WO2012062139A1

WO2012062139A1 - Fiber wound dressing having antibacterial effect and preparation method therefor

Info

Publication number: WO2012062139A1
Application number: PCT/CN2011/078210
Authority: WO
Inventors: 王锐; 岑荣章; 张大伟; 王晓东; 黄宗海; 史福军
Original assignee: 广东百合医疗科技有限公司; 南方医科大学珠江医院
Priority date: 2010-11-10
Filing date: 2011-08-10
Publication date: 2012-05-18
Also published as: CN102462860A

Abstract

A fiber wound dressing having an antibacterial effect and a preparation method therefor. The dressing is a fabric made of fibers having a surface coated with a polyhexamethylene biguanidine solvent or a polyhexamethylene biguanidine solution as an antibacterial agent, wherein the concentration of polyhexamethylene biguanidine coated in the dressing is 400-4000ppm. The fiber wound dressing contains high-concentration polyhexamethylene biguanidine having a broad-spectrum antibacterial effect, is applicable to treatment of a chronic wound, and can be used for consecutive 7 days or longer. The wound dressing has no silver resistance and toxic side effect, and can effectively prevent the infection caused by various bacteria and microorganisms to a wound.

Description

Fiber wound dressing with antibacterial effect and preparation method thereof

The present invention relates to a fibrous wound dressing having an antibacterial action, and a method of preparing a fibrous wound dressing containing an antibacterial agent. Background technique

It is well known that chronic wounds are very common in bacterial infection during the healing phase. Therefore, professional caregivers often use anti-infective dressings to treat wounds that may be infected. Currently, the most common antimicrobial dressings are silver-containing dressings. However, it is important to note that some patients are resistant to silver and that silver-containing antimicrobial dressings have toxic side effects.

Therefore, polyhexamethylene biguanide (PHMB), which has a broad-spectrum antibacterial effect, has been introduced, and attempts have been made to add polyhexamethylene biguanide as an antibacterial agent to medical dressings.

U.S. Patent No. 6,369,289 discloses a method of preparing a cellulose bandage containing PHMB by winding a cellulose stretcher onto a porous drum, inserting it into a closed container, adding PHMB to the container and circulating the solution. Thus, PHMB is applied to the cellulose bandage, and finally the cellulose bandage contains 1500-2500 f) m of PHMB.

European Patent EP1473047 discloses a microbial cellulose wound dressing containing PHMB containing no less than 7900 ppm of PHMB.

U.S. Patent No. 2,004,028, 925, and International Patent Application No. PCT/US2003/0325, the disclosure of which is incorporated herein incorporated by reference in its entire entire entire entire entire entire entire entire entire entire content The PHMB is immersed in the inner layer, the weave! Contains 1500-3500ppm PHMB.

Chinese Patent No. 20091-0029039.5 discloses a medical antibacterial gauze and a manufacturing method thereof. The method comprises adding clear water to a retort and adding PHMB so that the gauze wound on the hollow cylinder absorbing the solution containing PHMB, and the final fabric contains 0.1%. -0.35% PHMB.

The antibacterial fabric obtained in view of the above invention contains only a low concentration of polyhexamethylene diguanidine, and for chronic wounds, the antibacterial wound dressing is generally expected to be used continuously for 7 days or longer. At the same time, with the focus on silver resistance and its toxic side effects, it is urgent to develop a fiber-based dressing containing an antibacterial component of a high concentration of polyhexamethylene double fox. but Yes, polyhexamethylene 3⁄4胍 is water-soluble, so it is difficult to add polyhexamethylene biguanide to the fiber structure during spinning, and at the same time, it is exposed to water during the preparation of most wound dressings. The content of polyhexamethylene double fox in the fabric is difficult to control.

Accordingly, the present invention has an object of effectively spraying a high concentration of polyhexamethylene biguanide on a fabric or fiber to obtain a fiber-based wound dressing containing a high concentration of polyhexamethylene double fox. Summary of the invention

The present invention provides a fibrous wound dressing having an antibacterial action, comprising polyhexamethylene double vein as an antibacterial agent, which is a fabric made of fibers coated with a polyhexamethylene biguanide solution or sprayed. A fabric having a polyhexamethylene biguanide solution having a coating concentration of 400-40,000 ppm in the dressing.

In the wound dressing of the present invention, since it contains a high concentration of polyhexamethylene biguanide, it can be used as an antibacterial wound dressing for 7 days or longer in order to be suitable for chronic wounds. The polyhexamethylene biguanide is coated in the dressing at a concentration of

800-37000 ppm, preferably 2000-33000 ppm, most preferably 4000-25000 ppm.

The fiber used in the present invention may be a non-gelled fiber, and the polyhexamethylene biguanide solution sprayed on the surface thereof is a water-soluble solution or a solvent-type solution. It may also be a gellable fiber, and the polyhexamethylene biguanide solution sprayed on the surface thereof is a mixed solution of an aqueous solution and a solvent, and the mixed solution is a solvent type solution, and the ratio of water to solvent in the mixed solution For: 1: 20 to 16: 20. For fibers or fabrics that do not gel, spray an aqueous solution of polyhexamethylene biguanide, and for gelled fibers or fabrics, spray only a non-aqueous solution of polyhexamethylene biguanide or a solution containing a small amount of water. To prevent gelation of the outer surface of the fiber, and to lose the fluffy and soft hand of the fiber or fabric. Preferably, the polyhexamethylene biguanide is first dissolved in water and then mixed with a solvent, such as ethanol, so that the fiber or fabric does not gel, and the solvent is easier to evaporate than water, so it is easy to dry.

The wound dressing according to the present invention may be formed by spraying PHMB on the fiber and then processing the nonwoven fabric, or directly spraying the PHMB on the fabric, preferably by spraying the fiber and then performing the non-woven process. .

After the fiber or fabric is sprayed with the PHMB solution, especially after the high concentration solution, the surface of the fiber or fabric will be hard, which has little effect on the function of the dressing, but the hand feels a bit stiff. Therefore, although a dressing containing PHMB can be prepared by directly spraying a PHMB solution onto a fabric, the best effect is to spray on the fibers. Because the fiber is sprayed into a dressing package after the PHMB solution is sprayed, combed, screened and acupuncture. The fiber softens during this process by mechanical action. There will be a small amount of PHMB loss during this process, but it is not very significant.

An ideal spray is to spray the PHMB mixed solution directly onto the tow in continuous spinning. The most ideal spraying position is that the fiber bundle after spraying in the dryer can be directly dried by the dryer and then further softened by crimping/cutting the test fiber.

Another key to the present invention is the use of a high concentration of PHMB solution to spray a higher concentration of aqueous PHMB solution or mixed solution onto the fibers or fabric. Generally, the market can buy 80% of PHMB at high concentration. At this concentration, it is difficult to dilute directly with an alcohol solvent. It is preferred to first dissolve the material in water to about 70%, and then dilute with an alcohol solvent. In general, 10-65% of PHMB is better, and 15-60% is best.

The gellable fiber is alginate fiber, carboxymethyl cellulose fiber or carboxymethyl chitosan fiber. The gellable fiber is alginate fiber, carboxymethyl cellulose fiber, acylated chitosan fiber or carboxymethyl chitosan fiber.

The fabric sprayed with the polyhexamethylene biguanide solution is a fabric coated with a polyhexamethylene biguanide solution on one side or both sides.

The fabric coated with the polyhexamethylene biguanide solution is a non-woven fabric, a woven fabric or a knitted fabric.

The present invention provides a method for preparing a fibrous wound dressing having an antibacterial action, the method comprising the steps of:

Spraying the polyhexamethylene biguanide solution on the surface of the fiber in a fluffy state by atomization, and coating the polyhexamethylene biguanide at a concentration of 400-40000 ppm; mixing the poly six by stirring or shaking during spraying Methylene biguanide solution;

The resulting sprayed polyhexamethylene biguanide fibers are naturally dried at room temperature; the dried fibers are processed into a fabric by a nonwoven, woven or knitted process. Moreover, the present invention also provides a method for preparing a fibrous wound dressing having an antibacterial action, the method comprising the steps of:

Spraying the polyhexamethylene biguanide solution on the surface of the fiber tow in a continuous spinning state in an atomized form; the polyhexamethylene biguanide coating concentration is between 400-40000 ppm; Mixing the polyhexamethylene biguanide solution by continuous stirring or shaking during the coating process;

The obtained fiber strands of the sprayed polyhexamethylene biguanide are dried in a dryer in a spinning process;

The fibers obtained after drying are cut by crimping and then processed into a fabric by a nonwoven process.

In another aspect, the present invention provides a method of preparing a fibrous wound dressing having an antibacterial effect, the method comprising the steps of:

The polyhexamethylene biguanide solution is uniformly sprayed on the single surface or the double surface of the fabric which is in a flat state under tension; the polyhexamethylene biguanide coating concentration is between 400-40000 ppm; continuously stirring during the spraying process Or oscillating to mix the polyhexamethylene biguanide solution; the obtained sprayed polyhexamethylene biguanide fabric is naturally dried at room temperature. Further, the present invention provides a method for preparing a fibrous wound dressing having an antibacterial action, the method further comprising the steps of: cutting the obtained fabric into a suitable size, and sterilizing and encapsulating to obtain the dressing.

In addition, in the method for preparing a wound dressing having antibacterial action, the spraying device for providing a nozzle on the full width of the fabric, the method of moving the spraying device by spraying the fabric during spraying, or the moving of the fabric by the spraying device can be used. Methods.

The present invention relates to a fibrous wound dressing having an antibacterial effect, a fabric made of fibers coated with a solution of polyhexamethylene biguanide or a fabric sprayed with a solution of polyhexamethylene biguanide, said polyhexamethylene The base is applied to the dressing in a concentration of 400-40000ppm as a wound dressing. Because the fiber wound dressing contains high concentration of polyhexamethylene double M antibacterial ingredient, it is especially suitable for chronic wound treatment and can be used continuously for 7 days or more. For a long time, as a wound dressing containing polyhexamethylene double fox with broad-spectrum antibacterial effect, there is no silver anti-drug and other toxic side effects of other antibacterial dressings, which can effectively prevent various bacteria and microorganisms from being wounded. infection. DRAWINGS

Figure 1 shows the zone of inhibition of a dressing with a pH of 400 ppm in an E. coli dish for 1 day.

Figure 2 is a graph showing the zone of inhibition of the dressing with a PHMB content of 400 ppm after 7 days in an E. coli dish. Figure 3 is a graph showing the inhibition zone of a dressing having a PHMB content of 40,000 ppm after one day in a Staphylococcus aureus culture dish.

Figure 4 shows the zone of inhibition of the dressing with a PHMB content of 40000 ppm after 7 days in a Staphylococcus aureus culture dish.

Figure 5 shows the zone of inhibition of the dressing with a PHMB content of 6000 ppm after 1 day in a P. aeruginosa culture dish.

Figure 6 shows the zone of inhibition of the dressing with a PHMB content of 6000 ppm after 7 days in a P. aeruginosa culture dish.

Figure 7 shows the zone of inhibition of the dressing with a PHMB content of 1000 ppm after 1 day in an E. coli dish.

Figure 8 shows the zone of inhibition of the dressing with a PHMB content of 1000 ppm after 7 days in an E. coli dish.

Figure 9 shows the zone of inhibition of the dressing with a PHMB content of 8000 ppm after 1 day in a Staphylococcus aureus culture dish.

Figure 10 shows the zone of inhibition of the dressing with a PHMB content of 8000 ppm after 7 days in a Staphylococcus aureus culture dish.

Fig. 11 is a view showing the inhibition zone of the dressing having a PHMB content of 14000 ppm after one day in a P. aeruginosa culture dish.

Fig. 12 is a view showing the zone of inhibition of the dressing with a PHMB content of 14000 ppm after 7 days in a P. aeruginosa culture dish. Detailed ways

The technical solutions of the present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.

Example 1

The steps of preparing a wound dressing by spraying the fiber with a solution containing PHMB:

1. Spread 10kg of high M-type calcium alginate fiber evenly on a flat tabletop.

2. Prepare 10 ml of 40% aqueous PHMB solution, add 90 ml of absolute ethanol, and prepare a total volume of 100 ml of solution. The total weight of PHMB is about 4 g.

3. Spray the solution onto the fibers and keep spinning the fibers to ensure that the solution containing PHMB is evenly sprayed onto the fibers. 4. Place the sprayed fibers in an oven with an air blast system at 75 ° C and dry the fibers to a moisture content of 20%.

5. The dried fibers obtained in the above 4 are prepared into a nonwoven fabric by a process such as carding, laying, and needle punching.

6. Cut the non-woven fabric into a 10x10cm dressing, package it and sterilize it with gamma rays.

7. A dressing with a PHMB content of 400 ppm is obtained. Example 2

In order to observe the antibacterial property of the dressing, a certain amount of Escherichia coli was uniformly applied to the culture dish, and then the dressings obtained in Example 1 were respectively cut into 2x2 cm and placed therein, and cultured at a constant temperature of 37 ° C for 1 day or 7 days, respectively. The growth of bacteria on each plate was observed. Figure 1 shows the inhibition zone of a dressing with a pH of 400 ppm in an E. coli dish for 1 day. Figure 2 shows the zone of inhibition of a dressing with a pH of 400 ppm in an E. coli dish for 7 days. It can be seen that the dressing with a pH of 400 ppm still has good antibacterial properties after 7 days. Example 3

The steps of preparing a wound dressing by spraying a fabric with a solution containing PHMB:

1. Spread a high G-type calcium alginate fabric with a lm ² weight of 120 g on a flat tabletop.

2. Prepare 8 ml of a 60% aqueous solution of PHMB, and add 50 ml of absolute ethanol thereto to prepare a solution having a total volume of 58 ml.

3. Spray 50% of the above solution on one side of the fabric.

4. Turn the fabric over and spray 50% of the above solution on the other side.

5. Dry the fabric in an oven with a PHMB content of about 4.8g and a fabric weight ratio of 4% (40000 ppm).

6. Cut the fabric into a 10x10 cm dressing, encapsulate and sterilize with gamma rays.

7. A dressing with a PHMB content of 40000 ppm is obtained. Example 4

In order to observe the antibacterial properties of the dressing, uniformly apply a certain amount of gold in the culture dish. Staphylococcus, and then the dressings obtained in Example 3 were respectively cut into 2x2 cm and placed therein, and the growth of the bacteria on each plate was observed after incubating at 37 ° C for 1 day or 7 days, respectively. Figure 3 shows the zone of inhibition of the dressing with a PHMB content of 40,000 ppm after 1 day in a Staphylococcus aureus culture dish. Figure 4 shows the zone of inhibition of the dressing with a PHMB content of 40,000 ppm after 7 days in a Staphylococcus aureus culture dish. It can be seen that the dressing with a PHMB content of 40,000 ppm still has good antibacterial properties after 7 days. Example 5

A step of preparing a wound dressing by containing a solution of PHMB on the fibers in the spinning:

1. For the normal chitosan spinning process, the total fiber bundle (tow) dry weight can be calculated, for example 6 g/m.

2. Measure the linear velocity of the fiber, such as 20m/min. Thus, the dry weight of the tow per minute, such as 120 g/min, can be calculated.

3. The PHMB aqueous solution can be sprayed onto the tow during the spinning process. In the process

The higher the concentration of PHMB, the better. In this example, a 60% concentration of PHMB solution was used.

4. Adjust the spray nozzle to achieve a spray rate of 1.2g/min. The chitosan fiber produced at a coating speed of 1.2 g/min and a 60% PHMB solution contained 6 mg of PHMB per gram, i.e., 6000 ppm.

5. The fiber is made into a nonwoven fabric by a non-woven process at a suitable needling speed, and then cut, cut, packaged, and epoxidized to form a dressing.

6. A dressing with a PHMB content of 6000 ppm is obtained. Example 6

In order to observe the antibacterial property of the dressing, a certain amount of Pseudomonas aeruginosa was uniformly coated in the culture dish, and then the dressings obtained in Example 5 were respectively cut into 2×2 cm and placed therein, and cultured at a constant temperature of 37° C. for 1 day or 7 respectively. The growth of bacteria on each plate was observed after day. Figure 5 shows the zone of inhibition of the dressing with a PHMB content of 6000 ppm after 1 day in a P. aeruginosa culture dish. Figure 6 shows the zone of inhibition of the dressing with a PHMB content of 6000 ppm after 7 days in a P. aeruginosa culture dish. It can be seen that the dressing with a PHMB content of 6000 ppm remains after 7 days. Has good antibacterial properties. Example 7

The steps of preparing a wound dressing by a carboxymethyl chitosan fabric or an acylated chitosan fabric containing 10000 ppm PHMB:

1. Place lm ² carboxymethyl chitosan fabric or acylated chitosan fabric (120 g/m ² ) on a flat table top.

2. Weigh 24ml of 50% PHMB solution.

3. Add 100 ml of absolute ethanol.

4. Spray all the liquid on the fabric.

5. Make sure the solvent evaporates or the fabric is completely dry before proceeding to the next step.

6. The fabric was then cut, cut, packaged, and gamma sterilized to make a 10 x 10 cm dressing.

7. Get a dressing containing 10,000 ppm PHMB. Example 8

In order to observe the antibacterial property of the dressing, a certain amount of Escherichia coli was uniformly applied to the culture dish, and then the dressing obtained in Example 7 was cut into 2x2 cm and placed therein, and cultured at a constant temperature of 37 ° C for 1 day or 7 days, respectively. The growth of bacteria on each plate was observed. Figure 7 shows the inhibition zone of the dressing with a PHMB content of 1000 ppm in the E. coli dish for 1 day. Figure 8 shows the zone of inhibition of the dressing with a PHMB content of 1000 ppm in the E. coli dish for 7 days. It can be seen that the dressing with a PHMB content of 1000OOppm still has good antibacterial properties after 7 days. Example 9

The procedure for preparing a wound dressing by spraying a carboxymethylcellulose fabric with a solution containing 8000 ppm PHMB:

1. Place a lOxlOcm carboxymethylcellulose fabric (100 g/m ² ) on a flat table top.

2. Weigh 1.3ml of 60% PHMB solution.

3. Add 50 ml of absolute ethanol. 4. Spray 2 - the above solution on one side of the fabric.

5. Turn the fabric over and spray half of the above solution on the other side.

6. After the fabric is dried, it contains 0.8% by weight of PHMB.

7. The fabric is then packaged and gamma sterilized to form a dressing.

8. Get a dressing containing 8000 ppm PHMB. Example 10

In order to observe the antibacterial property of the dressing, a certain amount of Staphylococcus aureus was uniformly applied in the culture dish, and then the dressing obtained in Example 9 was cut into 2×2 cm and placed therein, and cultured at a constant temperature of 37° C. for 1 day or 7 respectively. The growth of bacteria on each plate was observed after day. Figure 9 shows the zone of inhibition of the dressing with a PHMB content of 8000 ppm after 1 day in a Staphylococcus aureus culture dish. Figure 10 shows the zone of inhibition of the dressing with a PHMB content of 8000 ppm after 7 days in a Staphylococcus aureus culture dish. It can be seen that the dressing with a PHMB content of 8000 ppm still has good antibacterial properties after 7 days. Example 11

Steps to prepare a wound dressing containing 14000 ppm PHMB:

1. For the normal high M-type calcium alginate process, the total fiber bundle (tow) dry weight can be calculated, for example 12 g/m.

2. Measure the linear velocity of the fiber, such as 20m/min. It is possible to calculate the dry weight per minute of the tow, such as 240g/min.

3. The PHMB aqueous solution can be sprayed onto the tow during the spinning process. The higher the concentration of PHMB in this process, the better. In this example, a 60% concentration of PHMB solution was used followed by twice the absolute ethanol. The PHMB content in this mixed solution was 20%.

4. Adjust the spray nozzle to achieve a spray rate of 21 ml/min. The efficiency of this spray method is generally around 80%, that is, only 16.8 ml/min of the mixture is sprayed onto the fibers. The calcium alginate fiber obtained at this rate and the above mixture contained 14 mg of PHMB per gram, g 卩 14,000 ppm.

5. The fiber is made into a non-woven fabric by a non-woven process at an appropriate needling speed, and then cut, cut, packaged, and epoxidized to form a dressing.

6. Get a dressing containing 8000 ppm PHMB. Example 12

In order to observe the antibacterial property of the dressing, a certain amount of Pseudomonas aeruginosa was uniformly coated in the culture dish, and then the dressings obtained in Example 11 were respectively cut into 2×2 cm and placed therein, and cultured at a constant temperature of 37° C. for 1 day or 7 respectively. The growth of bacteria on each plate was observed after day. Figure 11 shows the inhibitory zone of the dressing with a PHMB content of 14000 ppm after 1 day in a P. aeruginosa culture dish. Figure 12 shows the zone of inhibition of the dressing with a PHMB content of 14000 ppm after 7 days in a P. aeruginosa culture dish. It can be seen that the dressing with a PHMB content of 14000 ppm still has good antibacterial properties after 7 days.

Claims

Claim

A fibrous wound dressing having an antibacterial action, comprising polyhexamethylene biguanide as an antibacterial agent, characterized in that: the dressing is a fabric made of fibers coated with a solution of polyhexamethylene biguanide or A fabric sprayed with a polyhexamethylene biguanide solution having a coating concentration of 400-4000 ppm in the dressing.

The fibrous wound dressing having an antibacterial action according to claim 1, wherein the polyhexamethylene biguanide is applied in a dressing at a concentration of 800 to 37,000 ppm, preferably 2000 to 33,000 ppm, most preferably 4000-25000ppm.

3. The fibrous wound dressing having antibacterial action according to claim 1, wherein: the fiber may be a non-gelled fiber or a gelled fiber, preferably a gelled fiber, sprayed on the surface thereof. The polyhexamethylene biguanide solution is a water soluble solution or a solvent type solution.

4. The fibrous wound dressing having antibacterial action according to claim 1, wherein: the fiber is a gellable fiber, and the solution sprayed on the surface thereof is a mixture of a polyhexamethylene biguanide aqueous solution and a solvent. a type solution, the mixed solution is a solvent type solution, and the ratio of water to solvent in the mixture is 1:20 to 16:20.

The fibrous wound dressing having an antibacterial action according to claim 3, wherein the non-gelling fiber is viscose fiber or chitosan fiber.

6. The fibrous wound dressing having antibacterial action according to claim 4, wherein: the gellable fiber is alginate fiber, carboxymethyl cellulose fiber, acylated chitosan fiber or carboxyl group. Chitosan fiber.

The fibrous wound dressing having an antibacterial action according to any one of claims 1 to 6, wherein: the fabric coated with the polyhexamethylene biguanide solution is a single-sided or double-sided sprayed poly six Fabric of methylene biguanide solution.

The fibrous wound dressing having an antibacterial action according to any one of claims 1 to 6, wherein the fabric coated with the polyhexamethylene biguanide solution is a non-woven fabric, a woven fabric or a knitted fabric. Things.

9. A method of preparing a fibrous wound dressing having an antibacterial effect, the method comprising the steps of:

The polyhexamethylene biguanide mixed solution is prepared by using a polyhexamethylene biguanide aqueous solution and a solvent, and the ratio of water to solvent in the mixed solution is 1:20 to 16:20;

The polyhexamethylene biguanide mixed solution is sprayed on the surface of the fiber in a fluffy state while being continuously stirred; the polyhexamethylene biguanide coating concentration is between 400-40000 ppm;

The resulting sprayed polyhexamethylene biguanide fibers are naturally dried at room temperature; the dried fibers are processed into a fabric by a nonwoven, woven or knitted process.

10. A method of preparing a fibrous wound dressing having an antibacterial effect, characterized in that the method comprises the following steps:

The polyhexamethylene biguanide mixed solution is prepared by using a high polyhexamethylene biguanide aqueous solution and a solvent, and the ratio of water to solvent in the mixed solution is: 1:20 to 16:20;

The polyhexamethylene biguanide solution is sprayed on the surface of the fiber tow in a continuous spinning state while being continuously stirred; the polyhexamethylene biguanide coating concentration is between 400-40000 ppm;

11. A method of preparing a fibrous wound dressing having an antibacterial effect, characterized in that the method comprises the following steps:

The polyhexamethylene biguanide solution is uniformly sprayed while being uniformly sprayed on the single surface or the double surface of the fabric which is in a flat state under tension; the polyhexamethylene biguanide coating concentration is 400-40000 ppm;

A method for preparing a fibrous wound dressing having an antibacterial action according to claim 9 or 10 or 11, wherein the method

After cutting or processing the fabric, sterilizing and encapsulating, the dressing is obtained:

13. The method for preparing a fibrous wound dressing having an antibacterial action according to claim 11, wherein: the spraying device is provided with a nozzle over the full width of the fabric, and the method of moving the spraying device while spraying is used, or A method in which the fabric is moved while the spray device is fixed.