol, polyvinyl pyrrolidone or poly(ethylene oxide); What natural polymer was preferable is water-soluble chitosan, carboxymethyl chitin, chitosan, water-soluble chitosan, carboxymethyl chitosan, carboxymethyl cellulose, agar or collagen.What the content of described water-soluble polymer was preferable is mass percent 5～20%, and better is mass percent 6～15%, and best is mass percent 7～12%.Solvent can be distilled water or normal saline.
Aerogel dressing of the present invention also can contain medicine.Described medicine is preferable is selected from antimicrobial drug (as tetracycline, hydroxyl tetracycline and gentamycin etc.), the painful medicine (as naproxen sodium salt and aspirin etc.) in antiinflammatory town and/or promotes the medicine (as the Yunnan BAIYAO etc.) of wound healing; Described content of medicines preferable for mass percent be 0.005～5%.Among the present invention, aerogel dressing Chinese medicine content refers to the concentration of the drug solution that gel soaks.
Another object of the present invention is the preparation method that discloses this aerogel dressing, it is characterized in that comprising the steps:
(1) water-soluble polymer solution that will contain polyvinyl alcohol melts by circulating frozen and makes hydrogel.
That wherein, the thickness of the described solution that contains water-soluble polymer is preferable is 0.2～5mm; Described circulating frozen melts the preferable parameter of handling: cryogenic temperature is-30～-18 ℃, and the time is 0.5～7 hour; Melt temperature is 20～40 ℃, and the time is 0.5～7 hour; What the number of times that the circulating frozen thawing is handled was preferable is 1～7 time.
(2) on this hydrogel, pour the solution of water-soluble polymer into, under high-energy ray, carry out irradiation, get final product.
Wherein, described high-energy ray can be selected for use
60Co gamma-radiation or high-power electron beam ray; When being
60During the Co gamma-radiation, irradiation carries out in oxygen-free environment, and needs the front and back inverting container so that irradiation dose is even in the irradiation process; When being high-energy electron beam irradiation, can directly the container that fills solution be put into irradiation under the electron beam, need not oxygen-free environment; That the dosage of irradiation is preferable is 15～70kGy.
Irradiation can directly seal preservation after finishing; Also can further prepare the aerogel dressing that contains medicine, method is: irradiation under aseptic condition, with gel swelling in containing the solution of medicine (concentration can be mass percent 0.005～10%), gets final product after finishing.The solution that contains medicine can be distilled water or the normal saline solution that contains medicine.After the swelling, can wipe the aerogel dressing surface solution, sealing, cryopreservation.
Agents useful for same of the present invention and raw material are all commercially available to be got.
Positive progressive effect of the present invention is: this bilayer aerogel dressing has merged the advantage that freeze-thaw method and irradiation method prepare hydrogel: freeze thawing radiation hydrogel layer not only has good intensity but also have extraordinary toughness, simultaneously because also have irradiation layer gel, so thickness can be less, keep higher transparency; Irradiation layer gel itself has good absorption wound sepage ability, and it is support with the freeze thawing hydrogel layer, has guaranteed double-deck hydrogel integral intensity.And, aerogel dressing of the present invention is because unique preparation process, combination between the double-deck gel is very firm, do not need to use extra medical adhesive, fabric or, enhancement Layer such as non-woven fabrics, avoided the shortcoming of existing composite water gel dressing.In addition, the aerogel dressing that contains medicine has preferably slow release put performance to medicine, thus accelerating wound.Preparation method of the present invention need not added any chemical cross-linking agent and initiator, and the preparation of hydrogel can be finished synchronously with sterilization, and easy and simple to handle, cost is low.
Description of drawings
The monolayer hydrogel that Fig. 1 makes for the freeze thawing irradiation method and the swellbility comparison diagram of double-deck hydrogel of the present invention.Wherein, FT+Irra.-30kGy refers to the monolayer hydrogel of irradiation 30kGy after the freeze thawing; FT+Irra.-30kGy-30kGy refers to that lower floor is irradiation 30kGy after the freeze thawing, and the upper strata is the double-deck hydrogel of an irradiation 30kGy.
The monolayer hydrogel that Fig. 2 makes for irradiation method and the elastic modelling quantity comparison diagram of double-deck hydrogel of the present invention.Wherein, the monolayer hydrogel makes for irradiation 30kGy, and the freeze thawing irradiation layer in the double-deck hydrogel of the present invention is to distinguish freeze thawing 2,4 and 6 times behind the irradiation 30kGy again.
The specific embodiment
Mode below by embodiment further specifies the present invention, but does not therefore limit the present invention among the described scope of embodiments.
Preparation contains the 15wt% polyvinyl alcohol water solution, and this solution goes to pour into behind the bubble and forms the thick solution layer of 1mm in the plastic culture dish, and circulating frozen melts (cryogenic temperature-20 ℃, time 7h 2 times; 25 ℃ of melt temperatures, time 7h); On this physical gel, pour 10wt% polyvinyl alcohol and 2wt% carboxymethyl cellulose then again into, form the thick solution layer of 1mm, this culture dish is put into hermetic container, behind the letting nitrogen in and deoxidizing
60Irradiation 70kGy in the Co source, irradiation carries out in oxygen-free environment, and upset solution gets final product the gel vacuum seal afterwards so that irradiation dose is even before and after in the irradiation process.
Preparation contains the mixed aqueous solution of 6wt% polyvinyl alcohol and 2wt% water-soluble chitosan, and this solution goes to pour into behind the bubble and forms the thick solution layer of 3mm in the plastic culture dish, and circulating frozen melts (cryogenic temperature-20 ℃, time 7h 1 time; 25 ℃ of melt temperatures, time 7h); On this physical gel, pour the mixed aqueous solution of 7wt% polyvinyl alcohol and 5wt% polyvinyl pyrrolidone then again into, form the thick solution layer of 3mm, this culture dish is put into hermetic container, behind the letting nitrogen in and deoxidizing
60Irradiation 70kGy in the Co source, irradiation carries out in oxygen-free environment, and upset solution gets final product the gel vacuum seal afterwards so that irradiation dose is even before and after in the irradiation process.
Preparation contains the mixed aqueous solution of 10wt% polyvinyl alcohol and 5wt% carboxymethyl chitosan, pours into after this solution goes to steep and forms the thick solution layer of 0.2mm in the plastic culture dish, and circulating frozen melts (cryogenic temperature-20 ℃, time 0.5h 7 times; 25 ℃ of melt temperatures, time 0.5h); On this physical gel, pour into more then and contain 9wt% poly(ethylene oxide) and 3wt% agar, form the thick solution layer of 0.4mm, irradiation 40kGy under high-power electron beam, take out, under aseptic condition, be soaked in 48h in the aspirin soln of 5wt% of 2 times of volumes, take out and wipe behind the surface solution the gel vacuum seal.
Preparation contains the mixed aqueous solution of 9wt% polyvinyl alcohol and 1wt% carboxymethyl cellulose, pours into after this solution goes to steep and forms the thick solution layer of 1mm in the plastic culture dish, and circulating frozen melts (cryogenic temperature-30 ℃, time 1.5h 3 times; 20 ℃ of melt temperatures, time 1.5h); On this physical gel, pour into more then and contain 7wt% polyvinyl pyrrolidone, 5wt% polyvinyl alcohol and 8wt% water-soluble chitosan solution, form the thick solution layer of 0.2mm, use electron accelerator irradiation 50kGy, take out, under aseptic condition, be soaked in 24h in the YUNNAN BAIYAO solution of the 2wt% of volume, take out and wipe behind the surface solution the gel vacuum seal.
Preparation contains the mixed aqueous solution of 7wt% polyvinyl alcohol, 5wt% polyvinyl pyrrolidone and 3wt% carboxymethyl chitin, and this solution goes to pour into behind the bubble and forms the thick solution layer of 1.5mm in the plastic culture dish, and circulating frozen melts (cryogenic temperature-18 ℃, time 3h 2 times; 40 ℃ of melt temperatures, time 3h); On this physical gel, pour into more then and contain 7wt% poly(ethylene oxide) and 2wt% collagen solution, form the thick solution layer of 5mm, this culture dish is put into hermetic container, behind the letting nitrogen in and deoxidizing
60Irradiation 15kGy in the Co source, irradiation carries out in oxygen-free environment, and upset solution takes out so that irradiation dose is even before and after in the irradiation process, and vacuum seal gets final product.
Preparation contains the mixed aqueous solution of 7wt% polyvinyl alcohol, 2wt% chitosan and 5wt% carboxymethyl chitosan, pours into after this solution goes to steep and forms the thick solution layer of 0.5mm in the plastic culture dish, and circulating frozen melts (cryogenic temperature-20 ℃, time 4h 6 times; 25 ℃ of melt temperatures, time 5h); On this physical gel, pour into more then and contain 3wt% polyvinyl pyrrolidone, 1wt% poly(ethylene oxide) and 1wt% carboxymethyl chitosan sugar juice, form the thick solution layer of 1mm, with this gel solution layer irradiation 25kGy under high-power electron beam, take out, under aseptic condition, be soaked in 24h in the gentamycin solution of 0.005wt% of 4 times of volumes, take out and wipe behind the surface solution the gel vacuum seal.
Effect embodiment
(1) preparation of hydrogel
Preparation contains the aqueous solutions of polymers of 7wt% polyvinyl alcohol and 3wt% water-soluble chitosan, and ultrasonic going poured in the container behind the bubble, forms the thick solution layer of 1mm, circulation difference freeze thaw is 2,4,6 times in the circulating frozen machine, cryogenic temperature is-18 ℃, and the time is 1.5h, and melt temperature is a room temperature, time is 1h, pours above-mentioned solution afterwards in the gel that makes into, forms the 1mm solution layer, put into the hermetic container that is full of nitrogen again, use gamma-ray irradiation 30kGy, take out sealing, cryopreservation afterwards.Irradiation 30kGy and freeze thawing 2, the 4 and 6 times hydrogel sample in contrast of irradiation 30kGy more respectively.
(2) test of hydrogel performance
The above-mentioned aerogel dressing that makes is carried out following performance test:
(a) intensity of the elastic modelling quantity of hydrogel-reaction water gel
Test condition: 25 ℃, strain is 0.2%, and shearing frequency is 1rad/s.
(b) swelling behavior degree
Test condition: temperature is a room temperature, swellbility=W
s/ W
d
W
sWeight when-hydrogel reaches swelling equilibrium; W
dThe weight of-dried hydrogel
(3) the results are shown in Figure 1 and Fig. 2, the meaning that identifies among the figure is as follows:
Irradiation 30kGy after the FT+Irra.-30kGy-freeze thawing;
FT+Irra.-30kGy-30kGy-lower floor is irradiation 30kGy after the freeze thawing, and the upper strata is an irradiation 30kGy.
The monolayer hydrogel that Fig. 1 makes for the freeze thawing irradiation method and the swellbility comparison diagram of double-deck hydrogel of the present invention.As seen from Figure 1, obviously the monolayer hydrogel than the preparation of freeze thawing radiation method is big for the swellbility of double-deck aerogel dressing.The monolayer hydrogel that Fig. 2 makes for irradiation method and the elastic modelling quantity comparison diagram of double-deck hydrogel of the present invention.Wherein, the monolayer hydrogel makes for irradiation 30kGy, and the freeze thawing irradiation layer in the double-deck hydrogel of the present invention is to distinguish freeze thawing 2,4 and 6 times behind the irradiation 30kGy again.Because the intensity of double-deck gel of the present invention is mainly by the decision of freeze thawing radiating layer, therefore, the intensity of the hydrogel layer for preparing with the freeze thawing radiation method characterizes the intensity of double-deck gel herein.As shown in Figure 2, the intensity of double-deck hydrogel is obviously greater than the intensity of the hydrogel of irradiation method preparation.
Claims (14)
1. aerogel dressing is characterized in that: it is by two-layer composition up and down, and the lower layer of water gel adopts the preparation of freeze thawing radiation method, and the upper water gel adopts the radiation method preparation; All for containing water-soluble polymer, surplus is a solvent to two-layer hydrogel; Wherein, the lower layer of water gel contains polyvinyl alcohol.
2. aerogel dressing as claimed in claim 1 is characterized in that: described water-soluble polymer is one or more in the synthetic polymer, perhaps the mixture of one or more synthetic polymers and one or more natural polymers.
3. aerogel dressing as claimed in claim 2 is characterized in that: described synthetic polymer is polyvinyl alcohol, polyvinyl pyrrolidone or poly(ethylene oxide); Described natural polymer is water-soluble chitosan, carboxymethyl chitin, chitosan, water-soluble chitosan, carboxymethyl chitosan, carboxymethyl cellulose, agar or collagen.
4. aerogel dressing as claimed in claim 1 is characterized in that: the content of described water-soluble polymer is mass percent 5～20%.
5. aerogel dressing as claimed in claim 1 is characterized in that: the thickness of described upper water gel and/or lower layer of water gel is 0.2～5mm.
6. aerogel dressing as claimed in claim 1 is characterized in that: described aerogel dressing also contains medicine.
7. aerogel dressing as claimed in claim 6 is characterized in that: described medicine is one or more in painful medicine in antimicrobial drug, antiinflammatory town and the medicine that promotes wound healing.
8. aerogel dressing as claimed in claim 6 is characterized in that: described content of medicines is a mass percent 0.005～5%.
9. the preparation method of aerogel dressing as claimed in claim 1 is characterized in that comprising the steps:
(1) water-soluble polymer solution that will contain polyvinyl alcohol adopts circulating frozen to melt legal system and gets hydrogel after deaeration is handled;
(2) at the water-soluble polymer solution of pouring on this hydrogel after deaeration is handled, under high-energy ray, carry out irradiation, get final product.
10. method as claimed in claim 9 is characterized in that: in step (1) and/or the step (2), the thickness of described solution is 0.2～5mm.
11. method as claimed in claim 9 is characterized in that: in the step (1), it is-30～-18 ℃ that described circulating frozen melts the cryogenic temperature of handling, and the time is 0.5～7 hour; Melt temperature is 20～40 ℃, and the time is 0.5～7 hour; It is 1～7 time that circulating frozen melts the number of times of handling.
12. method as claimed in claim 9 is characterized in that: in the step (2), described high-energy ray is
60Co gamma-radiation or high-power electron beam ray; When being
60During the Co gamma-radiation, irradiation carries out in oxygen-free environment, and the solution that overturns before and after in the irradiation process is so that irradiation dose is even.
13. method as claimed in claim 9 is characterized in that: in the step (2), the dosage of described irradiation is 15-70kGy.
14. method as claimed in claim 9 is characterized in that: irradiation under the aseptic condition, carries out swelling after finishing in containing the solution of medicine, can make the aerogel dressing that contains medicine.
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