CN109778350A - A kind of alginate fibre preparation method and application of the antibacterials of class containing Chlorhexidine - Google Patents
A kind of alginate fibre preparation method and application of the antibacterials of class containing Chlorhexidine Download PDFInfo
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Abstract
The present invention relates to a kind of alginate fibre preparation methods of antibacterials of class containing Chlorhexidine, the method is to carry out grafting processing to alginate fibre with Dopamine hydrochloride or other or amine salt or glutaraldehyde as cross linker, connect chlorhexidine gluconate or chlorhexidine acetate, the alginate fibre of the antibacterials of class containing Chlorhexidine is obtained, grafting method includes impregnating or spraying.The present invention is different from traditional alginate fiber preparation invention, can effectively reduce production cost, is not necessarily to highly energy-consuming high consumption of resources, for preparation process also without high pollution, equipment investment is suitable, and with short production cycle, invention promotion and application are easier to.
Description
Invention field
The invention belongs to therapeutic wound healing invention fields, are related to a kind of alginate fibre of antibacterials of class containing Chlorhexidine
Preparation method and application.
Background invention
Wound healing is a complicated dynamic process, and bacterium infection is to influence one of the principal element of wound healing.
If treatment of wounds is not good at or dressing improper use, bacterium infection will cause many adverse consequences, serious possibility threat to life.
Traditional dressing has a single function, and no antibiotic property, imbibition rate is poor, easily stimulates skin and influences the healing of wound, bacterium infection it is several
Rate greatly increases, and secondary damage is easily caused when removing, therefore the exploitation of new pattern compress is hot spot.1962, Winter was first
It is secondary to propose the concept of wound moist healing, confirm that wet condition can accelerate to hurt in the human trial by Rovee et al. in 1970
Mouth epithelial cell migrates the speed of hyperplasia.Clinically, it needs more effective wound to restore doctor's material and more meets diversified disease wound
Mouthful dressing make up the deficiency of traditional dressing performance.The continuous popularization and receiving of wound wet union theory and other are a variety of
Factor promotes new pattern compress and continues to bring out, the more diversification of type, performance and function, especially with alginate dressing and
Aerogel dressing is representative.
Chlorhexidine gluconate (chlorhexidine gluconate) has great broad-spectrum antibacterial, bactericidal effect,
It is a kind of preferable sterilizing medicine.It is demonstrated experimentally that it is effective to gram-positive bacteria and negative bacterium, it is usually outer to be used for skin
Disinfection, wound irrigation, gargle etc..Chlorhexidine and its esters are longer than the bactericidal effect time of alcohols, have duration (residue
Attachment), it can be effectively controlled infectious bacteria growth.Chlorhexidine gluconate is alkali compounds, and alginates are anionic polymer, two
Person will not react, and can stablize and coexist.Appoint swallow etc. have studied 2% chlorhexidine gluconate disinfectant liquid for skin to MRSA in hospital,
The inhibitory effect of tetra- kinds of important pathogens of VRE, KPC and MDRAB, minimum inhibitory concentration (MIC value) be respectively 19.53mg/L,
39.06mg/L, 312.50mg/L and 625.00mg/L.
Traditional alginate dressing is prepared using wet spinning, and wet spinning needs many kinds of, bulky stoste
It prepares and prepares equipment before spinning, be furnished with coagulating bath, circulation and reclaimer, process flow complexity, factory building and equipment are thrown
Provide that expensive, spinning speed is low, higher cost.Compositional type alginate material is functional, but there is anti-microbial property deficiency
Defect, and multiple material is only simply to compound, and does not carry out effective molecule grafting.Novel medicine-carrying antibiosis dressing is mostly to receive
The silver-colored based compound of rice, nano-titanium dioxide, nano zine oxide and poly (hexamethylene) etc. are antibacterial agent, wherein nano silver and are received
Rice zinc oxide has cytotoxicity, and nano silver is easily oxidized to Ag2O and inactivate, the Antibacterial Mechanism of nano zine oxide is also not
It is clear.The antibacterial effect of nano-titanium dioxide is influenced by light-catalysed.The poly (hexamethylene) of high-content has potential cause
Cancer, mutagenesis and genotoxicity, American-European consumer safety Science committee (SCCS) in the new bill that in April, 2017 promulgates,
Its safety limit of clear stipulaties is 0.1%；And poly (hexamethylene) can occur ion complexation with alginates and react, and easily lead to it
Antibiotic property passivation.
Summary of the invention
It is an object of the invention to be directed to the deficiency of existing invention, a kind of alginates of antibacterials of class containing Chlorhexidine are provided
Fiber producing processes and application.
The scheme of the invention is:
A kind of alginate fibre preparation method of the antibacterials of class containing Chlorhexidine, the method be with Dopamine hydrochloride or its
He or amine salt or glutaraldehyde as cross linker carry out grafting processing to alginate fibre, connect chlorhexidine gluconate or acetic acid chlorine oneself
It is fixed, the alginate fibre of the antibacterials of class containing Chlorhexidine is obtained, grafting method includes impregnating or spraying.
Preferably, it the described method comprises the following steps:
Step 1: the spinning solution that sodium alginate/potassium obtains is added in water whipping process, continues to stir, gluconic acid is added
Chlorhexidine or chlorhexidine acetate and crosslinking agent are sufficiently stirred dissolution and react, spinning solution is obtained by filtration；
Step 2: wet-spinning frame is used, spinning solution is squeezed into CaCl2In the coagulation tank of solidification liquid, in process of setting
Stream plus replenisher CaCl2Solidification liquid and chlorhexidine gluconate or chlorhexidine acetate；
Step 3: stoste spinneret, one-off drawing, succeeding stretch after coagulating bath obtain fiber first product；
Step 4: fiber first product is impregnated through ethanol solution 2-3 times respectively, and centrifugal dehydration after impregnating every time is final to pass through
It winds, be dried to obtain finished fiber.
It is further preferred that the step 1 crosslinking agent is Dopamine hydrochloride solution, Dopamine hydrochloride concentration of polymer solution
For 30-40ug/mL, Dopamine hydrochloride solution and water volume ratio 0.4/150-0.5/150；
Or the step 1 crosslinking agent is monoethanolamine hydrochloride, monoethanolamine hydrochloride mass concentration is 10-20mg/
ML, Dopamine hydrochloride solution and water volume ratio 0.5/150-1/150；
Or the step 1 crosslinking agent is glutaraldehyde, glutaraldehyde mass concentration is 1.0%, glutaraldehyde solution and water volume ratio
0.5/150-0.6/150。
It is further preferred that sodium alginate/the potassium and water solid-to-liquid ratio are 0.033-0.04 (kg/L)；Step 1 grape
Saccharic acid chlorhexidine mass fraction is 20%, and the volume ratio of additional amount and water is 1:150, step chlorhexidine digluconate
Additional amount and the volume ratio of water are 1:150 or step 1 chlorhexidine acetate liquid quality fraction is 92% or more, additional amount
It is 0.14/150-0.16/150 (kg/L) with the solid-to-liquid ratio of water, the solid-to-liquid ratio of step chlorhexidine diacetate additional amount and water is
0.14/150-0.16/150(kg/L)。
It is further preferred that the step 1 whipping temp range is 45-65 DEG C；Step 2 CaCl2Solidification liquid quality
Concentration is 2.5%-5.0%；Spinning speed is in 100m/min or less during step 3 spinneret, one-off drawing, succeeding stretch；Step
Rapid tetraethoxide concentration of polymer solution is 35%-95%, is impregnated 2-3 times, each 1.5-2.5h.
The method can comprise the further steps of:
Step A: alginate fiber is laid in plate, and fixed；
Step B: crosslinking agent is sprayed on alginate fiber surface, obtains the alginate fibre containing grafting agent；
Step C: using sprinkling equipment the alginate fibre surface containing grafting agent uniformly spray chlorhexidine gluconate or
The methanol solution of chlorhexidine acetate, freeze-day with constant temperature obtain the alginate fiber containing chlorhexidine gluconate or chlorhexidine acetate；
Step D: the alginate fiber containing chlorhexidine gluconate or chlorhexidine acetate is placed in ethanol solution successively
Washing, stirring, take out freeze-day with constant temperature；
Step E: by the fiber after drying it is rolled and combing, obtain finished fiber.
Preferably, the step B crosslinking agent is Dopamine hydrochloride solution, and Dopamine hydrochloride concentration of polymer solution is 30-
40ug/mL, Dopamine hydrochloride solution and alginate fiber liquid-solid ratio are 0.4/2-0.5/2 (L/g)；Step C sprays 0.56mg/
The chlorhexidine acetate methanol solution of mL, chlorhexidine acetate methanol solution and alginate fiber liquid-solid ratio are (20-30)/2 (mL/
g)。
Preferably, the step B crosslinking agent is Dopamine hydrochloride solution, and Dopamine hydrochloride concentration of polymer solution is 30-
40ug/mL, Dopamine hydrochloride solution and alginate fiber liquid-solid ratio are 0.4/2-0.5/2 (L/g), step C gluconic acid chlorine
It is 20%1ml that oneself, which determines concentration of polymer solution, obtains chlorhexidine gluconate methanol solution to analyze methanol constant volume to 25mL, uses
Chlorhexidine gluconate methanol solution is uniformly sprayed on the alginate fibre surface containing grafting agent by sprinkling equipment；
Preferably, the step B crosslinking agent is glutaraldehyde solution, and glutaraldehyde solution mass concentration is 1.0%, and glutaraldehyde is molten
Liquid and alginate fiber liquid-solid ratio are 0.5/2-0.6/2 (L/g), and the chlorhexidine acetate methanol that step C sprays 0.56mg/mL is molten
Liquid, chlorhexidine acetate methanol solution and alginate fiber liquid-solid ratio are (20-30)/2 (mL/g).
Preferably, the step C or step D freeze-day with constant temperature temperature are 60 DEG C, drying time 2h.
The invention has the advantages that:
1, the present invention is different from traditional alginate fiber preparation, can effectively reduce production cost, consumes without highly energy-consuming height
Resource, for preparation process also without high pollution, equipment investment is suitable, with short production cycle, and invention promotion and application are easier to.
2, the present invention is on the basis of optimizing alginate fiber preparation method, with hydrochloric acid DOPA in fiber manufacturing process
Amine is grafting agent, using the intermolecular interaction of hydrogen bond of chlorhexidine gluconate alginate, creatively to alginate
Quaternized grafting is carried out, is grafted the chlorhexidine gluconate with broad spectrum antibacterial or chlorhexidine acetate to improve dressing antibiotic property
Energy.There are a large amount of hydroxyl and carboxyl in alginates structure, there are a large amount of hydroxyl and amino in chlorhexidine gluconate structure,
This is the molecular basis of hydrogen bond action.There are amino and hydroxyl in Dopamine hydrochloride molecular structure, can be compound with sodium alginate,
Make Dopamine hydrochloride be incorporated in alginate molecular structures to reach grafting purpose by dopamine polymerization reaction, fibre can be reinforced
Hydrogen bond action between dimension and antibacterials enhances intensity of the dressing in wet condition, extends its shelf-life, it is anti-to improve dressing
Bacterium performance, the grafting chlorhexidine gluconate of preparation or the dressings product absorption diffusate ability of chlorhexidine acetate are strong, have good
It can be rapidly after good gas exchange capacity, biodegradable and good biocompatibility, adhesion wound and absorption wound diffusate
Gel is formed, can be shortened wound healing time.The dressings product is used for preoperative disinfection simultaneously, can directly act on bacterial cell
On film, bactericidal effect and noresidue, wide adaptability with broad-spectrum long-acting can partially substitute traditional dressing.The casting product energy
Accelerate the growth of granulation tissue and the dissolution of necrotic tissue, promote body cell proliferation and differentiation, avoid causing secondary injury and
The swelling of surface of a wound surrounding skin is rotted.Ca in alginate dressing2+It can be with the Na in wound fluid+Ion exchange is carried out,
It forms sodium alginate gel layer and is covered on wound, maintain an anaerobic or hypoxemia, slightly sour, wet healing environment.Ca2+Also can make
For a kind of signaling molecule, the hemostatic composition in blood is activated, accelerates to form clot in site of injury, effectively control bleeding amount of wound,
It avoids that hemolytic reaction occurs.
3, medicinal functional alginate dressings series of products produced by the invention have broad spectrum antibacterial, safely may be used
It leans on, it is non-toxic.The product can be used for simultaneously it is preoperative, in art and the disinfection of postoperative skin, the surface of a wound and instrument etc..
4, the imbibition rate that antibacterial alginate fibre dressing prepared by the present invention stands 0.5 hour in simulation diffusate is not low
In 100%, the pH value of dressing soak is 5.5-7.5.
5,3 months under the conditions of antibacterial alginate fibre dressing prepared by the present invention is stored at room temperature, antibacterials in dressing
Adsorption rate is about 48.5%, and it is 0.5% that the ultimate density of antibacterials, which is not less than, in dressing, and content is about 78mg/g.Product tool
There are non-toxic, good gas exchange capacity, humectant energy, high liquid-absorbing energy, biodegradable and good bio-compatible
Property.
6, the present invention is grafted antibacterials in alginate fibre dressing will not influence its tensile property and chemical stability.
7, antibacterial alginate fibre dressing prepared by the present invention has excellent anti-microbial property, to gram-positive bacteria and leather
Lan Shi negative bacterium is effective；And the bactericidal effect time is long, has duration (residue attachment), can be effectively controlled infectious bacteria taste
It is raw.
8, the present invention carries out at grafting medical alginate matrix with the amine salt such as Dopamine hydrochloride or glutaraldehyde cross-linking agent
Reason is grafted broad spectrum antibacterial drug chlorhexidine gluconate or chlorhexidine acetate, and primary first-order equation is used in this preparation process, is impregnated
Or spray pattern is grafted, during the appendix mode of antibacterials therein is one-time reaction grafting, impregnates or spray
It is grafted by thermal response, obtains the long-acting serial alginate dressing of performance stabilization and antibacterials not easy to lose.
9, the present invention maintains alginates in alginate and chlorhexidine gluconate or chlorhexidine acetate grafting process
The original excellent properties of fiber, improve the anti-microbial property of alginate fibre, to staphylococcus aureus and pseudomonas aeruginosa
Gram-positives such as (Pseudomonas aeruginosas), negative bacterium have preferable effect, these experimental verification results are pass of the invention
Key point.
Detailed description of the invention
The structure chart (b) of M and G unit structure figure (a) and chlorhexidine gluconate in Fig. 1 alginate fibre: Fig. 1 a is algae
M and G unit structure figure in silicate fiber, Fig. 1 b are the structure chart of chlorhexidine gluconate；
Fig. 2 is that chlorhexidine gluconate (b) is schemed in the HPLC of 258nm in standard items chlorhexidine acetate (a) and fiber sample；
Biocidal property result of 1 test thread of Fig. 3 embodiment to staphylococcus aureus: b is to carry medicine content as 23mg/g
The fungistatic effect figure of Sorbsan；C is the fungistatic effect figure for carrying the Sorbsan that medicine content is 79mg/g；
Biocidal property result of 1 test thread of Fig. 4 embodiment to pseudomonas aeruginosa: b is to carry the algae that medicine content is 23mg/g
The fungistatic effect figure (embodiment 3) of sour calcium fiber；C is that the fungistatic effect figure for the Sorbsan that load medicine content is 79mg/g is (real
Apply example 1)；
Resistance bacterium the performance test results of Fig. 5 embodiment 1 to staphylococcus aureus: it is cultivated for 24 hours after throwing off sample: (a) No. 1
Sample, common gauze have bacterium growth on dry conditions, ware；(b) No. 2 samples, pure Sorbsan have on dry conditions, ware
Bacterium growth；(c) No. 3 samples, the Sorbsan that load medicine content is 23mg/g asepsis growth on dry conditions, ware；(d) No. 4
Sample, the Sorbsan that load medicine content is 79mg/g asepsis growth on dry conditions, ware；
Resistance bacterium the performance test results of Fig. 6 embodiment 1 to pseudomonas aeruginosa: it is cultivated for 24 hours before throwing off sample: (a) No. 1 sample
Product, common gauze have bacterium growth on dry conditions, ware；(b) No. 2 samples, pure Sorbsan have bacterium on dry conditions, ware
Growth；(c) No. 3 samples, the Sorbsan that load medicine content is 23mg/g asepsis growth on dry conditions, ware；(d) No. 4 samples
Product, the Sorbsan that load medicine content is 79mg/g asepsis growth on dry conditions, ware；
Fig. 7 is that the load medicine content of embodiment 1 is after 79mg/g drug-loading fibre inhibits staphylococcus aureus culture, and sampling carries out
SEM scanning figure；
Fig. 8 is that the load medicine content of embodiment 1 is after 23mg/g drug-loading fibre inhibits staphylococcus aureus culture, and sampling carries out
SEM scanning figure；
Fig. 9 is that the load medicine content of embodiment 1 is after 79mg/g drug-loading fibre inhibits Pseudomonas aeruginosa culture, and sampling carries out SEM and sweeps
Tracing；
Figure 10 is that the load medicine content of embodiment 1 is after 23mg/g drug-loading fibre inhibits Pseudomonas aeruginosa culture, and sampling carries out SEM and sweeps
Tracing；
In Fig. 7-10, SEM scanning figure shows drug-loading fibre prepared by two kinds of embodiments to staphylococcus aureus and green
Purulence bacillus all has preferably absorption inhibitory effect, and there are more dead thallus for fiber surface
1 difference drug-loading fibre FT-IR of Figure 11 embodiment detection；No. 1 sample drugloading rate is 0mg/g, No. 2 drugloading rates are 23mg/
G, No. 3 drugloading rates are 79mg/g；
Figure 12 embodiment 1-3 carries resistance bacterium the performance test results when medicine content is 23mg/g for staphylococcus aureus；
Figure 13 is resistance bacterium the performance test results of the embodiment 6 to pseudomonas aeruginosa: Figure 13 a is blank control, and Figure 13 b is
6 drug-loading fibre of embodiment；
Figure 14 is resistance bacterium the performance test results of the embodiment 6 to staphylococcus aureus: Figure 14 a is blank control, Figure 14 b
It is 6 drug-loading fibre of embodiment.
Specific embodiment
The present invention is further illustrated below with reference to embodiment, but the scope of protection of present invention is not limited to implement
The range of example statement.
As shown in Figure 2: object has larger absorption peak at 258nm.The appearance time of chlorhexidine acetate is shorter, with grape
Saccharic acid Chlorhexidine appearance time difference is less than 1min, and methodological study result is good.Using certain density formic acid solution conduct
Acid modification agent, both reasonable analysis appearance difference, establishes the HPLC of chlorhexidine acetate and chlorhexidine gluconate assay
Method, it is simple and feasible, there is certain reference value to researchs such as assay, the Control of Impurities of Chlorhexidine class compound.
Embodiment 1
A kind of alginate fibre preparation method of the antibacterials of class containing Chlorhexidine, the described method comprises the following steps:
Step 1: 150L water and high-speed stirred are added into reactor, while being slowly added to 5-6kg sodium alginate/potassium powder
End obtains the spinning solution that mass fraction is 3.5% or so, and temperature range is 45-65 DEG C, continues to stir, 1000mL mass point is added
The Dopamine hydrochloride solution 0.4-0.5L that the chlorhexidine gluconate solution and concentration that number is 20% are 30-40ug/mL, is sufficiently stirred
It mixes dissolution and reacts, spinning solution is obtained by filtration.
Step 2: wet-spinning frame is used, stoste is squeezed into concentration into metering pump, filter from spinning head (10000 hole)
CaCl of the range 2.5%~5.0%2In coagulation tank, through CaCl2Solidification liquid makes its stabilization, stream plus replenisher in process of setting
CaCl2The chlorhexidine gluconate solution that aqueous solution (concentration is consistent with solidification liquid) and 1000mL mass fraction are 20%.
Step 3: stoste spinneret, one-off drawing, succeeding stretch after coagulating bath obtain fiber first product, and spinning speed exists
100m/min or less.
Step 4: respectively through the ethanol solution 2-3 times immersion that content is 35%-95%, each 2h soaks fiber first product every time
Centrifugal dehydration after bubble, it is final it is rolled, be dried to obtain finished fiber, wherein ethanol solution is reusable, passes through control
Concentration of alcohol, soaking time respectively obtain the Sorbsan for carrying that medicine content is 23mg/g, 79mg/g.
Testing result is shown in Fig. 3-11, it is known that with the raising for being grafted chlorhexidine gluconate content in Sorbsan
(23mg/g → 79mg/g), to staphylococcus aureus, scope of restraining fungi is gradually expanded on agar plate.Sample is fine in (b, c)
Dimension is largely dissolved in nutrient agar, illustrates that Sorbsan is a kind of dissolution type anti-bacterial fibre.As shown in Figure 4, (c) in there are bright
Aobvious inhibition zone, result of extraction is stronger, and (b) in fiber surface and surrounding have a large amount of bacteriums, this illustrate increase fiber in resist
Bacterium medicament contg can effectively improve the bacteriostasis property of fiber.Comparison diagram 3 and Fig. 4, pure Sorbsan is to Staphylococcus aureus
Bacterium has certain fungistatic effect, and cannot inhibit P. aeruginosa growth.Have largely in Fig. 5 (a) and Fig. 6 (a) plate
Experimental bacteria growth, illustrate common gauze cannot be hindered under dry conditions staphylococcus aureus and pseudomonas aeruginosa penetrate and
Growth.There are a small number of bacterium colonies in Fig. 5 (b) plate, and clump count is more on Fig. 6 (b) plate, illustrates Sorbsan in dry state item
There is more preferably resistance bacterium property to staphylococcus aureus under part and three repeated experiments result is almost the same, this may be since leather is blue
Family name's positive bacteria is different with the membrane structure of Gram-negative bacteria, and the mechanism of action and effect between Sorbsan are different.
It is grown in Fig. 5 (c, d) and Fig. 6 (c, d) plate without experimental bacteria, illustrates the algae for being grafted chlorhexidine gluconate under dry conditions
Sour calcium fiber has good resistance bacterium property to two kinds of experimental bacterias, and the content for being grafted antibacterials is higher, and resistance bacterium property is better.Fig. 7-10
In, SEM scanning figure show drug-loading fibre prepared by two kinds of embodiments to staphylococcus aureus and Pseudomonas aeruginosa all have compared with
Good absorption inhibitory effect, there are more dead thallus for fiber surface.In Figure 11,2960cm-1The absorption at place is weaker, reason
In " Egg box " structure, the stretching vibration of C-H on hexatomic ring is limited, so that dipole moment variation is smaller, therefore absorption peak is weaker.
3500cm-1The stretching vibration of O-H is also limited on place's hexatomic ring, and the position of O-H stretching vibration peak is mobile to lower wave number, together
When observe that O-H stretching vibration peak broadens in calcium alginate fibre, illustrate only part hydroxyl participate in coordination, other hydroxyl phases
Mutually association, higher wave number formed absorb, and with lower wave number overlap of peaks and peak shape is broadened.The result shows that: after fiber carries medicine,
Therebetween there are hydrogen bond actions, and carry medicine and will not influence " Egg box " structure of fibrous inside, the i.e. stabilization to fiber itself
Property and mechanical property have no significant effect.
Embodiment 2
A kind of alginate fibre preparation method of the antibacterials of class containing Chlorhexidine, the described method comprises the following steps:
Step 1: 150L water and high-speed stirred are added into reactor, while being slowly added to 5-6kg sodium alginate/potassium powder
End obtains the spinning solution that mass fraction is 3.2-3.8%, and temperature range is 45-65 DEG C, continues to stir, 1000mL mass point is added
The monoethanolamine HCI solution 0.5-1.0L that the chlorhexidine gluconate solution and concentration that number is 20% are 10-20mg/mL, fills
Point stirring and dissolving simultaneously reacts, spinning solution is obtained by filtration.
Step 2: wet-spinning frame is used, stoste is squeezed into concentration into metering pump, filter from spinning head (10000 hole)
CaCl of the range 2.5%~5.0%2In coagulation tank, through CaCl2Solidification liquid makes its stabilization, stream plus replenisher in process of setting
CaCl2The chlorhexidine gluconate solution that aqueous solution liquid (concentration is consistent with solidification liquid) and 1000mL mass fraction are 20%.
Step 3: stoste spinneret, one-off drawing, succeeding stretch after coagulating bath obtain fiber first product, and spinning speed exists
100m/min or less.
Step 4: respectively through the ethanol solution 2-3 times immersion that content is 35%-95%, each 2h soaks fiber first product every time
Centrifugal dehydration after bubble, it is final it is rolled, be dried to obtain finished fiber, wherein ethanol solution is reusable.Pass through control
Concentration of alcohol, soaking time respectively obtain the Sorbsan for carrying that medicine content is 23mg/g, 79mg/g.
Embodiment 3
A kind of alginate fibre preparation method of the antibacterials of class containing Chlorhexidine, the described method comprises the following steps:
Step 1: 150L water and high-speed stirred are added into reactor, while being slowly added to 5-6kg sodium alginate/potassium powder
End obtains the spinning solution that mass fraction is 3.2-3.8%, and temperature range is 45-65 DEG C, continues to stir, 1000mL mass point is added
The glutaraldehyde solution 0.5-0.6L that the chlorhexidine gluconate solution and concentration that number is 20% are 1.0%, is sufficiently stirred dissolution simultaneously
It reacts, spinning solution is obtained by filtration.
Step 2: wet-spinning frame is used, stoste is squeezed into concentration into metering pump, filter from spinning head (10000 hole)
CaCl of the range 2.5%~5.0%2In coagulation tank, through CaCl2Solidification liquid makes its stabilization, stream plus replenisher in process of setting
CaCl2The chlorhexidine gluconate solution that aqueous solution liquid (concentration is consistent with solidification liquid) and 1000mL mass fraction are 20%.
Step 3: stoste spinneret, one-off drawing, succeeding stretch after coagulating bath obtain fiber first product, and spinning speed exists
100m/min or less.
Step 4: respectively through the ethanol solution 2-3 times immersion that content is 35%-95%, each 2h soaks fiber first product every time
Centrifugal dehydration after bubble, it is final it is rolled, be dried to obtain finished fiber, wherein ethanol solution is reusable.Pass through control
Concentration of alcohol, soaking time respectively obtain the Sorbsan for carrying that medicine content is 23mg/g, 79mg/g.
Comparing embodiment 1-3, which is carried when medicine content is 23mg/g, sees the resistance bacterium the performance test results of staphylococcus aureus
Figure 12 is cultivated for 24 hours after throwing off sample, it is known that: crosslinking agent is that fungistatic effect is Dopamine hydrochloride solution > monoethanolamine hydrochloride
> glutaraldehyde.
Embodiment 4
A kind of alginate fibre preparation method of the antibacterials of class containing Chlorhexidine, the described method comprises the following steps:
Step 1: the pure alginate fiber for weighing 2.0g is laid in the glass dish of diameter 9cm, and suitably fixed；
Step 2: the glutaraldehyde solution 0.5-0.6L of sprinkling 1.0% on alginate fiber surface is obtained containing grafting agent
Alginate fibre；
Step 3: measuring the 20% chlorhexidine gluconate solution of 1.0mL, to analyze methanol constant volume to 25mL, using spray
It is uniformly sprayed on the alginate fibre surface containing grafting agent by leaching equipment, and the freeze-day with constant temperature 2h at 60 DEG C is obtained containing glucose
The alginate fiber of sour Chlorhexidine；
Step 4: the alginate fiber containing chlorhexidine gluconate is placed in the ethyl alcohol that volume fraction is 20%-60%
In solution successively washing, same direction stir 10s, after taking-up at 60 DEG C freeze-day with constant temperature 2h；
Step 5: by the fiber after drying is rolled and combing, finished fiber is obtained, wherein the repeatable benefit of ethanol solution
With.It is respectively obtained by control concentration of alcohol, soaking time and carries the Sorbsan that medicine content is 23mg/g, 79mg/g.
Embodiment 5
A kind of alginate fibre preparation method of the antibacterials of class containing Chlorhexidine, the described method comprises the following steps:
Step 1: the pure alginate fiber for weighing 2.0g is laid in the glass dish of diameter 9cm, and suitably fixed；
Step 2: it in the Dopamine hydrochloride solution 0.4-0.5L of alginate fiber surface sprinkling 30-40ug/mL, obtains
Alginate fibre containing grafting agent；
Step 3: measuring the 20% chlorhexidine gluconate solution of 1.0mL, to analyze methanol constant volume to 25mL, using spray
It is uniformly sprayed on the alginate fibre surface containing grafting agent by leaching equipment, and the freeze-day with constant temperature 2h at 60 DEG C is obtained containing glucose
The alginate fiber of sour Chlorhexidine；
Step 4: the alginate fiber containing chlorhexidine gluconate is placed in the ethyl alcohol that volume fraction is 20%-60%
In solution successively washing, same direction stir 10s, after taking-up at 60 DEG C freeze-day with constant temperature 2h；
Step 5: by the fiber after drying is rolled and combing, finished fiber is obtained, wherein the repeatable benefit of ethanol solution
With.It is respectively obtained by control concentration of alcohol, soaking time and carries the Sorbsan that medicine content is 23mg/g, 79mg/g.
Embodiment 6
A kind of alginate fibre preparation method of the antibacterials of class containing Chlorhexidine, the described method comprises the following steps:
Step 1: 150L water and high-speed stirred are added into reactor, while being slowly added to 5-6kg sodium alginate/potassium powder
End obtains the spinning solution that mass fraction is 3.5% or so, and temperature range is 45-65 DEG C, continues to stir, 0.14-0.16kg is added
The chlorhexidine acetate and concentration of 92% or more purity are the Dopamine hydrochloride solution 0.4-0.5L of 30-40ug/mL, are sufficiently stirred molten
It solves and reacts, spinning solution is obtained by filtration.
Step 2: wet-spinning frame is used, stoste is squeezed into concentration into metering pump, filter from spinning head (10000 hole)
CaCl of the range 2.5%~5.0%2In coagulation tank, through CaCl2Solidification liquid makes its stabilization, stream plus replenisher in process of setting
CaCl2Aqueous solution liquid (concentration is consistent with solidification liquid, the chlorhexidine acetate of 92% or more purity containing 0.14-0.16kg).
Step 3: stoste spinneret, one-off drawing, succeeding stretch after coagulating bath obtain fiber first product, and spinning speed exists
100m/min or less.
Step 4: respectively through the ethanol solution 2-3 times immersion that content is 35%-95%, each 2h soaks fiber first product every time
Centrifugal dehydration after bubble, it is final it is rolled, be dried to obtain finished fiber, wherein ethanol solution is reusable.Pass through control
Concentration of alcohol, soaking time respectively obtain chlorhexidine acetate and carry the Sorbsan that medicine content is 79mg/g.
Figure 13,14 are respectively resistance bacterium the performance test results of the embodiment 6 to pseudomonas aeruginosa, staphylococcus aureus:
Figure 13 a, 14a points are blank control, there is bacterium growth in ware；Figure 13 b, 14b are 6 drug-loading fibre of embodiment, sterile life in ware
It is long.Show chlorhexidine acetate as drugloading rate also available preferable fungistatic effect.
Embodiment 7
A kind of alginate fibre preparation method of the antibacterials of class containing Chlorhexidine, the described method comprises the following steps:
Step 1: 150L water and high-speed stirred are added into reactor, while being slowly added to 5-6kg sodium alginate/potassium powder
End obtains the spinning solution that mass fraction is 3.2-3.8%, and temperature range is 45-65 DEG C, continues to stir, 0.14-0.16kg is added
The chlorhexidine acetate and concentration of 92% or more purity be 1.0% glutaraldehyde solution 0.5-0.6L, be sufficiently stirred dissolution and react,
Spinning solution is obtained by filtration.
Step 2: wet-spinning frame is used, stoste is squeezed into concentration into metering pump, filter from spinning head (10000 hole)
CaCl of the range 2.5%~5.0%2In coagulation tank, through CaCl2Solidification liquid makes its stabilization, stream plus replenisher in process of setting
CaCl2Aqueous solution (concentration is consistent with solidification liquid, the chlorhexidine acetate of 92% or more purity containing 0.14-0.16kg).
Step 3: stoste spinneret, one-off drawing, succeeding stretch after coagulating bath obtain fiber first product, and spinning speed exists
100m/min or less.
Step 4: respectively through the ethanol solution 2-3 times immersion that content is 35%-95%, each 2h soaks fiber first product every time
Centrifugal dehydration after bubble, it is final it is rolled, be dried to obtain finished fiber, wherein ethanol solution is reusable.
Embodiment 8
A kind of alginate fibre preparation method of the antibacterials of class containing Chlorhexidine, the described method comprises the following steps:
Step 1: the pure alginate fiber for weighing 2.0g is laid in the glass dish of diameter 9cm, and suitably fixed；
Step 2: it in the Dopamine hydrochloride solution 0.4-0.5L of alginate fiber surface sprinkling 30-40ug/mL, obtains
Alginate fibre containing grafting agent；
Step 3: the acetic acid of 0.56mg/mL is uniformly sprayed on the alginate fibre surface containing grafting agent using sprinkling equipment
Chlorhexidine methanol solution 25mL, the freeze-day with constant temperature 2h at 60 DEG C, obtains the alginate fiber containing chlorhexidine acetate；
Step 4: the alginate fiber containing chlorhexidine acetate is placed in the ethanol solution that volume fraction is 20%-60%
In successively washing, same direction stir 10s, after taking-up at 60 DEG C freeze-day with constant temperature 2h；
Step 5: by the fiber after drying is rolled and combing, finished fiber is obtained, wherein the repeatable benefit of ethanol solution
With.
Embodiment 9
A kind of alginate fibre preparation method of the antibacterials of class containing Chlorhexidine, the described method comprises the following steps:
Step 1: 150L water and high-speed stirred are added into reactor, while being slowly added to 5-6kg sodium alginate/potassium powder
End obtains the spinning solution that mass fraction is 3.2-3.8%, and temperature range is 45-65 DEG C, continues to stir, 0.14-0.16kg is added
The chlorhexidine acetate and concentration of 92% or more purity are the monoethanolamine HCI solution 0.5-1.0L of 10-20mg/mL, are sufficiently stirred
It mixes dissolution and reacts, spinning solution is obtained by filtration.
Step 2: wet-spinning frame is used, stoste is squeezed into concentration into metering pump, filter from spinning head (10000 hole)
CaCl of the range 2.5%~5.0%2In coagulation tank, through CaCl2Solidification liquid makes its stabilization, stream plus replenisher in process of setting
CaCl2Aqueous solution liquid (concentration is consistent with solidification liquid, the chlorhexidine acetate of 92% or more purity containing 0.14-0.16kg).
Step 3: stoste spinneret, one-off drawing, succeeding stretch after coagulating bath obtain fiber first product, and spinning speed exists
100m/min or less.
Step 4: respectively through the ethanol solution 2-3 times immersion that content is 35%-95%, each 2h soaks fiber first product every time
Centrifugal dehydration after bubble, it is final it is rolled, be dried to obtain finished fiber, wherein ethanol solution is reusable.
Embodiment 10
A kind of alginate fibre preparation method of the antibacterials of class containing Chlorhexidine, the described method comprises the following steps:
Step 1: the pure alginate fiber for weighing 2.0g is laid in the glass dish of diameter 9cm, and suitably fixed；
Step 2: the glutaraldehyde solution 0.5-0.6L of sprinkling 1.0% on alginate fiber surface is obtained containing grafting agent
Alginate fibre；
Step 3: the acetic acid of 0.56mg/mL is uniformly sprayed on the alginate fibre surface containing grafting agent using sprinkling equipment
Chlorhexidine methanol solution 25mL, the freeze-day with constant temperature 2h at 60 DEG C, obtains the alginate fiber containing chlorhexidine acetate；
Step 4: the alginate fiber containing chlorhexidine acetate is placed in the ethanol solution that volume fraction is 20%-60%
In successively washing, same direction stir 10s, after taking-up at 60 DEG C freeze-day with constant temperature 2h；
Step 5: by the fiber after drying is rolled and combing, finished fiber is obtained, wherein the repeatable benefit of ethanol solution
With.
Hygroscopicity is that can fastidious fiber as an important indicator of superior bio dressing.Good hygroscopicity is to ensure
The essential condition of wound healing.As shown in Table 1, it is grafted absorption of the Sorbsan of antibacterials to distilled water and physiological saline
There are larger differences for rate, and being grafted drug has good moisture pick-up properties to physiological saline, illustrate to can be very good to absorb wound exudation
Liquid, the fiber for not carrying medicine also have this effect.As shown in Table 2, grafting antibacterials do not substantially change the stretching spy of fiber
Property.
Study on Hygroscopicity result of 1 embodiment of table, 1 test thread to distilled water and physiological saline
2 test thread tensile property test result of table
The preferred embodiment of the present invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for the common invention personnel of this field
For, without departing from the inventive concept of the premise, several deformations can also be made, improves and substitutes, these belong to this hair
Bright protection scope.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of alginate fibre preparation method of the antibacterials of class containing Chlorhexidine, which is characterized in that the method is with hydrochloric acid
Dopamine or other or amine salt or glutaraldehyde as cross linker carry out grafting processing to alginate fibre, connect chlorhexidine gluconate or
Chlorhexidine acetate, obtains the alginate fibre of the antibacterials of class containing Chlorhexidine, and grafting method includes impregnating or spraying.
2. according to the method described in claim 1, it is characterized by: the described method comprises the following steps:
Step 1: being added the obtained spinning solution of sodium alginate/potassium, continue to stir in water whipping process, be added gluconic acid chlorine oneself
Fixed or chlorhexidine acetate and crosslinking agent, are sufficiently stirred dissolution and react, spinning solution is obtained by filtration；
Step 2: wet-spinning frame is used, spinning solution is squeezed into CaCl2In the coagulation tank of solidification liquid, stream plus benefit in process of setting
Filling liquid CaCl2Solidification liquid and chlorhexidine gluconate or chlorhexidine acetate；
Step 3: stoste spinneret, one-off drawing, succeeding stretch after coagulating bath obtain fiber first product；
Step 4: fiber first product is respectively through alcohol solution dipping, centrifugal dehydration after impregnating every time, final rolled, dry
Obtain finished fiber.
3. according to the method described in claim 2, it is characterized by: the step 1 crosslinking agent is Dopamine hydrochloride solution, salt
Sour dopamine solution mass concentration is 30-40 ug/mL, Dopamine hydrochloride solution and water volume ratio 0.4/150-0.5/150；
Or the step 1 crosslinking agent is monoethanolamine hydrochloride, monoethanolamine hydrochloride mass concentration is 10-20 mg/mL, salt
Sour dopamine solution and water volume ratio 0.5/150-1/150；
Or the step 1 crosslinking agent is glutaraldehyde, glutaraldehyde mass concentration is 1.0%, glutaraldehyde solution and water volume ratio 0.5/
150-0.6/150。
4. according to the method described in claim 3, it is characterized by: the sodium alginate/potassium and water solid-to-liquid ratio are 0.033-
0.04(kg/L)；Step 1 chlorhexidine gluconate liquid quality fraction is 20%, and the volume ratio of additional amount and water is 1:150,
Step chlorhexidine digluconate additional amount and the volume ratio of water are 1:150 or step 1 chlorhexidine acetate solution quality point
Number is 92% or more, and the solid-to-liquid ratio of additional amount and water is 0.14/150-0.16/150(kg/L), step chlorhexidine diacetate adds
The solid-to-liquid ratio for entering amount and water is 0.14/150-0.16/150(kg/L).
5. according to the method described in claim 4, it is characterized by: the step 1 whipping temp range is 45-65 DEG C；Step
Two CaCl2Solidification liquid mass concentration is 2.5%-5.0%；Spinning speed exists during step 3 spinneret, one-off drawing, succeeding stretch
100 m/min or less；Step 4 ethanol solution mass concentration is 35%-95%, is impregnated 2-3 times, each 1.5-2.5 h.
6. according to the method described in claim 1, it is characterized by: the described method comprises the following steps:
Step A: alginate fiber is laid in plate, and fixed；
Step B: crosslinking agent is sprayed on alginate fiber surface, obtains the alginate fibre containing grafting agent；
Step C: chlorhexidine gluconate or acetic acid are uniformly sprayed on the alginate fibre surface containing grafting agent using sprinkling equipment
The methanol solution of Chlorhexidine, freeze-day with constant temperature obtain the alginate fiber containing chlorhexidine gluconate or chlorhexidine acetate；
Step D: by the alginate fiber containing chlorhexidine gluconate or chlorhexidine acetate be placed in ethanol solution successively washing,
Freeze-day with constant temperature is taken out in stirring；
Step E: by the fiber after drying it is rolled and combing, obtain finished fiber.
7. according to the method described in claim 6, it is characterized in that, the step B crosslinking agent is Dopamine hydrochloride solution, hydrochloric acid
Dopamine solution mass concentration is 30-40 ug/mL, and Dopamine hydrochloride solution and alginate fiber liquid-solid ratio are 0.4/2-
0.5/2(L/g)；Step C sprays the chlorhexidine acetate methanol solution of 0.56 mg/mL, chlorhexidine acetate methanol solution and alginic acid
Salt fiber liquid-solid ratio is (20-30)/2(mL/g).
8. according to the method described in claim 6, it is characterized by: the step B crosslinking agent is Dopamine hydrochloride solution, hydrochloric acid
Dopamine solution mass concentration is 30-40 ug/mL, and Dopamine hydrochloride solution and alginate fiber liquid-solid ratio are 0.4/2-
0.5/2(L/g), step C chlorhexidine gluconate concentration of polymer solution is 20%, obtains grape to analyze methanol constant volume to 25mL
Chlorhexidine gluconate methanol solution is uniformly sprayed on the algae containing grafting agent using sprinkling equipment by saccharic acid Chlorhexidine methanol solution
Silicate fiber surface.
9. according to the method described in claim 6, glutaraldehyde is molten it is characterized by: the step B crosslinking agent is glutaraldehyde solution
Liquid mass concentration is 1.0%, and glutaraldehyde solution and alginate fiber liquid-solid ratio are 0.5/2-0.6/2(L/g), step C sprinkling
The chlorhexidine acetate methanol solution of 0.56 mg/mL, chlorhexidine acetate methanol solution and alginate fiber liquid-solid ratio are (20-
30)/2(mL/g).
10. according to the method described in claim 6, it is characterized by: the step C or step D freeze-day with constant temperature temperature are 60-70
DEG C, drying time is 2-2.5 h.
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| CN113244436A (en) * | 2021-03-23 | 2021-08-13 | 安徽医科大学 | Chlorhexidine and catecholamine copolymerized antibacterial coating and preparation method and application thereof |
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