CN109806439A - A kind of class aquogel type compound film dressing and preparation method thereof based on alginate - Google Patents
A kind of class aquogel type compound film dressing and preparation method thereof based on alginate Download PDFInfo
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Abstract
The present invention relates to a kind of class aquogel type compound film dressing and preparation method thereof based on alginate, belongs to medical products technical field.The present invention selects sodium alginate, carboxymethyl chitosan and bivalent cation (strontium ion and/or zinc ion) isoreactivity ion as raw material, through being swollen ingredient, air-dry film forming, ionomer etc. generates three-dimensional porous structure, and finally freeze-drying obtains the compound film dressing of biologically active class hydrogel structure.Compound film dressing of the invention is the dressing of external application laminated film; with good water suction performance of keeping humidity, toughness, degradability and good biocompatibility and bioactivity; be primarily adapted for use in skin surface wound such as scratch, scald, cut wound; it shields to the skin wound of the wounded; and play the role of analgesia, anti-inflammatory, debridement, promote growth factor synthesis, promote wound healing, improve wound repair quality, also it is used in the Wound treatment that position is wrapped up after performing the operation.
Description
Technical field
The invention belongs to medical products technical field, be related to a kind of class aquogel type compound film dressing based on alginate and
Preparation method.
Background technique
Dressing is to handle most general one of the mode of wound.The mechanical property protection wound that ideal dressing needs to have certain
Mouthful, good hygroscopicity absorbs the diffusate of wound, and certain penetrability prevents the surface of a wound is dry from preventing from creating with excellent antibiotic property
Face infection.Particularly, the dressing in forward position needs to have good bioactivity, for example can promote revascularization, cell adherence
With proliferation etc., to promote wound healing.
Alginate dressing is widely used in wound healing neck since it is with good hygroscopicity and biocompatibility
Domain.Alginates can be changed into hydrogel with cross-linked bivalent cation, make it have the tridimensional network of class extracellular matrix, tool
There is good sucting wet air permeability.Now using most wide for calcium ion crosslinking alginate dressing, due to its good mechanical property
Matter, but such dressing does not have good bioactivity.
Therefore, it is very necessary for assigning the good bioactivity of alginate dressing.Material bioactivity is assigned now
Method is mostly to add bioactive substance, for example add some drugs, growth factor, the substances such as antibacterial agent.But this method
Body would generally be damaged because sustained release is undesirable, and because of the using effect of active material inactivation material.And it lives
Property ion, such as strontium ion and zinc ion have good stability, and can pass through alginates cross-linked bivalent cation
Ability is in conjunction with dressing, the problem of effective solution sustained release is unstable, and active material inactivates.Strontium ion be it is a kind of activity from
Son can promote the regeneration of blood vessel；Zinc ion is also the synthesis that a kind of active ion can participate in body zinc lipoprotein, and the two can
To effectively promote wound healing.And sodium alginate and carboxymethyl chitosan will form inierpeneirating network structure, dry by freezing
The film with class hydrogel structure is formd after dry.
Therefore, the present invention is by using strontium ion and the compound freeze-drying film of zinc ion crosslinked alginate/carboxymethyl chitosan,
Dressing bioactivity is imparted, and optimizes the structure of dressing.
Summary of the invention
In view of this, one of the objects of the present invention is to provide a kind of, the class aquogel type composite membrane based on alginate is applied
Material, the second object of the present invention are to provide a kind of preparation method of class aquogel type compound film dressing based on alginate.
In order to achieve the above objectives, the invention provides the following technical scheme:
1, a kind of class aquogel type compound film dressing based on alginate, the compound film dressing include alginate,
Carboxymethyl chitosan, bioactive ions and water.
Preferably, the water is deionized water.
Preferably, the bioactive ions are at least one of strontium ion or zinc ion.
Preferably, the alginate is sodium alginate.
Preferably, the mass-volume concentration of the alginate is 0.5~2%, the mass body of the carboxymethyl chitosan
Product concentration is 1~3%, and the unit of the mass-volume concentration is g/v.
Preferably, the molar concentration of the zinc ion is 0.3~1.18mM, the molar concentration of the strontium ion is 7.5~
75mM。
2, the preparation method of above-mentioned a kind of class aquogel type compound film dressing based on alginate, the preparation method packet
Include following steps:
(1) preparation of reaction solution: taking water as a solvent, and carboxymethyl chitosan and alginate is added, and stirs to transparent uniform
Afterwards and 6~8h degassing is placed, obtains SA/CMCH mixed solution；
(2) membranae praeformativa: by 20mL step (1)) obtained in SA/CMCH mixed solution be layered on the polyethylene culture dish of 90mm
In, in 40 DEG C of dry 8~12h, obtain the composite membrane of SA/CMCH interpenetrating polymer networks structure；
(3) configuration of living solution: choosing at least one of strontium ion or zinc ion is bioactive ions, with water
Bioactive ions solution is configured for solvent；
(4) active ion is crosslinked: active ion crosslinking: the SA/CMCH interpenetrating polymer networks knot that will be prepared in step (2)
It is crosslinked in the smooth active ion solution being placed in step 3) of the composite membrane of structure, the composite membrane after being crosslinked；
(5) it freeze-drying molding: is freeze-dried again after the composite membrane after crosslinking in step (4) is first freezed
Obtain a kind of class aquogel type compound film dressing based on alginate.
Preferably, the mass-volume concentration of carboxymethyl chitosan in deionized water described in step (1) is 0.5~2%,
The alginate is sodium alginate, and the mass-volume concentration of the sodium alginate in deionized water is 1~3%.
Preferably, the molar concentration of zinc ion described in step (2) is 0.3~1.18mM, the strontium ion it is mole dense
Degree is 7.5~75mM.
Preferably, the time of crosslinking described in step (4) is 40~60min.
Preferably, the temperature that progress is freezed described in step (5) is -20 DEG C, and the time of freezing is 3h.
Preferably, freeze-drying described in step (5) carries out in freeze drier, and the time of the freeze-drying is 6
~12h.
The beneficial effects of the present invention are:
1, the invention discloses a kind of class aquogel type compound film dressing based on alginate, the compound film dressing tool
There is the tridimensional network of hydrogel, impart the good sucting wet air permeability of material, and to impart material good for double ion crosslinking
Good bioactivity has very big development potentiality in art of wound dressings；
2, compound film dressing of the invention is the dressing of external application laminated film, has good water suction performance of keeping humidity, toughness, drop
Solution property and good biocompatibility and bioactivity, be primarily adapted for use in skin surface wound such as scratch, scald, cut wound,
Shield to the skin wound of the wounded, and have analgesia, anti-inflammatory, debridement, promote growth factor synthesis, promote wound healing,
The effect for improving wound repair quality is also used in the Wound treatment at wrapping position after operation；
3, the preparation method of the invention also discloses a kind of class aquogel type compound film dressing based on alginate utilizes
The method of alginate cross-linked bivalent cationic (strontium ion and zinc ion) assigns alginate dressing bioactivity, using preparatory
Film forming is crosslinked again, is had the three-dimensional netted structure of class hydrogel finally by film made from freeze-drying, is improved thin
The water imbibition and penetrability of film dressing, while having the easy to operate of preparation method, it is excellent that reaction condition is mild and at low cost etc.
Point.
Other advantages, target and feature of the invention will be illustrated in the following description to a certain extent, and
And to a certain extent, based on will be apparent to those skilled in the art to investigating hereafter, Huo Zheke
To be instructed from the practice of the present invention.Target of the invention and other advantages can be realized by following specification and
It obtains.
Detailed description of the invention
To make the objectives, technical solutions, and advantages of the present invention clearer, the present invention is made below in conjunction with attached drawing excellent
The detailed description of choosing, in which:
The class aquogel type based on alginate that Fig. 1, which is 1 strontium ion concentration of the embodiment of the present invention, to be prepared when being 7.5mM is multiple
Close the scanning electron microscope (SEM) photograph of film dressing.
The class aquogel type based on alginate that Fig. 2 is prepared when being 1 strontium ion concentration 15mM of the embodiment of the present invention is compound
The scanning electron microscope (SEM) photograph of film dressing.
The class aquogel type based on alginate that Fig. 3 is prepared when being 1 strontium ion concentration 30mM of the embodiment of the present invention is compound
The scanning electron microscope (SEM) photograph of film dressing.
The class aquogel type based on alginate that Fig. 4 is prepared when being 1 strontium ion concentration 45mM of the embodiment of the present invention is compound
The scanning electron microscope (SEM) photograph of film dressing.
The class aquogel type based on alginate that Fig. 5 is prepared when being 1 strontium ion concentration 75mM of the embodiment of the present invention is compound
The scanning electron microscope (SEM) photograph of film dressing.
Fig. 6 is the class aquogel type composite membrane based on alginate of the different strontium ion concentration preparations of the embodiment of the present invention 1
The pore analysis histogram of dressing.
Fig. 7 is the class aquogel type composite membrane based on alginate of the different strontium ion concentration preparations of the embodiment of the present invention 1
The evaluation of the swellbility of dressing.
Fig. 8 is the class aquogel type composite membrane based on alginate of the different zinc ion concentration preparations of the embodiment of the present invention 3
The Cytotoxic evaluation of dressing.
Fig. 9 is the wound healing situation of 4 blank elements of the embodiment of the present invention.
Figure 10 is that strontium ion concentration is that the class aquogel type based on alginate of 45mM preparation is multiple in the embodiment of the present invention 1
Close the wound healing situation of film dressing.
Figure 11 is the wound healing situation of 4 double ion crosslinked film of the embodiment of the present invention.
Specific embodiment
Illustrate embodiments of the present invention below by way of specific specific example, those skilled in the art can be by this specification
Other advantages and efficacy of the present invention can be easily understood for disclosed content.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints and application, without departing from
Various modifications or alterations are carried out under spirit of the invention.It should be noted that diagram provided in following embodiment is only to show
Meaning mode illustrates basic conception of the invention, and in the absence of conflict, the feature in following embodiment and embodiment can phase
Mutually combination.
Wherein, the drawings are for illustrative purposes only and are merely schematic diagrams, rather than pictorial diagram, should not be understood as to this
The limitation of invention；Embodiment in order to better illustrate the present invention, the certain components of attached drawing have omission, zoom in or out, not
Represent the size of actual product；It will be understood by those skilled in the art that certain known features and its explanation may be omitted and be in attached drawing
It is understood that.
Embodiment 1
A kind of preparation method of the class aquogel type compound film dressing based on alginate, comprising the following steps:
(1) mixed solution of configuration quality volume (g/v) concentration is 2% carboxymethyl chitosan and 1% sodium alginate, is stirred
It mixes to transparent uniform, and places 8h degassing, obtain SA/CMCH mixed solution；
(2) mixed solution in 20mL step (1) is layered in the polyethylene culture dish of 90mm, in 40 DEG C of dry 12h, is obtained
To the composite membrane of SA/CMCH interpenetrating polymer networks structure (INPs)；
(3) the strontium ion solution that 7.5mM is configured using deionized water as solvent, is stirred uniform；
(4) by the composite membrane of SA/CMCH interpenetrating polymer networks structure (INPs), smooth is placed in 20mL step (3)
7.5mM strontium ion solution in 40min, completed wait be crosslinked, composite membrane after being crosslinked；
(5) composite membrane after the crosslinking in step 4) is placed in -20 DEG C of freezing 3h, is put into freeze drier 6h later,
Obtain a kind of class aquogel type compound film dressing based on alginate.
In addition change the concentration for preparing strontium ion solution, its concentration is made to be respectively 15mM, 30mM, 45mM and 75mM, then
It is crosslinked with the composite membrane of SA/CMCH interpenetrating polymer networks structure (INPs), obtains being formed by different strontium ion concentration
Class aquogel type compound film dressing based on alginate, SEM scheme as shown in Fig. 1~5: when strontium ion concentration for 7.5mM~
When 15mM, the membrane structure of the compound film dressing formed is loose, and hole diameter is big (as shown in Figures 1 and 2)；When strontium ion is dense
When degree is 30mM~45mM, the membrane structure of the compound film dressing formed is close, and hole diameter is small (as shown in Figure 3 and Figure 4)；
When strontium ion concentration is 75mM, the membrane structure and 45mM strontium ion cross linking membrane of the compound film dressing formed become without obvious
Change, but the surface of its compound film dressing formed can cover a tunic because being crosslinked excessively, as shown in Figure 5.It can be seen that one
The pore size of class aquogel type compound film dressing of the kind based on alginate is gradually reduced with the increase of strontium ion concentration,
When concentration is more than 45mM, pore size is without significant change (as shown in Figure 6).
To preparing the class aquogel type compound film dressing based on alginate formed by the strontium ion solution of various concentration
Swellbility evaluation is carried out, its water absorbing properties is studied.Dressing is cut into the square disk of 1cm × 1cm, after moisture equilibrium at dry side, meter
Calculate the swellbility of dressing.Experimental result is as shown in fig. 7, illustrate the class aquogel type compound film dressing based on alginate with good
Good hygroscopicity, with the increase of cross-linking ion concentration, the swellbility of dressing is gradually reduced, but when strontium ion concentration is 45mM
When, swellbility can also be of about 1000%.
Embodiment 2
A kind of preparation method of the class aquogel type compound film dressing based on alginate, comprising the following steps:
(1) mixed solution of configuration quality volume (g/v) concentration is 1% carboxymethyl chitosan and 2% sodium alginate, is stirred
It mixes to transparent uniform, and places 6h degassing, obtain SA/CMCH mixed solution；
(2) mixed solution in 20mL step (1) is layered in the polyethylene culture dish of 90mm, in 40 DEG C of dry 8h, is obtained
To the composite membrane of SA/CMCH interpenetrating polymer networks structure (INPs)；
(3) the zinc ion solution that 0.3mM is configured using deionized water as solvent, is stirred uniform；
(4) by the composite membrane of SA/CMCH interpenetrating polymer networks structure (INPs), smooth is placed in 20mL step (3)
0.3mM strontium ion solution in 40min, completed wait be crosslinked, composite membrane after being crosslinked；
(5) composite membrane after the crosslinking in step 4) is placed in -20 DEG C of freezing 3h, is put into freeze drier 6h later,
Obtain a kind of class aquogel type compound film dressing based on alginate.
Further according to identical preparation flow, only change the concentration for preparing zinc ion solution, makes its concentration be respectively
0.5mM, 0.8mM, 1.0mM and 1.18mM, then handed over the composite membrane of SA/CMCH interpenetrating polymer networks structure (INPs)
Connection, obtains the class aquogel type compound film dressing based on alginate formed by different zinc ion concentrations.
The results showed that is be prepared is compound when using the strontium ion concentration crosslinked film of 0.3~1.18mM as template
Film dressing has good cell adherence and proliferative capacity.When zinc ion concentration is in 0.3~0.74mM, material is shown well
Promotion cell Proliferation effect, especially when zinc ion concentration be 0.74mM, promote cell Proliferation effect it is most obvious.
Embodiment 3
A kind of preparation method of the class aquogel type compound film dressing based on alginate, comprising the following steps:
(1) carboxymethyl chitosan and quality volume (g/v) concentration that configuration quality volume (g/v) concentration is 2% are 1%
The mixed solution of sodium alginate, stirring place 6h degassing to transparent uniform, obtain SA/CMCH mixed solution；
(2) mixed solution in 20mL step 1) is layered in the polyethylene culture dish of 90mm, in 40 DEG C of dry 8h, is obtained
The composite membrane of SA/CMCH interpenetrating polymer networks structure (INPs)；
(3) mixed solution containing 45mM strontium ion and 0.30mM zinc ion is configured, is stirred uniform；
(4) by the composite membrane of SA/CMCH interpenetrating polymer networks structure (INPs), smooth is placed in 20mL step 3)
1h in mixed solution, is completed wait be crosslinked, the composite membrane after being crosslinked；
(5) composite membrane after the crosslinking in step 4) is placed in -20 DEG C of freezing 3h, is put into freeze drier 12h later,
Obtain a kind of film-type dressing of biologically active class hydrogel structure；
(6) material is cut into the disk of 1.4cm × 1.4cm, is placed in 24 orifice plates, ultraviolet sterilization 1h；
It (7) is 1 × 10 by concentration4The L929 cell inoculation of cells/mL is in above-mentioned material, to 1-3 day cell of culture
MTS experiment is carried out, the hole of no film is as blank control group (ctr).
In addition change prepare zinc ion solution concentration, make its concentration be respectively 0.3mM, 0.44mM, 0.74mM and
1.18mM, then be crosslinked with the composite membrane of SA/CMCH interpenetrating polymer networks structure (INPs), it obtains dense by different zinc ions
Spend the class aquogel type compound film dressing based on alginate formed
The results showed that when using the strontium ion concentration crosslinked film of 45mM as template, the compound film dressing that is prepared
With good cell adherence and proliferative capacity.When zinc ion concentration is in 1.18mM, material shows apparent toxicity, still
In 1.18mM or less, the effect for promoting cell Proliferation is shown, especially when zinc ion concentration is 0.74mM, promotion cell increases
It is most obvious (as shown in Figure 8) to grow effect.
Embodiment 4
A kind of preparation method of the class aquogel type compound film dressing based on alginate, comprising the following steps:
(1) configuration quality volume (g/v) concentration is for 3.0% carboxymethyl chitosan and quality volume (g/v) concentration
The mixed solution of 0.5% sodium alginate, stirring place 7h degassing to transparent uniform, obtain SA/CMCH mixed solution；
(2) membranae praeformativa: by 20mL step (1)) obtained in SA/CMCH mixed solution be layered on the polyethylene culture dish of 90mm
In, in 40 DEG C of dry 10h, obtain the composite membrane of SA/CMCH interpenetrating polymer networks structure；
(3) configuration of living solution: any one chosen in strontium ion and zinc ion is bioactive ions, with go from
Sub- water is that solvent configures bioactive ions solution, and wherein the concentration of strontium ion is 45mM, and the concentration of zinc ion is 0.74mM；
(4) active ion is crosslinked: the composite membrane of the SA/CMCH interpenetrating polymer networks structure prepared in step (2) is flat
Crosslinking 50min, the composite membrane after being crosslinked are carried out in the whole active ion solution being placed in 20mL step (3)；
(5) freeze-drying molding: the composite membrane after crosslinking in step (4) is placed at -20 DEG C after freezing 3h and is put into freezing
Freeze-drying 8h is carried out in drying machine, and a kind of class aquogel type compound film dressing based on alginate can be obtained.
Dressing is studied to the Wound Healing of rabbit full thickness skin excision model: rabbit full thickness skin cuts off model experiment: choosing
2kg or so 3 months or so big rabbits are taken to be tested, all experiments aseptically carry out.Take intraperitoneal injection chlorine
Amine ketone (0.1mg/kg) is anaesthetized, and the hair at rabbit back is cut, and with alcohol and iodine disinfection, cuts off the circle of 1.5cm diameter
Full thickness skin is handled with strontium ion cross linking membrane, strontium ion and zinc ion cross linking membrane and blank respectively, and observation wound is cured within 15 days
Close situation.
The results showed that in the excision experiment of rabbit full thickness skin, compared to blank group, containing strontium ion, zinc ion or
Person's strontium ion and the cross linking membrane of zinc ion mixing possess more preferable faster wound-healing abilities, can promote the recovery of wound (such as
Shown in Fig. 9-11).
Finally, it is stated that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to compared with
Good embodiment describes the invention in detail, those skilled in the art should understand that, it can be to skill of the invention
Art scheme is modified or replaced equivalently, and without departing from the objective and range of the technical program, should all be covered in the present invention
Scope of the claims in.
Claims (10)
1. a kind of class aquogel type compound film dressing based on alginate, which is characterized in that the compound film dressing includes sea
Alginates, carboxymethyl chitosan, bioactive ions and water.
2. a kind of class aquogel type compound film dressing based on alginate according to claim 1, which is characterized in that described
Bioactive ions are at least one of strontium ion or zinc ion.
3. a kind of class aquogel type compound film dressing based on alginate according to claim 1, which is characterized in that described
Alginate is sodium alginate.
4. a kind of class aquogel type compound film dressing based on alginate according to claim 1, which is characterized in that described
The mass-volume concentration of alginate is 0.5~2%, and the mass-volume concentration of the carboxymethyl chitosan is 1~3%, described
The unit of mass-volume concentration is g/v.
5. a kind of class aquogel type compound film dressing based on alginate according to claim 2, which is characterized in that described
The molar concentration of zinc ion is 0.3~1.18mM, and the molar concentration of the strontium ion is 7.5~75mM.
6. a kind of any one of Claims 1 to 5 preparation method of the class aquogel type compound film dressing based on alginate,
It is characterized in that, the preparation method comprises the following steps:
(1) preparation of reaction solution: to go water as solvent, being added carboxymethyl chitosan and alginate, stirring to it is transparent it is uniform after
And 6~8h degassing is placed, obtain SA/CMCH mixed solution；
(2) membranae praeformativa: SA/CMCH mixed solution obtained in 20mL step (1) is layered in polyethylene culture dish, dry 8~
12h obtains the composite membrane of SA/CMCH interpenetrating polymer networks structure；
(3) configuration of living solution: choosing at least one of strontium ion or zinc ion is bioactive ions, is molten with water
Agent configures bioactive ions solution；
(4) active ion is crosslinked: the composite membrane of the SA/CMCH interpenetrating polymer networks structure prepared in step (2) is smooth
It is crosslinked in the active ion solution being placed in step (3), the composite membrane after being crosslinked；
(5) it freeze-drying molding: is freeze-dried, can be obtained again after the composite membrane after crosslinking in step (4) is first freezed
A kind of class aquogel type compound film dressing based on alginate.
7. a kind of preparation method of the class aquogel type compound film dressing based on alginate according to claim 6, special
Sign is that the mass-volume concentration of carboxymethyl chitosan in water described in step (1) is 1~3%, and the alginate is sea
Mosanom, the mass-volume concentration of the sodium alginate in deionized water are 0.5~2%, the list of the mass-volume concentration
Position is g/v.
8. a kind of preparation method of the class aquogel type compound film dressing based on alginate according to claim 6, special
Sign is, the molar concentration of zinc ion described in step (2) is 0.3~1.18mM, the molar concentration of the strontium ion is 7.5~
75mM。
9. a kind of preparation method of the class aquogel type compound film dressing based on alginate according to claim 6, special
Sign is that the time of crosslinking described in step (4) is 40~60min.
10. a kind of preparation method of the class aquogel type compound film dressing based on alginate according to claim 6, special
Sign is that the temperature that progress is freezed described in step (5) is -20 DEG C, and the time of freezing is 3h；The freeze-drying is dry in freezing
It is carried out in dry machine, the time of the freeze-drying is 6~12h.
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| CN113336974A (en) * | 2021-07-21 | 2021-09-03 | 浙江大学 | Easily degradable histidine-based coordination hydrogel with fluidity and preparation method and application thereof |
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