A waterproof liquid band-aid and a method for preparing the same

Abstract

The application relates to the field of medical dressings, in particular to a waterproof liquid band-aid and a preparation method thereof, which comprises xylan esterification derivatives, polyvinyl alcohol, castor oil, chitin / carbon nanoparticle microspheres, polyphenol substances, allicin, acetyl tri-butyl citrate, glycerol and a solvent. The liquid band-aid prepared by the application has excellent waterproof and breathable properties after film formation, and the tensile strength is greater than or equal to 8.90 MPa, and the mechanical properties and the antibacterial properties are excellent.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of medical dressings, and particularly relates to a waterproof liquid band-aid and a preparation method thereof. BACKGROUND

[0002] In daily life, various skin wounds such as cuts, abrasions and chaps will inevitably occur, and in the treatment process of the wounds, the application of wound dressings can protect the wounds from secondary damage and accelerate healing.

[0003] The use of wound dressings has been recorded for thousands of years, and people use Chinese herbal medicine, animal fat, honey and the like to cover wounds to close the wounds and promote healing. An ideal wound dressing should have good permeability and can effectively isolate the invasion of microorganisms; good mechanical properties to ensure the compliance of the user and the protection of irregular wounds; accelerate the formation of epithelial tissue and inhibit bacteria and inflammation.

[0004] Since the 20th century, traditional band-aids have been widely used and used to date due to their characteristics of compression hemostasis, protection of wound surface and convenient use, but they have poor waterproof and breathable effects and are inconvenient to use at joints. SUMMARY

[0005] The application aims at the above technical problems, and provides a waterproof liquid band-aid and a preparation method thereof.

[0006] The technical scheme adopted is as follows:

[0007] The waterproof liquid band-aid comprises the following components in parts by weight:

[0008] xylan esterification derivative, polyvinyl alcohol, castor oil, chitin / carbon nanoparticle microspheres, polyphenol, allicin, acetyl tri-butyl citrate, glycerol and solvent.

[0009] Further, the components comprise the following components in parts by weight:

[0010] xylan esterification derivative 5-10 parts, polyvinyl alcohol 4-8 parts, castor oil 1-3 parts, chitin / carbon nanoparticle microspheres 1-3 parts, polyphenol 0.5-1 part, allicin 0.1-0.5 part, acetyl tri-butyl citrate 1-2 parts, glycerol 0.05-0.1 part and solvent 70-90 parts.

[0011] Further, the xylan esterification derivative is the product after reaction of alkyl acyl halide, alkyl acid anhydride and alkyl carboxylic acid with xylan.

[0012] Further, the alkyl acyl halide, alkyl acid anhydride and alkyl carboxylic acid have ≥4 carbon atoms.

[0013] Further, the alkyl acyl halide is selected from any one or more of butyryl chloride, valeryl chloride, caproyl chloride, heptyl chloride, octanoyl chloride, nonanoyl chloride, decanoyl chloride;

[0014] The alkyl acid anhydride is any one or more of butyric anhydride, valeric anhydride, caproic anhydride, heptyl anhydride, octanoic anhydride, nonanoic anhydride, decanoic anhydride, succinic anhydride, glutaric anhydride, adipic anhydride, pimelic anhydride, suberic anhydride, sebacic anhydride.

[0015] The alkyl carboxylic acid is any one or more of butyric acid, valeric acid, caproic acid, heptyl acid, octanoic acid, nonanoic acid, decanoic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, sebacic acid.

[0016] Further, the xylan esterified derivative is xylan butyric acid ester.

[0017] Further, the preparation method of the chitin / carbon nanoparticle microsphere is as follows:

[0018] The chitin powder is dispersed in a solvent composed of sodium hydroxide, urea and water, and after multiple freeze-thawing, a chitin solution is obtained; carbon nanoparticles are added into the chitin solution, and stirred uniformly at 0-5 DEG C to obtain a chitin / carbon nanoparticle composite solution; Span 85 is added into isooctane, and after being stirred uniformly at 0-5 DEG C, the chitin / carbon nanoparticle composite solution is added, and the stirring is warmed to 60-80 DEG C for 20-50 min; the system is adjusted to neutral pH with hydrochloric acid, and after being left to stand and separated, the isooctane is separated out; the water phase is poured into ethanol under low-speed stirring, and stirred and dispersed for 1-3 h; the solid product is separated out by filtration; the solid product is soaked in t-butyl alcohol for 24-48 h, and filtered again; after being washed with water, the product is freeze-dried.

[0019] Further, the polyphenolic substance is any one or more of catechin, epicatechin, gallocatechin, epigallocatechin, epicatechin gallate and epigallocatechin gallate.

[0020] Further, the solvent comprises butyl acetate and ethanol, and the weight ratio of the butyl acetate and the ethanol is 1-5:1-5.

[0021] The application provides a preparation method of a waterproof liquid band-aid.

[0022] The xylan esterified derivative, polyvinyl alcohol, castor oil, chitin / carbon nanoparticle microsphere, polyphenolic substance, allicin, acetylcitric acid tributyl ester and glycerol are added into a solvent, mixed uniformly, and then sealed and stored.

[0023] The application has the following beneficial effects:

[0024] The application provides a waterproof liquid band-aid, xylan film has good biocompatibility and liquid barrier property, has important application value in the fields of drug sustained release, packaging materials and coating, the inventor increases the solubility of xylan in a solvent and waterproof performance through esterification modification of hydroxyl groups on the xylan, reduces the tendency of xylan to form a strong hydrogen bond combination network, improves the mechanical property of the formed film, and makes the xylan become a good film forming material of the liquid band-aid, has better film forming performance with the aid of polyvinyl alcohol, chitin / carbon nanoparticle microspheres, polyphenols and allicin can realize antibacterial or bacteriostatic action through various mechanisms, including mechanical damage of bacterial cell wall / cell membrane, bacterial oxidative stress (active oxygen dependent and active oxygen independent), lipid extraction, bacterial metabolic growth inhibition, wrapping and isolation, etc., bacteria can be killed and inflammation can be eliminated through the synergistic effect of the three, and the healing of a wound is accelerated, and the addition of chitin / carbon nanoparticle microspheres and polyphenols can also reduce the irritating smell of allicin and reduce the discomfort of a user, the liquid band-aid prepared in the application has excellent waterproof and breathable performance after film forming, and the tensile strength is greater than or equal to 8.90 MPa, and the mechanical property and bacteriostatic property are excellent. BRIEF DESCRIPTION OF DRAWINGS

[0025] Figure 1 The figure is a photo of the liquid band-aid prepared in example 1 in the application after film forming. DETAILED DESCRIPTION

[0026] If the specific conditions are not indicated in the examples, the conventional conditions or the conditions recommended by the manufacturer are used. If the manufacturers of the reagents or instruments are not indicated, the conventional products that can be obtained through market purchase are used. The technologies not mentioned in the application refer to the prior art, and the following examples and comparative examples are parallel tests, and the same treatment steps and parameters are used.

[0027] Xylan butyrate: self-made;

[0028] Polyvinyl alcohol 400: Guangzhou Xiangmei Chemical Technology Co., Ltd.;

[0029] Castor oil: Klein (Shandong) Biological Technology Co., Ltd.;

[0030] Chitin / carbon nanoparticle microspheres: self-made;

[0031] Catechin: Shaanxi Haochen Biological Technology Co., Ltd.;

[0032] Allicin: Jinan Lantian Gaokai Chemical Technology Co., Ltd.;

[0033] Acetyl tri-butyl citrate: Shandong Xinqi Chemical Co., Ltd.;

[0034] Glycerol: Guangzhou Ju Hui Chemical Co., Ltd.;

[0035] Butyl acetate: Guangzhou Guhui Chemical Co., Ltd.

[0036] Ethanol: Guangzhou Guhui Chemical Co., Ltd.

[0037] Example 1:

[0038] A waterproof liquid band-aid, comprising, in parts by weight:

[0039] Xylan butyric acid ester 8 parts, polyvinyl alcohol 400 5 parts, castor oil 2 parts, chitin / carbon nanoparticle microspheres 2 parts, catechin 1 part, allicin 0.3 parts, acetyl tri-butyl citrate 1.5 parts, glycerol 0.05 parts, butyl acetate 20 parts, ethanol 60 parts.

[0040] The preparation method of xylan butyric acid ester is as follows:

[0041] 100g of xylan is added to a three-necked flask equipped with stirring device and condenser, 4L of DMAc is added, after stirring and dispersion, the temperature is raised to reflux for 2h, and then cooled to 100℃, 175g of LiCl is added, and the mixture is stirred until the xylan is dissolved, then the temperature is restored to room temperature, 2.5L of butyric anhydride, 2.5L of pyridine and 300g of DMAP are added, and the mixture is stirred at 50℃ for 48h, after the reaction is completed, the reaction solution is slowly poured into 300L of ethanol to form a precipitate, which is separated by filtration, washed with ethanol and water for 3 times respectively, dissolved in CHCl3, and recrystallized with ethanol, and the obtained product is freeze-dried with liquid nitrogen.

[0042] The preparation method of chitin / carbon nanoparticle microspheres is as follows:

[0043] 60g of chitin powder is dispersed in a solvent composed of 110g of sodium hydroxide, 40g of urea and 850g of water, stirred at 1000rpm for 10min, and then subjected to 3 times of freeze-thawing to obtain a chitin solution, 10g of carbon nanoparticles is added to the chitin solution, and stirred at 0-5℃ for 30min to uniformly disperse, to obtain a chitin / carbon nanoparticle composite solution, 68g of Span 85 is added to 1000g of isooctane, stirred uniformly at 0-5℃, and then quickly injected into the chitin / carbon nanoparticle composite solution, and stirred to raise the temperature to 65℃ for 30min, and then the temperature is restored to room temperature, the pH of the system is adjusted to neutral with 0.1M hydrochloric acid, and after standing and layering, the isooctane is separated out, the water phase is poured into 1000mL of ethanol stirred at 30rpm for 2h, and the solid product is separated by filtration, the solid product is soaked in 500mL of tert-butyl alcohol for 24h, and then filtered again, and the obtained solid is washed with water and then freeze-dried with liquid nitrogen.

[0044] The preparation method of the above-mentioned waterproof liquid band-aid is as follows:

[0045] Butyl acetate and ethanol are mixed to obtain a mixed solvent, then xylan butyric acid ester, polyvinyl alcohol 400, castor oil, chitin / carbon nanoparticle microspheres, catechin, allicin, acetyl tri-butyl citrate, glycerol are added into the mixed solvent, and the mixture is stirred at 1000 rpm for 1 h and then sealed for storage.

[0046] Example 2:

[0047] A waterproof liquid band-aid, by weight fraction, comprises:

[0048] Xylan butyric acid ester 10 parts, polyvinyl alcohol 400 8 parts, castor oil 3 parts, chitin / carbon nanoparticle microspheres 3 parts, catechin 1 part, allicin 0.5 part, acetyl tri-butyl citrate 2 parts, glycerol 0.1 part, butyl acetate 20 parts, and ethanol 60 parts.

[0049] The preparation method of the chitin / carbon nanoparticle microspheres is the same as that in Example 1.

[0050] The preparation method of the waterproof liquid band-aid is as follows:

[0051] Butyl acetate and ethanol are mixed to obtain a mixed solvent, then xylan butyric acid ester, polyvinyl alcohol 400, castor oil, chitin / carbon nanoparticle microspheres, catechin, allicin, acetyl tri-butyl citrate, glycerol are added into the mixed solvent, and the mixture is stirred at 1000 rpm for 1 h and then sealed for storage.

[0052] Example 3:

[0053] A waterproof liquid band-aid, by weight fraction, comprises:

[0054] Xylan butyric acid ester 5 parts, polyvinyl alcohol 400 4 parts, castor oil 1 part, chitin / carbon nanoparticle microspheres 1 part, catechin 0.5 part, allicin 0.1 part, acetyl tri-butyl citrate 1 part, glycerol 0.05 part, butyl acetate 20 parts, and ethanol 60 parts.

[0055] The preparation method of the chitin / carbon nanoparticle microspheres is the same as that in Example 1.

[0056] The preparation method of the waterproof liquid band-aid is as follows:

[0057] Butyl acetate and ethanol are mixed to obtain a mixed solvent, then xylan butyric acid ester, polyvinyl alcohol 400, castor oil, chitin / carbon nanoparticle microspheres, catechin, allicin, acetyl tri-butyl citrate, glycerol are added into the mixed solvent, and the mixture is stirred at 1000 rpm for 1 h and then sealed for storage.

[0058] Example 4:

[0059] A waterproof liquid band-aid, by weight fraction, comprises:

[0060] Xylan butyrate 10 parts, polyvinyl alcohol 400 4 parts, castor oil 3 parts, chitin / carbon nanoparticle microspheres 1 part, catechin 1 part, allicin 0.1 part, acetyl tri-butyl citrate 2 parts, glycerol 0.05 parts, butyl acetate 20 parts, ethanol 60 parts.

[0061] The preparation method of the chitin / carbon nanoparticle microspheres is the same as that in Example 1.

[0062] The preparation method of the waterproof liquid band-aid is as follows:

[0063] The butyl acetate and the ethanol are mixed to obtain a mixed solvent, and then the xylan butyrate, the polyvinyl alcohol 400, the castor oil, the chitin / carbon nanoparticle microspheres, the catechin, the allicin, the acetyl tri-butyl citrate, and the glycerol are added into the mixed solvent, and stirred at 1000 rpm for 1 h, and then sealed and stored.

[0064] Example 5:

[0065] A waterproof liquid band-aid, in terms of weight parts, comprises:

[0066] Xylan butyrate 5 parts, polyvinyl alcohol 400 8 parts, castor oil 1 part, chitin / carbon nanoparticle microspheres 3 parts, catechin 0.5 parts, allicin 0.5 parts, acetyl tri-butyl citrate 1 part, glycerol 0.1 parts, butyl acetate 20 parts, ethanol 60 parts.

[0067] The preparation method of the chitin / carbon nanoparticle microspheres is the same as that in Example 1.

[0068] The preparation method of the waterproof liquid band-aid is as follows:

[0069] The butyl acetate and the ethanol are mixed to obtain a mixed solvent, and then the xylan butyrate, the polyvinyl alcohol 400, the castor oil, the chitin / carbon nanoparticle microspheres, the catechin, the allicin, the acetyl tri-butyl citrate, and the glycerol are added into the mixed solvent, and stirred at 1000 rpm for 1 h, and then sealed and stored.

[0070] Comparative Example 1:

[0071] The same as Example 1, except that the chitin / carbon nanoparticle microspheres are not added.

[0072] Comparative Example 2:

[0073] The same as Example 1, except that the catechin is not added.

[0074] Comparative Example 3:

[0075] The same as Example 1, except that the allicin is not added.

[0076] Performance test:

[0077] The waterproof liquid band-aid prepared in Examples 1 to 5 and Comparative Examples 1 to 3 of the present application were used as samples;

[0078] ①, ②, ③Before testing, the samples were poured into a flat-bottomed petri dish and placed in a fume hood, and after the solvent was completely volatilized, the obtained film was tested;

[0079] ①Waterproofness: The inverted cup method was used, a 12 mm diameter test tube was used, 10 mL of distilled water was added, the test tube opening was covered with a film, and a rubber band was used for fixation. The weight difference before and after 24 h was recorded, and the calculation method is shown in the following formula:

[0080] Loss Ratio = (M0-M 24h ) / M W

[0081] M0: Initial test tube weight;

[0082] M 24h : Test tube weight after 24 h;

[0083] M W : Water weight in the test tube;

[0084] ②Breathability: The moisture vapor transmission rate (MVTR) was used as the evaluation index, which is the mass of water vapor passing through a unit area of film per unit time. The test method was as follows: an appropriate amount of distilled water was added to a 10 mL test tube, the opening was covered with a film and sealed, the water surface was 5 mm ± 1 mm from the film, and the test tube was placed in a desiccator. The weight difference after 24 h was recorded, and the calculation method is shown in the following formula:

[0085] MVTR = (M0-M 24h ) / (s×t)

[0086] M0: Initial test tube weight;

[0087] M 24h : Test tube weight after 24 h;

[0088] s: Opening area;

[0089] t: 24 h

[0090] ③The tensile strength of the sample was measured using a tensile testing machine to evaluate its strength. Tensile strength is the ratio of the force that the film can withstand at the moment of tensile fracture to the area of the film. This parameter is a standard for evaluating the maximum tensile force that a wound dressing can withstand;

[0091] Tensile Strength = F / S

[0092] F: tensile force;

[0093] S: cross-sectional area of the sample;

[0094] (4) Bacteriostatic property: according to the provisions of 2.1.8 of the Anti-(bacteriostatic) test in the Technical Standard for Disinfection 2002 edition, the prepared liquid band-aid was tested for bacteriostatic performance. Different concentration gradients were formed by continuously dissolving the liquid band-aid in agar to show the bacteriostatic effect, and the bacteriostatic ability was judged by the size of the bacteriostatic ring diameter;

[0095] The results of tests 1, 2 and 3 are shown in Table 1, and the results of test 4 are shown in Table 2.

[0096] Table 1:

[0097]

[0098] From the above Table 1, it can be seen that the prepared liquid band-aid has excellent waterproof and breathable properties after film formation, and the tensile strength is ≥8.90 MPa, and the mechanical properties are excellent.

[0099] Table 2:

[0100]

[0101] From the above Table 2, it can be seen that the prepared liquid band-aid has excellent inhibitory effect on Staphylococcus aureus, Escherichia coli and Candida albicans, can kill bacteria and relieve inflammation, and can accelerate the healing of wounds.

[0102] The above examples are only used to illustrate the technical solutions of the present application, but not to limit it. Although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that they can still modify the technical solutions recorded in the foregoing embodiments, or make equivalent replacements to some technical features therein. Such modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present application.

Claims

1. A waterproof liquid adhesive bandage, characterized in that, By weight, it includes: 5-10 parts xylan esterified derivative, 4-8 parts polyvinyl alcohol, 1-3 parts castor oil, 1-3 parts chitin / carbon nanoparticle microspheres, 0.5-1 part polyphenols, 0.1-0.5 parts allicin, 1-2 parts tributyl acetylacetonate, 0.05-0.1 parts glycerol, and 70-90 parts solvent; The xylan esterified derivative is xylan butyrate.

2. The waterproof liquid bandage as described in claim 1, characterized in that, The preparation method of the chitin / carbon nanoparticle microspheres is as follows: Chitosan powder was dispersed in a solvent composed of sodium hydroxide, urea, and water. After multiple freeze-thaw cycles, a chitosan solution was obtained. Carbon nanoparticles were added to the chitosan solution and stirred at 0–5°C until homogeneous, resulting in a chitosan / carbon nanoparticle composite solution. Span 85 was added to isooctane and stirred at 0–5°C until homogeneous. Then, the chitosan / carbon nanoparticle composite solution was added, and the mixture was stirred and heated to 60–80°C and held for 20–50 minutes. After returning to room temperature, the pH of the system was adjusted to neutral with hydrochloric acid. After standing and separating the layers, the isooctane was separated. The aqueous phase was poured into ethanol and stirred and dispersed at low speed for 1–3 hours. The solid product was separated by filtration and soaked in tert-butanol for 24–48 hours. After filtration again, the product was washed with water and then freeze-dried.

3. The waterproof liquid bandage as described in claim 1, characterized in that, The polyphenolic substances are any one or more of catechin, epicatechin, gallocatechin, epigallocatechin, epicatechin gallate, and epigallocatechin gallate.

4. The waterproof liquid bandage as described in claim 1, characterized in that, The solvent includes butyl acetate and ethanol, wherein the weight ratio of butyl acetate to ethanol is 1-5:1-5.

5. A method for preparing a waterproof liquid bandage as described in any one of claims 1 to 4, characterized in that, The xylan esterified derivative, polyvinyl alcohol, castor oil, chitin / carbon nanoparticles, polyphenols, allicin, tributyl acetyl citrate, and glycerol are mixed evenly in a solvent and then sealed for storage.

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