CN109276745A - A kind of cellulose combine dressing of high wet strength and preparation method thereof - Google Patents

A kind of cellulose combine dressing of high wet strength and preparation method thereof Download PDF

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Publication number
CN109276745A
CN109276745A CN201811495331.1A CN201811495331A CN109276745A CN 109276745 A CN109276745 A CN 109276745A CN 201811495331 A CN201811495331 A CN 201811495331A CN 109276745 A CN109276745 A CN 109276745A
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China
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cellulose
aqueous solution
dressing
wet strength
high wet
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Chinese (zh)
Inventor
迟少萍
盛励斌
隋纹龙
李重标
朱亮
张鹏
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SHANGHAI XINHUA RUISI MEDICAL SCIENCE & TECHNOLOGY Co Ltd
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SHANGHAI XINHUA RUISI MEDICAL SCIENCE & TECHNOLOGY Co Ltd
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Priority to CN201811495331.1A priority Critical patent/CN109276745A/en
Publication of CN109276745A publication Critical patent/CN109276745A/en
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L15/00Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/22Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
    • A61L15/28Polysaccharides or their derivatives
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L15/00Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/40Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing ingredients of undetermined constitution or reaction products thereof, e.g. plant or animal extracts
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L15/00Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/42Use of materials characterised by their function or physical properties
    • A61L15/425Porous materials, e.g. foams or sponges

Abstract

The invention discloses a kind of cellulose combine dressing of high wet strength, the dressing is from top to bottom respectively cellulose sponge layer, sterile gauze layer, cellulose sponge layer;The cellulose sponge layer is made using cellulose and its derivates aqueous solution, acidic aqueous solution or alkaline aqueous solution, crosslinking agent mixing crosslinking;The dressing is in spongy.In addition, including the following steps: to be sequentially added into acidic aqueous solution or alkaline aqueous solution in the aqueous solution of cellulose and its derivates the invention also discloses the preparation method of the cellulose combine dressing of the high wet strength, crosslinking agent, water-bath cross-linking reaction is carried out;By sterile gauze single berth on mold, crosslinker solution progress pre-freeze is poured into, freeze-drying obtains combination product;Combination product is cut, is dispensed, sterilize to get.The present invention efficiently solves the insufficient defect of bio-sponge mechanical property, and effectively reduces cost;The flexibility and water imbibition of cellulosic material are remained, and significantly improves product wet strength.

Description

A kind of cellulose combine dressing of high wet strength and preparation method thereof
Technical field
The present invention relates to biomedical materials fields, the porous absorbent dressing suitable for body surface for hemostasis, especially It is related to a kind of cellulose combine dressing of high wet strength;Moreover, it relates to the preparation side of the cellulose combine dressing Method.
Background technique
Chronic wounds, as venous congestion ulcer, pressure ulcer, diabetic foot ulcers and other chronic ulcers are hurt Mouthful, including cave type or umbilicate type ulcer wound, a large amount of diffusates can be generated in agglutination, some wounds can be at 24 hours Interior exudation is up to the diffusate of 50ml.Therefore the dressing with high liquid absorption amount is needed to absorb diffusate, clinically to prevent bacterium It breeds and infects, the most ideal situation is that after wound dressing absorbs diffusate, it can be by full wafer for the surface wound of large area Removal, and then can entirely taking away for chamber hole type wound, while wet strength is lower after will not absorbing diffusate because of wound dressing And it is damaged.In general wound dressing of the wet strength lower than 0.1N/cm cracky in removal process, to aggravate wound care The degree of difficulty of work, or even the possibility for having damaged wound dressing to remain in wound surface, can cause wound and surrounding skin Accompanying infection.
In recent years, with the further investigation of biomedical material, people increasingly pay attention to the safety of nursing class product, It is required that it is also higher and higher, it can such as be absorbed degradation with the contact material of the surface of a wound, can be metabolized in vivo, is non-toxic, it is clinical right The demand of biological species material is very vigorous, but biological species material have the defects that one it is common be exactly that mechanical strength is poor, replacement of products Fracture is easily caused in the process.
Aquacel wound dressing is most common Wound care dressing, and products characteristics are as follows: 1) having very strong suction Receipts ability, imbibition rate are up to 15 times of own wt;2) clear gel is formed after absorbent solution;3) there is lower lateral hair Thin characteristic;4) in absorbing wound exudate after-contraction.Afterwards two for chronic wounds processing it is especially important, at chronic wounds In reason mostly undesired situation first is that the dipping of wound fluid, i.e. wound fluid bleed around until periphery healthy skin Skin, dipping is likely to result in the infection or damage of periphery healthy skin frequent occurrence.Most of other kinds of wound dressings Wound fluid can be caused to spread to the healthy skin of surrounding due to lateral capillarity, but there is low-down lateral capillary Characteristic, it is possible to reduce the generation of such case.In addition, reducing after water suction, this will reduce the weight of the skin and wound dressing of surrounding A possibility that folding, further reduced dipping.Another is plastic in the advantages of clinical application, during wound healing, wound The few fibers of dressing " are sticked to " on wound sometimes and are not easy to remove.Using plastic characteristic, can first be soaked with physiological saline deposited Expect the fiber plastic after-tack for making these " viscous " on wound or washed away by physiological saline, so that wound removal be made no longer to be one The process of pain, improves the quality of life of patient during wound care.
The structure of existing wound dressing generally uses whole spongelike structure, but it has following defects that polymeric hydantoin Continuous (polyvinyl alcohol, polyurethane etc.) because its hardness is relatively high, brittleness is larger, is not suitable for winding and uses;Bio-sponge (gelatin sea Silk floss, collagen protein sponge, chitosan etc.) because of its preparation process complexity, so production higher cost, and it is used alone Poor mechanical property, nursing process are easily broken off, so clinic needs a kind of i.e. economical and practical and mechanical strength higher while flexible The preferable sponge dressing of property.
Chinese utility model patent CN201520871794 discloses a kind of dedicated wrapping dressing of limbs war wound emergency treatment, specially Sharp product design mainly solves the case where war wound emergency treatment big bleeding, and major function design inclination is in quick-acting haemostatic powder, quick drainage, The big feature of liquid absorption amount, the polyvinyl formal spongy layer that middle layer uses, major function are exactly imbibition expansion while oppressing Hemostasis, but the generally existing hardness of macromolecule sponge is high, the feature of flexibility difference, so the design of middle layer macromolecule sponge will lead to Entire product applicating property is poor.
Chinese invention patent application CN201711166122.8 discloses a kind of biologically active composite sponge auxiliary material And the preparation method and application thereof.Its object is to develop a kind of cellulose casting product of promoting healing, by adding γ-polyglutamic Acid and epoxychloropropane are reacted, and wherein experimental example can clearly find out the addition with gamma-polyglutamic acid, promoting healing effect Fruit is obvious, and the effect of gamma-polyglutamic acid additive is promoting healing, but due to gamma-polyglutamic acid and epichlorohydrin crosslinker, It uses toxicologic study still immature in human body, so to develop into medical supplies, still needs to carry out material toxicity, internal generation It thanks, the further research such as carcinogenicity.And it is using traditional whole spongelike structure, however it remains poor mechanical property, The problems such as nursing process is easily broken off.
United States Patent (USP) US3096228 discloses a kind of method of reinforcing fiber product wet strength.It is in cellulose fibre A kind of reagent for being named as glyoxal is introduced, cellulosic molecule can be made more closely with the radical polymerisations such as the hydroxyl of cellulose, crosslinking It links together, so as to while keeping this substance high-hygroscopicity and at colloidality, keep higher wet strong Degree.However the glyoxal toxicity of this method addition is higher.
Therefore, so far, it is still necessary to which developing a kind of highly-safe can either have absorbability and gelation and can also It is enough that the wound dressing of bigger wet strength is provided.
Summary of the invention
One of the technical problem to be solved in the present invention is to provide a kind of high humidity strength element combine dressing, effectively solve Bio-sponge mechanical property insufficient defect, and effectively reduce cost;Retain the comfort of cellulose material itself and soft It is soft, while increasing gelation and high wet strength of the product in use process, enhance clinical applicability, such as the burning of large area When scald and chronic wounds processing, removing for full wafer is may be implemented in when dressing, brings convenience to nursing, while product gelation can The secondary damage to wound is avoided, and highly-safe.
The second technical problem to be solved by the present invention is to provide a kind of preparation side of high humidity strength element combine dressing Method, this method simple process, easy to operate, feasibility is strong.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is that:
In one aspect of the invention, a kind of cellulose combine dressing of high wet strength is provided, the dressing is from top to bottom distinguished For cellulose sponge layer, sterile gauze layer, cellulose sponge layer;The cellulose sponge layer uses cellulose and its derivates water Solution, acidic aqueous solution or alkaline aqueous solution, crosslinking agent mixing crosslinking are made;The dressing is in spongy.
As currently preferred technical solution, the dressing is from top to bottom respectively the cellulose sponge of 1-4cm thickness The cellulose sponge layer of layer, the sterile gauze layer of 0.01mm thickness, 1-4cm thickness.
As currently preferred technical solution, the porosity of the cellulose sponge layer reaches 80% or more, and micropore is big Small is 10-50 μm.
In another aspect of this invention, a kind of preparation method of the cellulose combine dressing of high wet strength is provided, including such as Lower step:
(1) certain density cellulose and its derivates aqueous solution is prepared, stirs evenly and makes it completely dissolved;
(2) acidic aqueous solution or alkaline aqueous solution will be sequentially added in order in solution, crosslinking agent stirs evenly;
(3) mixed liquor of step (2) is subjected to water-bath cross-linking reaction at a certain temperature;
(4) by sterile gauze single berth on mold, the reaction solution for pouring into step (3) carries out pre-freeze, freeze-drying obtains sponge Shape combine dressing;
(5) the spongy combine dressing that step (4) obtains cut, dispensed, sterilized, obtain a kind of fiber of high wet strength Plain combine dressing.This is used for cellulose combine dressing for wound care, hemostasis.
As currently preferred technical solution, in step (1), the cellulose and its derivates aqueous solution, including And the one or more for being not limited to carboxymethyl cellulose (CMC), hydroxyethyl cellulose (HEC), hydroxypropyl cellulose (HPMC) etc. Mixture, the concentration of solution about 1-5%.
As currently preferred technical solution, the brookfield viscosity of the cellulose and its derivates is about 150- 6500mPa.s。
As currently preferred technical solution, in step (2), the alkaline aqueous solution is sodium hydroxide, carbonic acid Any one in hydrogen sodium, calcium bicarbonate, the concentration of the alkaline aqueous solution are 0.2-0.8mol/L, the alkaline aqueous solution with The volume ratio of reaction solution is 2:100-6:100;The acidic aqueous solution is acetic acid, malic acid, citric acid, any in hydrochloric acid One kind, the concentration of the acidic aqueous solution are 0.1-1.0mol/L, and the volume ratio of the acidic aqueous solution and reaction solution is 2: 100-8:100.
As currently preferred technical solution, in step (2), the crosslinking agent, including 1,4-butanediol two are shunk Glycerin ether (BDDE) or 1, diepoxides or 1- (3- dimethylamino-propyl) -3- ethyl of 2,7,8- diepoxyoctanes Carbodiimide (EDC);The mass ratio of the crosslinking agent and material is 1:0.1-1:0.8.
As currently preferred technical solution, in step (3), the bath temperature of the water-bath cross-linking reaction is 30- 90 DEG C, reaction time 2-12h.
As currently preferred technical solution, in step (4), the temperature of the pre-freeze is -20 DEG C, freeze-drying temperature Degree is -50 DEG C.
Compared with prior art, the beneficial effects of the present invention are:
Compared with the existing general traditional dressing using whole spongelike structure, the present invention is added single layer sterile gauze and answers It closes, efficiently solves the insufficient defect of bio-sponge mechanical property, and effectively reduce cost.
Compared with Chinese utility model patent CN201520871794, present invention design continues mainly for chronic wounds Sepage and oozing of blood, product design is simple, and the flexibility for remaining cellulose material is good, stick close advantage, inhale simultaneously Gelation easily removes and noresidue after liquid, and Chinese utility model patent CN201520871794 and the internal layer of skin contact are shells Glycan fiber filament may result in undesirable infection easily with wound adhesion when nursing is replaced.
Compared with Chinese patent application CN201711166122.8 and United States Patent (USP) US3096228, Chinese patent application The safety of CN201711166122.8 additive gamma-polyglutamic acid is not confirmed, the friendship that the glyoxal toxicity present invention uses Connection agent has successful application case in medical instruments field, what Q-med company of Sweden beauty and shaping product Restylane was used It is exactly that diepoxides is crosslinked, Seprafilm biological absorbable anti-adhesion membrane in the U.S. uses EDC crosslinking agent, faces Bed safety has been approved, and safety is higher.Gamma-polyglutamic acid adds in Chinese patent application CN201711166122.8 The effect of agent is promoting healing, and the effect of acidic aqueous solution or alkaline aqueous solution is to form ester bond or ehter bond must be anti-in the present invention Condition is answered, to maintain the gelation of sponge, therefore, the effect of the two is different.
High humidity strength element combine dressing of the present invention retains the flexibility and water imbibition, comfort of cellulose material itself And flexibility, while increasing gelation and high wet strength of the product in use process, enhance clinical applicability.By cellulose and Its derivative aqueous solution (for example, HPMC and HEC) carries out crosslinking and is made the form of sponge, the space three-dimensional porous structure of intersection, Make product have high-absorbable and gelation, while be added single layer sterile gauze carry out it is compound, efficiently solve bio-sponge power Learn the insufficient defect of performance.In practical applications, when for example the burn and scald of large area and chronic wounds handle, when dressing, can be real Removing for existing full wafer, brings convenience to nursing, while product gelation can avoid the secondary damage to wound.In addition, of the invention High humidity strength element combine dressing detects through determining heavy metals, aseptic experiment, endotoxin detection, vitro cytotoxicity, is intradermal Stimulation, sensitization test (STT) verifying prove that its toxicity is lower, securely and reliably.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of the cellulose combine dressing of high wet strength of the present invention.
Fig. 2 is the micro-structure diagram of cellulose combine dressing spongy layer in the embodiment of the present invention 2.
Fig. 3 is the healing photo of the small porcine skin surface of a wound in experimental example 8 of the present invention, wherein 1 to represent cellulose of the present invention compound Casting product group;2 represent absorbability gelatin foam group;3 represent sterile gauze group.
Fig. 4 is the dyeing schematic diagram of the full cortex healing skin of pig in experimental example 8 of the present invention, and wherein Fig. 4 (a) represents the present invention Cellulose combine dressing product group;Fig. 4 (b) represents absorbability gelatin foam group;Fig. 4 (c) represents sterile gauze group.
Specific embodiment
The present invention will be described in the following with reference to the drawings and specific embodiments, involved in technical method such as in this hair It is not illustrated in bright, is then this field convenient technical process, therefore repeat no more.
As shown in Figure 1, a kind of cellulose combine dressing of high wet strength of the present invention is from top to bottom respectively cellulose sponge Layer A, sterile gauze layer B, cellulose sponge layer C;The cellulose sponge layer A and cellulose sponge layer C using cellulose and its Derivative aqueous solution, acidic aqueous solution or alkaline aqueous solution, the mixing crosslinking of diepoxides crosslinking agent are made;The dressing In spongy.The thickness of cellulose sponge layer A is about 1-4cm, and the thickness of sterile gauze layer B is about 0.01mm, cellulose sponge The thickness of layer C is about 1-4cm.The porosity of cellulose sponge layer A and cellulose sponge layer C reach 80% or more, and micropore size is 10-50μm。
It is to prepare embodiment below:
Embodiment 1
A kind of cellulose combine dressing of high wet strength and preparation method thereof, includes the following steps:
It (1) is the ratio (body of 1% HPMC aqueous solution and 4% HEC aqueous solution in 1:1 by prepared mass percent concentration Product ratio) mixing 600mL, and stir evenly;
(2) by the mixed liquor of step (1) sequentially add in proportion 0.2mol/L sodium bicarbonate solution and a certain amount of bis-epoxy 1,2,7,8-diepoxyoctane 3g of compound crosslink agent, stirs evenly;
(3) reaction solution of step (2) is subjected to water-bath, 60 DEG C of bath temperature, reaction time 3h;
(4) by sterile gauze single berth on mold, the reaction solution of step (3) is poured into, carries out -20 DEG C of pre-freezes, -50 DEG C of freezings are dry It is dry to obtain combination product;
(5) the spongy combination product that step (4) obtains cut, dispensed, sterilized, obtained for the compound of wound care Dressing.
The raw material HPMC solution viscosity is 150-400mPa.s, and the HEC solution viscosity is 1500- 2500mPa.s。
In the reaction mixture, the mass ratio of 1,2,7,8-diepoxyoctane of raw material and crosslinking agent is 1:0.1 (W/W), the volume ratio of lye sodium bicarbonate solution and reaction solution is 6:100(V:V).
Embodiment 2
A kind of cellulose combine dressing of high wet strength and preparation method thereof, includes the following steps:
(1) the HEC aqueous solution 600mL that prepared mass percent concentration is 2% is stirred evenly;
(2) by the solution of step (1) sequentially add in proportion 0.8mol/L NaOH solution and a certain amount of diepoxides Crosslinking agent 1,4-butanediol diglycidyl ether 3.6g, stirs evenly;
(3) reaction solution of step (2) is subjected to water-bath, 45 DEG C of bath temperature, reaction time 4h;
(4) by sterile gauze single berth on mold, the reaction solution of step (3) is poured into, carries out -20 DEG C of pre-freezes, -50 DEG C of freezings are dry It is dry to obtain combination product;
(5) the spongy combination product that step (4) obtains cut, dispensed, sterilized, obtained for the compound of wound care The microstructure of dressing, gained cellulose combine dressing spongy layer is as shown in Figure 2.
The raw material HEC solution viscosity is 1500-2500mPa.s.
In the reaction mixture, the mass ratio of raw material and crosslinking agent 1,4-butanediol diglycidyl ether is 1:0.3 (W/W), lye NaOH solution and the volume ratio of reaction solution are 2:100(V:V).
Embodiment 3
A kind of cellulose combine dressing of high wet strength and preparation method thereof, includes the following steps:
(1) the CMC aqueous solution 600mL for being 1% by prepared mass percent concentration, stirs evenly;
(2) solution of step (1) is sequentially added to the citric acid solution and a certain amount of bis-epoxy chemical combination of 0.5mol/L in proportion 1,2,7,8- diepoxyoctane 4.8g of object crosslinking agent, stirs evenly;
(3) reaction solution of step (2) is subjected to water-bath, 90 DEG C of bath temperature, reaction time 2h;
(4) by sterile gauze single berth on mold, the reaction solution of step (3) is poured into, carries out -20 DEG C of pre-freezes, -50 DEG C of freezings are dry It is dry to obtain combination product;
(5) the spongy combination product that step (4) obtains cut, dispensed, sterilized, obtained for the compound of wound care Dressing.
The raw material CMC solution viscosity is 4000-6500mPa.s
In the reaction mixture, the mass ratio of 1,2,7,8- diepoxyoctane of raw material and crosslinking agent is 1:0.8(W/W), The volume ratio of acid solution citric acid solution and reaction solution is 8:100(V:V).
Embodiment 4
A kind of cellulose combine dressing of high wet strength and preparation method thereof, includes the following steps:
It (1) is the ratio of 2.5% CMC aqueous solution and 2.5% HEC aqueous solution in 1:1 by prepared mass percent concentration (volume ratio) mixes 600mL, and stirs evenly;
(2) mixed liquor of step (1) is sequentially added to the acetum and a certain amount of bis-epoxy chemical combination of 1.0mol/L in proportion Object crosslinking agent 1,4-butanediol diglycidyl ether 7.5g, stirs evenly;
(3) reaction solution of step (2) is subjected to water-bath, 60 DEG C of bath temperature, reaction time 4h;
(4) by sterile gauze single berth on mold, the reaction solution of step (3) is poured into, carries out -20 DEG C of pre-freezes, -50 DEG C of freezings are dry It is dry to obtain combination product;
(5) the spongy combination product that step (4) obtains cut, dispensed, sterilized, obtained for the compound of wound care Dressing.
The raw material CMC solution viscosity is 4000-6500mPa.s, and the HEC solution viscosity is 4700- 5500mPa.s。
In the reaction mixture, raw material and crosslinking agent 1,4-butanediol diglycidyl ether mass ratio are 1:0.5(W/ W), the volume ratio of acid solution acetum and reaction solution is 2:100(V:V).
Embodiment 5
A kind of cellulose combine dressing of high wet strength and preparation method thereof, includes the following steps:
It (1) is ratio mixing (volume ratio) of the 5%CMC and 1%HPMC solution in 1:5 by prepared mass percent concentration 600mL is stirred evenly;
(2) aqueous solution of step (1) is sequentially added to the hydrochloric acid solution and a certain amount of bis-epoxy chemical combination of 0.1mol/L in proportion Object crosslinking agent 1- (3- dimethylamino-propyl) -3- ethyl carbodiimide (EDC) 5g, stirs evenly;
(3) reaction solution of step (2) is subjected to water-bath, 65 DEG C of bath temperature, reaction time 4h;
(4) by sterile gauze single berth on mold, the reaction solution of step (3) is poured into, carries out -20 DEG C of pre-freezes, -50 DEG C of freezings are dry It is dry to obtain combination product;
(5) the spongy combination product that step (4) obtains cut, dispensed, sterilized, obtained for the compound of wound care Dressing.
The raw material CMC solution viscosity is 1500-2500mPa.s, and HPMC solution viscosity is 150- 400mPa.s
In the reaction mixture, raw material and crosslinking agent 1- (3- dimethylamino-propyl) -3- ethyl carbodiimide (EDC) quality Than for 1:0.5(W/W), the volume ratio of acid solution hydrochloric acid solution and reaction solution is 5:100(V:V).
Experimental example
Effect of the invention is further elaborated below by way of experimental example:
The measurement of 1 water absorption rate of experimental example
Water absorption rate indicates the weight of every gram of product imbibition.The sponge sample for taking the present invention dry, thickness is identical, cut out rectangle, It is each 3 pieces round and irregular shape, respective weight W1 is weighed, is immersed in 37 DEG C of physiological saline respectively, 5min is impregnated and sufficiently inhales Water gently clamps one jiao with pincet, leaves the water, drain after moisture (aerial to stop about 1min) afterwards weigh its weight W2.It presses It is calculated according to water absorption rate calculation formula, water absorption rate (g/g)=[W2(g)-W1(g)]/W1(g) averaged.It the results are shown in Table 1.
The test of 2 wet strength of experimental example
Wound dressing sample of the present invention is cut into the strip sample of 5.5cm wide, length is at least 8cm.Sample doubling is put into Sheng Have in the container of physiological saline, solution height about 2cm, sample infiltration after take out, guarantee both ends there are about 1cm at be drying regime, Specimen holder is gone out into container, its both ends is put into the fixture of imported electronic fabric strength tester, clamps the top and bottom of sample respectively, is surveyed The two jaws distance for trying instrument is 5cm, and the speed of service that jaw is arranged is 10cm/ min, and the maximum that record destroys sample is exerted oneself (N), same wound dressing is repeated above-mentioned experiment at least 5 times, obtains 5 wet strength values, and calculate average value, as a result sees Table 1.
The comparison of the water absorption rate, dry strength and wet strength of 1 sample of table
Remarks: the sample before not combining does not add the sponge products of sterile gauze;Product after combination is to load sterile gauze Joint product.
As can be seen from Table 1, combination front and back only slightly increases the change of product liquid absorption amount, and dry strength can be enhanced To original at least 7 times or more, wet strength be can be enhanced to original 20 times or more, hence it is evident that increase product in use process Gelation and high wet strength, provide convenience to clinical nursing procedure.
3 determining heavy metals of experimental example
The joint product 1g of Example 1 ~ 5 is surveyed according to the Residue on ignition check method of " Chinese Pharmacopoeia 2015 editions " the 4th 0841 Fixed (blazing temperature is 500 ~ 600 DEG C).According to " Chinese Pharmacopoeia 2015 editions " the 4th 0821 heavy metal inspection technique measurement, heavy metal Testing result < 20ppm.
4 aseptic experiment of experimental example
It is carried out according to method as defined in GB/T 14233.2-2005, the joint product obtained to embodiment 1 ~ 5 detects, and ties Fruit shows sterile.
The detection of 5 endotoxin of experimental example
It is carried out according to test according to method as defined in GB/T 14233.2-2005.Endogenous toxic material is carried out to the joint product of embodiment 1 ~ 5 Element detection, as the result is shown endotoxin all≤0.5Eu/ml.
The detection of 6 vitro cytotoxicity of experimental example
According to GB/T 16886.5-2003 BiologicalEvaluationofMedicalDevice: vitro cytotoxicity test obtains embodiment 1 ~ 5 The joint product obtained carries out cytotoxin detection, takes leaching liquor, and testing result shows cytotoxicity≤2 grade.
The intradermal stimulation of experimental example 7, sensitization test (STT)
Picosecond laser pulse: carrying out according to method as defined in GB/T 16886.10-2005, obtains to embodiment 1 ~ 5 compound Product is detected, as the result is shown without skin wound repair;Sensitization of skin: according to side as defined in GB/T 16886.10-2005 Method carries out, and the joint product obtained to embodiment 1 ~ 5 detects, and reacts as the result is shown without sensitization of skin.
The test of 8 piggy skin healing of experimental example
Healthy miniature pig 10 is randomly divided into negative control group (sterile gauze), positive controls (the auspicious grace absorbability in Jiangxi Gelfoam), product group (cellulose combine dressing of the present invention), full cortex resection operation model, 3d is free before miniature pig is tested Feed.8% sodium sulfide solution removal back wool of 1d before testing.After for 24 hours, in 70% ethanol disinfection of preserved skin area, 10% is hydrated chlorine Sour intraperitoneal injection of anesthesia (1-1.5mL/kg).With surgical scissors and tweezers, 6 diameters are cut off in each pig back linea vertebralis two sides For the full thick-layer skin of 1.5 × 1.5cm.Combine dressing product of the present invention and absorbability gelfoam (positive control) are used respectively It in two sides wound, is covered, then bandaged with paraffin degreasing gauze.15d after operation, 10% hydration chloric acid intraperitoneal injection fiber crops Liquor-saturated, the clip holostrome surface of a wound is observed for histology.Histoorgan is fixed through 10% formalin, routine paraffin wax embedding, slice thick 4~5 μm, HE and Masson trichrome stain.The healing state of the digital camera shooting record surface of a wound,
See that Fig. 3 photo records: 1: cellulose combine dressing product group of the present invention;2: absorbability gelatin foam group;3: sterile yarn Cloth group.As shown in Figure 1, more 1st day in oozing of blood and sepage, from figure 3, it can be seen that cellulose combine dressing of the invention Product group 1 compares absorbability gelatin foam group 2, and imbibition is preferable, applicating property is preferable, and product bounces back after imbibition, Bu Huifa Raw infiltrate to surrounding health tissue is infected, and does not have the case where blood exudation.The skin of miniature pig heals substantially in 15 days, more Phenomena such as during conjunction without obvious hemotoncus, necrosis, infection, compare gauze group 3, it can be seen that the wound of healing is also more smooth.
As shown in figure 4, the dyeing of the full cortex healing skin of miniature pig, cellulose combine dressing product group of the present invention is (see Fig. 4 (a)) many less than sterile gauze group (see Fig. 4 (c)) inflammatory cell, the case where healing of tissue no hyper-proliferative, occurs. Since cellulose material has the presence of sodium ion, so participating in playing the work of a degree of control infection in agglutination With so product group is compared with the control group, inflammatory cell will lack.

Claims (10)

1. a kind of cellulose combine dressing of high wet strength, which is characterized in that the dressing is from top to bottom respectively cellulose Spongy layer, sterile gauze layer, cellulose sponge layer;The cellulose sponge layer uses cellulose and its derivates aqueous solution, acid Property aqueous solution or alkaline aqueous solution, crosslinking agent mixing crosslinking be made;The dressing is in spongy.
2. dressing as described in claim 1, which is characterized in that the dressing is from top to bottom respectively the fiber of 1-4cm thickness Plain spongy layer, the sterile gauze layer of 0.01mm thickness, 1-4cm thickness cellulose sponge layer.
3. dressing as claimed in claim 1 or 2, which is characterized in that the porosity of the cellulose sponge layer reach 80% with On, micropore size is 10-50 μm.
4. a kind of preparation method of the cellulose combine dressing of high wet strength as described in any one of claims 1-3, feature It is, includes the following steps:
(1) certain density cellulose and its derivates aqueous solution is prepared, is stirred evenly;
(2) solution of step (1) is sequentially added into a certain amount of acidic aqueous solution or alkaline aqueous solution and crosslinking agent in order, is stirred It mixes uniformly;
(3) mixed liquor of step (2) is subjected to water-bath cross-linking reaction at a certain temperature;
(4) by sterile gauze single berth on mold, the reaction solution of step (3) is poured into, carries out pre-freeze, freeze-drying obtains sponge Shape combination product;
(5) the spongy combination product that step (4) obtains cut, dispensed, sterilized, obtain a kind of fiber of high wet strength Plain combine dressing.
5. a kind of preparation method of the cellulose combine dressing of high wet strength according to claim 4, it is characterised in that: In step (1), the cellulose and its derivates aqueous solution is selected from carboxyl methyl cellulose, hydroxyethyl cellulose HEC, hydroxypropyl One or more of base cellulose HPMC mixture, the mass percent concentration of solution are 1-5%.
6. a kind of preparation method of the cellulose combine dressing of high wet strength according to claim 5, it is characterised in that: institute The brookfield viscosity for stating cellulose and its derivates is 150-6500mPa.s.
7. a kind of preparation method of the cellulose combine dressing of high wet strength according to claim 4, it is characterised in that: In step (2), the alkaline aqueous solution is sodium hydroxide, sodium bicarbonate, any one in calcium bicarbonate, the alkaline water The concentration of solution is 0.2-0.8mol/L, and the volume ratio of the alkaline aqueous solution and reaction solution is 2:100-6:100;The acid Property aqueous solution be acetic acid, malic acid, citric acid, any one in hydrochloric acid, the concentration of the acidic aqueous solution is 0.1- The volume ratio of 1.0mol/L, the acidic aqueous solution and reaction solution is 2:100-8:100.
8. a kind of preparation method of the cellulose combine dressing of high wet strength according to claim 4, it is characterised in that: In step (2), the crosslinking agent, including 1,4-butanediol diglycidyl ether or 1, the bis-epoxy of 2,7,8- diepoxyoctanes Compound or 1- (3- dimethylamino-propyl) -3- ethyl carbodiimide;The mass ratio of the crosslinking agent and material is 1:0.1-1: 0.8。
9. a kind of preparation method of the cellulose combine dressing of high wet strength according to claim 4, it is characterised in that: In step (3), the bath temperature of the water-bath cross-linking reaction is 30-90 DEG C, reaction time 2-12h.
10. a kind of preparation method of the cellulose combine dressing of high wet strength according to claim 1, it is characterised in that: In step (4), the temperature of the pre-freeze is -20 DEG C, and the freeze-drying temperature is -50 DEG C.
CN201811495331.1A 2018-12-07 2018-12-07 A kind of cellulose combine dressing of high wet strength and preparation method thereof Pending CN109276745A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113332039A (en) * 2021-05-31 2021-09-03 西南大学 Continuous drainage sugarcane sponge dressing
CN115160637A (en) * 2021-04-01 2022-10-11 诺一迈尔(山东)医学科技有限公司 Degradable hemostatic sponge and preparation method thereof

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CN103877606A (en) * 2014-01-23 2014-06-25 华侨大学 Absorbable bleeding-stopping compound sponge and preparation method thereof
CN107189111A (en) * 2016-11-23 2017-09-22 浙江美华鼎昌医药科技有限公司 A kind of preparation method of cellulose composite sponge

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CN102552965A (en) * 2012-01-17 2012-07-11 东华大学 Method for preparing nano-cellulose antibacterial composite material through on-line culture
CN103877606A (en) * 2014-01-23 2014-06-25 华侨大学 Absorbable bleeding-stopping compound sponge and preparation method thereof
CN107189111A (en) * 2016-11-23 2017-09-22 浙江美华鼎昌医药科技有限公司 A kind of preparation method of cellulose composite sponge

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CN115160637A (en) * 2021-04-01 2022-10-11 诺一迈尔(山东)医学科技有限公司 Degradable hemostatic sponge and preparation method thereof
CN115160637B (en) * 2021-04-01 2023-12-01 诺一迈尔(山东)医学科技有限公司 Degradable hemostatic sponge and preparation method thereof
CN113332039A (en) * 2021-05-31 2021-09-03 西南大学 Continuous drainage sugarcane sponge dressing

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Application publication date: 20190129