CN120815216B

CN120815216B - Hydrogel dressing with antibacterial repairing function and preparation method thereof

Info

Publication number: CN120815216B
Application number: CN202511315777.1A
Authority: CN
Inventors: 权宁子; 周涛; 周雷; 周子潇
Original assignee: Feilang Biotechnology Hubei Co ltd
Current assignee: Feilang Biotechnology Hubei Co ltd
Priority date: 2025-09-16
Filing date: 2025-09-16
Publication date: 2025-12-09
Anticipated expiration: 2045-09-16
Also published as: CN120815216A

Abstract

A hydrogel dressing with antibacterial and repairing effects comprises, by weight, 18-22 parts of honeysuckle hydrosol, 6-8 parts of Phellinus linteus polysaccharide extract, 1-3 parts of gelatin, 2-4 parts of humectant and 1-3 parts of nutritional agent. According to the invention, the polysaccharide in the Phellinus linteus powder is extracted by adopting an ultrasonic synergistic cellulase method, cellulose in plants can be effectively degraded by utilizing cellulase, and then plant cell walls are effectively broken down, so that plant cell polysaccharide is effectively dissolved out, the extraction amount of Phellinus linteus polysaccharide is improved, the process is simple, the cost is low, the condition is mild, the environment is not polluted, and the environment-friendly industrial production is facilitated. The Phellinus linteus polysaccharide prepared by the invention has strong antibacterial capability and good antioxidant capability, and is easier to deeply nourish skin. The natural weak acid honeysuckle pure dew with strong anti-inflammatory and antibacterial capabilities is adopted to replace deionized water to prepare cosmetics, so that the cosmetics are more attached to skin due to weak acidity, and the special plant fragrance emitted by the cosmetics can be pleasant.

Description

Hydrogel dressing with antibacterial repairing function and preparation method thereof

Technical Field

The invention relates to the technical field of skin care products, in particular to a hydrogel dressing with antibacterial repairing function and a preparation method thereof.

Background

Phellinus linteus is used as a traditional rare Chinese herbal medicine in China, wherein the folk is adress sb. respectfully of forest gold, and a plurality of Chinese medicinal books are recorded with medicinal values, for example, phellinus linteus Li Wuzang and Xuan Chang are mentioned in the compendium of materia medica, and stomach qi and toxin expelling gas are recorded. It belongs to a cold drug, and has bitter and astringent taste. The research shows that the main active ingredients of Phellinus linteus include polysaccharide, flavone, ergosterol, triterpenes, etc. (Zhao Peng, li Caixia, levojiao, et al Sang Huanghua), pharmacological activity research progress and quality Marker (Q-Marker) prediction [ J ]. Drug evaluation research), wherein Phellinus linteus polysaccharide is used as core active ingredient, and has effects of resisting tumor, oxidation, sugar, enhancing immunity, resisting mutation, scavenging free radical, etc.

The Phellinus linteus polysaccharide is extracted by various methods, such as water extraction, enzymolysis, and ultrasonic assisted extraction. However, as a biological macromolecule, the extraction difficulty is high, and the biological macromolecule is easy to inactivate under high temperature conditions, which greatly limits the extraction efficiency. Therefore, optimizing the extraction and purification process of Phellinus linteus polysaccharide by innovative means is of great importance. The polysaccharide in the Phellinus linteus powder is extracted by adopting an ultrasonic synergistic cellulase method in the experiment, simultaneously the release of active ingredients is promoted by combining the ultrasonic, the experiment cost is effectively reduced, the extraction efficiency is improved, no harmful chemical reagent is added in the whole process, the environment is protected, no pollution is caused, the traditional complex process is simplified, and the industrialization production is expected to be realized.

The plant hydrolat is a byproduct obtained in the process of extracting essential oil by distillation of aromatic plants, has special plant aroma, contains trace amounts of esters, ketones, olefins and alcohols, has hydrophilicity, and most of the hydrolat is weak acid, so that the plant hydrolat has the effects of relieving and diminishing inflammation on skin as cosmetics. Researches show that the honeysuckle flower hydrosol is rich in chlorogenic acid and the like, and has better anti-inflammatory and antibacterial capabilities than the essential oil (Wang Jialu, zhang Caifeng, xu Runyang, and the like).

Hydrogels are receiving attention because of their excellent biocompatibility and biomimetic structure. When used as a wound dressing, it is effective in absorbing secretions, preventing infection and maintaining a moist environment, thereby promoting cell adhesion. Gelatin is widely used for preparing hydrogel wound dressing by virtue of its strong moisture retention, plasticity, promotion of wound healing and the like. Although the efficacy of Phellinus linteus polysaccharides in the field of medical care has been widely accepted, their use in cosmeceuticals and medical repair cosmetics with antibacterial, antioxidant and repair effects is still under investigation. In particular, phellinus linteus polysaccharides are used to develop natural hydrogel dressings with these effects, and there is still a technical gap.

Disclosure of Invention

The invention provides a method for preparing hydrogel dressing with antibacterial and repairing functions by taking Phellinus linteus polysaccharide with excellent antibacterial and antioxidant effects as an effective component.

The invention belongs to the field of plant extraction and cosmetics, and adopts Phellinus linteus polysaccharide and honeysuckle flower hydrolat as main raw materials to prepare a skin care product with the functions of antioxidation, mildness and moisture preservation, and the skin care product has the advantages of simple process, environment friendliness and filling in the blank of Phellinus linteus polysaccharide in the field of cosmetics.

The hydrogel dressing with the antibacterial repairing function comprises the following components in parts by weight:

18-22 parts of honeysuckle flower hydrosol

6-8 Parts of Phellinus linteus polysaccharide extract

1-3 Parts of gelatin

2-4 Parts of humectant

1-3 Parts of nutritional agent.

Preferably, the Phellinus linteus polysaccharide extract is extracted from Phellinus linteus powder by ultrasonic synergistic cellulase method, and the extraction rate is 2% -5%.

Preferably, the preparation method of the Phellinus linteus polysaccharide extract comprises the following steps:

Degreasing, namely mixing Phellinus linteus powder with 90% ethanol according to a feed liquid ratio of 1:20-1:30, and refluxing for 2-3 hours at 80-85 ℃;

Adding water into defatted Phellinus linteus powder according to a solid-to-liquid ratio of 1:20-1:30, adding 0.5-1.0 g of biological enzyme, performing enzymolysis at 40-55 ℃ for 90 min, performing enzyme deactivation at 80-100 ℃ for 5-10 min, and performing ultrasonic treatment for 0.5-2 h at 300-360 w;

purifying, namely mixing and precipitating the enzymolysis liquid and 79% ethanol for 10-12 hours according to the volume ratio of 1:5, and centrifuging and drying to obtain the Phellinus linteus polysaccharide extract.

Preferably, in the enzymolysis ultrasonic step, the defatted Phellinus linteus powder is added with water to prepare an aqueous solution with a solid-to-liquid ratio of 1:20-1:30, and the biological enzyme adopted in the enzymolysis is at least one of cellulase, papain, pectase and amylase.

Preferably, the humectant is at least one selected from sodium hyaluronate, glycerin, and sodium polyglutamate.

Preferably, the nutritional agent is selected from at least one of vitamin C, panthenol, nicotinamide.

Preferably, the preparation method of the honeysuckle hydrosol comprises the steps of adding water into branches and leaves of the honeysuckle according to a feed liquid ratio of 1:2, distilling at 120 ℃ to obtain 3 h, and collecting condensate at the lower layer to obtain the honeysuckle hydrosol.

The preparation method of the hydrogel dressing with the antibacterial repairing function comprises the following steps:

s1, weighing gelatin powder, placing the gelatin powder into a container, adding honeysuckle flower hydrolat into the container, and continuously stirring to completely dissolve the gelatin to obtain a gelatin water solution;

S2, adding the Phellinus linteus polysaccharide solution, the humectant and the nutritional agent into the gel water solution, continuously stirring uniformly, and cooling to room temperature to form the required hydrogel dressing.

Preferably, the mass concentration of gelatin in the gel water solution is 10% -20%, and the stirring temperature is 40-50 ℃.

The invention has the advantages that:

According to the invention, the polysaccharide in the Phellinus linteus powder is extracted by adopting an ultrasonic synergistic cellulase method, cellulose in plants can be effectively degraded by utilizing cellulase, and then the plant cell wall is effectively broken down, so that the polysaccharide in plant cells is effectively dissolved out, the extraction quantity of Phellinus linteus polysaccharide is improved, the process is simple, the cost is low, the condition is mild, the environment is not polluted, and the environment-friendly industrial production is facilitated. The Phellinus linteus polysaccharide prepared by the invention has strong antibacterial capability and good antioxidant capability, and is easier to deeply nourish skin. The natural weak acid honeysuckle pure dew with strong anti-inflammatory and antibacterial capabilities is adopted to replace deionized water to prepare cosmetics, so that the cosmetics are more attached to skin due to weak acidity, and the special plant fragrance emitted by the cosmetics can be pleasant. Therefore, the Phellinus linteus polysaccharide and the honeysuckle flower hydrolat are combined to prepare the hydrogel dressing with antibacterial and repairing effects, which is mild and not irritating, can effectively inhibit the activity of active free radicals, and is suitable for urgent relief of skin damage, long-term anti-aging and anti-oxidation.

Drawings

FIG. 1 is an infrared spectrum of Phellinus linteus polysaccharide extract.

Fig. 2 is a schematic representation of the swelling ratio of a hydrogel dressing.

Detailed Description

For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments.

Example 1]

(1) Preparation of Phellinus linteus polysaccharide:

Taking 5.0 g Phellinus linteus powder in a 250 mL round bottom flask, adding a 90% ethanol solution 125 mL, placing in an 80 ℃ oil bath pot for refluxing for two hours, dissolving lipid in Phellinus linteus powder in the process, dissolving in ethanol, filtering the solution in the flask for two hours, adding a 90% ethanol solution 125 mL, and repeating the above operations to dissolve all lipid in Phellinus linteus powder. Filtering to obtain defatted Phellinus linteus powder, drying in a vacuum drying oven at 60deg.C to constant weight, and storing defatted Morus alba Huang Fenfeng in self-sealing bag.

Adding 3.0 g defatted Phellinus linteus powder into 80mL deionized water, adding 0.5 g cellulase, extracting at 45deg.C to obtain 90 min. Then the temperature is raised to 80 ℃, and the enzyme is inactivated 5min. After 1: 1h was sonicated at 80℃and 360 w ℃power, the pH of the system was adjusted to 4 after the temperature had dropped to 50 ℃. And centrifuging the solution, wherein the polysaccharide to be extracted is dissolved in water, so that the supernatant is reserved, and simultaneously, in order to remove residues completely, the centrifuged supernatant is subjected to suction filtration, so that the filtrate is reserved. And concentrating the filtrate by rotating to about 20 mL to obtain high-concentration extract. Since the polysaccharide is insoluble in ethanol, 79% ethanol can be added into the extractive solution to precipitate polysaccharide in the extractive solution, and the volume ratio of Phellinus Linteus concentrated solution to ethanol is 1:5. Standing 12h to precipitate completely, centrifuging the solution after alcohol precipitation, collecting precipitate, and lyophilizing to obtain Phellinus linteus polysaccharide extract, wherein the infrared spectrum is shown in figure 1, and other extraction methods are shown in table 1 below.

TABLE 1

(2) Preparation of honeysuckle flower hydrolat:

Fresh 3 kg honeysuckle branches and leaves are cut into sections, the sections are placed into a distillation flask, 6 kg deionized water is added according to a feed-liquid ratio of 1:2, the distillation temperature is set to be 120 ℃, a condensing device is started when water starts to generate steam after boiling, the heating temperature is set to be 100 ℃, the distilled aromatic is cooled and kept stand in a collecting device after 3 h, and the liquid at the lower layer is collected to be the honeysuckle pure dew.

(3) Preparing a finished product:

the following substances were added according to mass specific gravity. Adding 2 parts of gelatin with the concentration of 10% into 20 parts of honeysuckle flower hydrolat prepared in the step (2), and preparing gelatin water solution at 50 ℃ as phase A for standby. And (3) adding 7 parts of Phellinus linteus polysaccharide prepared in the step (1) into the phase A, then adding 3 parts of humectant acetylated sodium hyaluronate and 2 parts of nutrient vitamin C, and stirring uniformly. Until the product is cooled to room temperature, and is solidified into a finished product sample.

< Test experiment >

(1) Antibacterial property experiment

160 Μl of the hydrogel pre-polymer was tiled into a 48-well plate and blue-light irradiated at 30 min to form a hydrogel scaffold. Then preparing staphylococcus aureus suspension with the concentration of 10 ⁵ CFU/L. 70 mu L of the bacterial suspension is coated on an M-H plate, then the hydrogel bracket is paved on the M-H plate, 1d is cultivated in a constant temperature 37 ℃ environment, and the inhibition zone on the plate is observed and measured. As shown in the table, the test samples showed a good inhibitory effect against Staphylococcus aureus, as shown in Table 2.

TABLE 2

(2) Hydrogel Performance test (swelling ratio experiment)

The sample was immersed in a phosphate buffer solution and placed under a constant temperature of 37 ℃ for 2 d. And taking out, sucking out redundant phosphate buffer solution on the surface of the material, weighing and recording, and recording as V ₁. Thereafter, the sample was dried again, and the record was weighed and recorded as V ₂. The hydrogel swelling ratio was then calculated as:

The experimental results are shown in fig. 2, and the results show that the sample hydrogel swells well.

(3) Wound healing condition

The wound healing condition is evaluated according to the wound healing treatment and time in the facial skin defect repair treatment operation of a patient, and is particularly classified into 3 grades of excellent grade, good grade and poor grade. And the excellent rate of wound healing is calculated according to the method. And (3) according to the wound scar hyperplasia condition, carrying out VSS evaluation on the wound scar hyperplasia condition of each group of patients after operation for a certain time according to the Vancouver scar scale. The evaluation adopts a Linker six-level score, namely 0-5 score. The higher the VSS score, the more severe the wound scar hyperplasia that represents a period of time after surgery in the patient. Patient satisfaction condition, the satisfaction visit of the patient 6 months after the operation of the facial skin defect repair treatment is carried out by adopting a questionnaire mode. The total score of the evaluation was set to 10 points, wherein less than 6 points were unsatisfactory, 6 to 7 points indicated satisfactory, and 8 to 10 points indicated very satisfactory. Thereby calculating patient satisfaction. Each data in this study was processed using SPSS 25.0 software, where "P <0.05" indicates that there was a statistical significance of the differences in each set of data. 92 patients were selected for facial skin defect repair treatment. The patients were randomly grouped, and the number of cases of facial skin defect repair treatment patients in the control group and the test group was 46. The patient inclusion criteria were (1) aware of and willing to agree to participate in the study, (2) patient age 18-60 years, (3) facial surgery treatment was accepted within 6 hours of facial injury, and (4) patient was facial skin defect. The exclusion criteria of the patients are (1) once receiving similar surgical treatment, (2) the patients have mental diseases or infectious diseases, and (3) the patients have serious abnormal heart, liver and kidney functions. In the facial skin defect repair treatment, each patient in the control group is treated by a common skin flap prosthesis, and each patient in the test group is treated by a hydrogel dressing. The dressing change date, dressing fixation mode and the like of each group of patients are not different.

The experimental results are shown in the following table 3, and the wound healing condition of the sample hydrogel is good.

TABLE 3 Table 3

(4) Skin irritation conditions

The test was performed using a 0.5 mL hydrogel solution according to the multiple complete skin irritation test method in the disinfection technical Specification (2002 edition). Prior to the test 24 h, the hairing on both sides of the back spine of guinea pigs was removed and the skin was not damaged. The dehairing range was about 3 cm x3 cm each on the left and right. In the test, the hydrogel solution 0.5 mL is directly dripped on 2-4 layers of gauze with the area of 2.5 cm multiplied by 2.5 cm and is applied to the left skin removing surface, and then is covered by a layer of non-irritating plastic film and then is fixed by a non-irritating adhesive tape. The right side was coated with 0.5 mL of 0.9% sodium chloride injection as a control, and after the coating, 4 h was washed with warm water to remove the residue. The hydrogel is applied once a day, 14 d is continuously applied, 4 h is applied each time, the residual test substance is cleaned by water or a proper solvent without stimulation, the red spots and edema of animal skin are observed by applying the test substance 24 h, and the hydrogel is scored according to the scoring standard of skin stimulation reaction, so that the hydrogel has no stimulation to the multiple complete skin stimulation intensity of guinea pigs and meets the requirements of the disinfection technical Specification (2002 edition).

The experimental results are shown in table 4 below, with almost no irritation of the samples.

TABLE 4 Table 4

The above embodiments are only for illustrating the technical solution and features of the present invention, and are intended to be better implemented by those skilled in the art, but not to limit the scope of the present invention, and all equivalent changes or modifications made according to the spirit of the present invention are within the scope of the present invention, wherein the prior art is not specifically illustrated.

Claims

1. A hydrogel dressing with antibacterial and repairing effects, characterized in that it comprises the following components in parts by weight:

Honeysuckle hydrosol 18-22 parts

Phellinus linteus polysaccharide extract 6-8 parts

1-3 parts gelatin

Moisturizer 2-4 parts

Nutrient supplement 1-3 servings;

The method for preparing the hydrogel dressing includes the following steps:

S1. Weigh out gelatin powder and place it in a container, then add honeysuckle hydrosol and stir continuously until the gelatin is completely dissolved to obtain a gel aqueous solution.

S2. Add the Phellinus linteus polysaccharide solution, moisturizer, and nutrient to the gel aqueous solution and continue stirring until homogeneous. Cool to room temperature to form the desired hydrogel dressing.

The gelatin concentration in the aqueous gel solution is 10%~20%, and the stirring temperature is 40~50℃.

2. The hydrogel dressing with antibacterial and repairing effects according to claim 1, characterized in that the polysaccharide extract of Phellinus linteus is extracted from Phellinus linteus powder by ultrasonic synergistic cellulase method, with an extraction rate of 2%~5%.

3. The hydrogel dressing with antibacterial and repairing effects according to claim 2, characterized in that the preparation method of the Phellinus linteus polysaccharide extract includes the following steps:

Degreasing treatment: Mix Phellinus linteus powder with 90% ethanol at a material-to-liquid ratio of 1:20 to 1:30 and reflux at 80 to 85°C for 2 to 3 hours;

Enzymatic hydrolysis and sonication: Defatted Phellinus linteus powder is mixed with water at a solid-liquid ratio of 1:20~1:30, 0.5~1.0 g of biological enzyme is added, and the mixture is enzymatically hydrolyzed at 40~55℃ for 90 min, then the enzyme is inactivated at 80~100℃ for 5~10 min, and then sonicated at 300~360 w for 0.5~2 h.

Purification: The enzymatic hydrolysate was mixed with 79% ethanol at a volume ratio of 1:5 and precipitated for 10-12 h. After centrifugation and drying, the polysaccharide extract of Phellinus linteus was obtained.

4. A hydrogel dressing with antibacterial and repairing effects according to claim 3, characterized in that, in the enzymatic hydrolysis and ultrasonication step, defatted Phellinus linteus powder is mixed with water to prepare an aqueous solution with a solid-liquid ratio of 1:20 to 1:30, and the biological enzyme used for enzymatic hydrolysis is at least one of cellulase, papain, pectinase, and amylase.

5. A hydrogel dressing with antibacterial and repairing effects according to claim 1, characterized in that the moisturizer is selected from at least one of acetylated sodium hyaluronate, glycerin, and sodium polyglutamate.

6. The hydrogel dressing with antibacterial and repairing effects according to claim 1, characterized in that the nutrient agent is selected from at least one of vitamin C, panthenol, and nicotinamide.

7. The hydrogel dressing with antibacterial and repairing effects according to claim 1, characterized in that the honeysuckle hydrosol is prepared by adding water to honeysuckle branches and leaves at a ratio of 1:2, distilling at 120°C for 3 hours, and collecting the lower condensate to obtain the honeysuckle hydrosol.