Gel with antibacterial and anti-inflammatory effects and method for preparing the same

Abstract

This invention discloses a gel with antibacterial and anti-inflammatory effects and its preparation method, belonging to the field of decontamination gel technology. The gel, by weight, comprises the following components: 10-25 parts of *Hippophae rhamnoides* flavonoid extract, 10-30 parts of *Hippophae rhamnoides* polysaccharide extract, 1-3 parts of gel matrix, 5-10 parts of humectant, 5-10 parts of surfactant, and 0.2-1 parts of preservative. This invention separates flavonoids and polysaccharides from *Hippophae rhamnoides* using ultrasound-assisted extraction technology and combines them with a gel matrix to form a stable hydrogel system. By optimizing the extraction process of active ingredients from *Hippophae rhamnoides* and combining it with a gel delivery system, this invention achieves synergistic antibacterial and anti-inflammatory effects of flavonoids and polysaccharides. The product has stable performance and high safety, suitable for clinical and home decontamination scenarios.

Description

Technical Field

[0001] This invention relates to the field of decontamination gel technology, and in particular to a gel with antibacterial and anti-inflammatory effects and its preparation method. Background Technology

[0002] Disinfection products play an important role in medical care, public health, and daily life; however, existing products mostly rely on chemically synthesized ingredients (such as chlorhexidine and benzalkonium chloride), which can easily lead to drug resistance, skin irritation, and microbial imbalance with long-term use. In recent years, natural plant extracts have attracted attention due to their broad-spectrum antibacterial properties and safety, but they also have problems such as low extraction rates of active ingredients, poor stability, and unclear synergistic effects.

[0003] Golden hibiscus (Abelmoschus manihot) is a plant of the Malvaceae family, whose petals and stems are rich in flavonoids and polysaccharides. Current technologies mostly use flavonoids or polysaccharides alone, failing to fully utilize their combined use, and lack stable formulations suitable for disinfection applications. Furthermore, in traditional extraction processes, flavonoid yield is limited by insufficient solvent polarity matching, and polysaccharides are easily degraded, leading to loss of active ingredients. Therefore, developing an efficient extraction process and combining it with a gel carrier to prepare a disinfection product that combines rapid sterilization, long-lasting anti-inflammatory properties, and mild, non-irritating effects has significant application value. Summary of the Invention

[0004] The purpose of this invention is to provide a gel with antibacterial and anti-inflammatory effects and its preparation method, thereby solving the problems existing in the prior art. The gel prepared by this invention has highly effective antibacterial, anti-inflammatory, and mild, non-irritating properties, making it suitable for clinical and home disinfection scenarios.

[0005] To achieve the above objectives, the present invention provides the following solution:

[0006] Technical Solution 1: A gel with antibacterial and anti-inflammatory effects, comprising flavonoid extract and polysaccharide extract of *Hippophae rhamnoides*.

[0007] Further, by weight, it includes the following components: 10-25 parts of golden hibiscus flavonoid extract, 10-30 parts of golden hibiscus polysaccharide extract, 1-3 parts of gel matrix, 5-10 parts of humectant, 5-10 parts of surfactant and 0.2-1 parts of preservative.

[0008] Further, the gel matrix is ​​one or more of carbomer 934, carbomer 940, carbomer 980, sodium carboxymethyl cellulose, sodium alginate, gelatin, and aluminum distearate; the humectant is one or more of glycerin and propylene glycol; the surfactant is one or more of polysorbate 40, polysorbate 60, polysorbate 80, and sodium lauryl sulfate; and the preservative is one or more of sodium benzoate, potassium sorbate, and chlorobutanol.

[0009] Furthermore, the gel matrix is ​​carbomer 940, the humectant is glycerin, the surfactant is polysorbate 40, and the preservative is sodium benzoate.

[0010] Furthermore, the preparation method of the golden sunflower flavonoid extract includes: extracting the crushed golden sunflower petals with a 70% ethanol solution at 50-60℃ using ultrasound 2-3 times, 45 minutes each time; combining the extracts and concentrating under reduced pressure; freeze-drying to obtain a crude flavonoid extract; and purifying to obtain the golden sunflower flavonoid extract.

[0011] Furthermore, the preparation method of the golden sunflower polysaccharide extract includes: reflux extraction of pulverized golden sunflower stems and leaves with deionized water at 85-95℃ for 2-3 hours, centrifugation to collect the supernatant, elution of protein, precipitation of polysaccharides with anhydrous ethanol, and freeze-drying to obtain the golden sunflower polysaccharide extract.

[0012] Furthermore, the pH value of the gel is 5.8.

[0013] Technical Solution 2: A method for preparing the gel, comprising the following steps:

[0014] The gel matrix was dispersed in deionized water, swollen, and then a humectant was added and stirred until homogeneous to obtain a matrix solution. The flavonoid extract, polysaccharide extract, surfactant, and preservative of *Hippophae rhamnoides* were dissolved in deionized water and ultrasonically dispersed to obtain an active ingredient solution. The obtained active ingredient solution was added to the matrix solution, homogenized, and the pH was adjusted to obtain the gel.

[0015] Furthermore, the homogenization speed is 4000 rpm, and the homogenization time is 25 minutes.

[0016] Technical Solution 3: The application of the gel in the preparation of decontamination products.

[0017] The present invention discloses the following technical effects:

[0018] This invention provides an antibacterial and anti-inflammatory gel based on flavonoids and polysaccharides from *Hippophae rhamnoides*. The extraction process of the active ingredients was optimized using ultrasound-assisted extraction technology, significantly improving the yield and purity of flavonoids and polysaccharides. The gel formulation uses excipients such as carbomer 940, glycerin, polysorbate 40, and sodium benzoate, combined with homogenization (4000 rpm, 25 minutes) and pH adjustment to form a stable hydrogel system. After two months of high-temperature and light exposure testing at 55°C, the gel maintained its colloidal stability. Antibacterial experiments showed that the gel in Example 1 achieved antibacterial rates of 96.2% and 95.1% against *Escherichia coli* and *Staphylococcus aureus*, respectively, significantly superior to the control group with a single component or unoptimized process (e.g., Comparative Example 4 had an antibacterial rate of only 67.7%), verifying the synergistic effect of flavonoids and polysaccharides. This gel possesses highly effective antibacterial, anti-inflammatory, and mild, non-irritating properties, making it suitable for clinical and home disinfection scenarios. Given that both flavonoids and polysaccharides of *Hippophae rhamnoides* have anti-inflammatory effects, the gel material containing flavonoids and polysaccharides prepared by this invention can also be used in the research and development of anti-inflammatory products. Therefore, the gel prepared by this invention has important application value in the field of antibacterial and anti-inflammatory treatment. Detailed Implementation

[0019] Various exemplary embodiments of the present invention will now be described in detail. This detailed description should not be considered as a limitation of the present invention, but rather as a more detailed description of certain aspects, features, and embodiments of the present invention.

[0020] It should be understood that the terminology used in this invention is merely for describing particular embodiments and is not intended to limit the invention. Furthermore, with respect to numerical ranges in this invention, it should be understood that each intermediate value between the upper and lower limits of the range is also specifically disclosed. Any stated value or intermediate value within a stated range, as well as each smaller range between any other stated value or intermediate value within said range, is also included in this invention. The upper and lower limits of these smaller ranges may be independently included or excluded from the range.

[0021] Unless otherwise stated, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. While only preferred methods and materials have been described herein, any methods and materials similar or equivalent to those described herein may be used in the implementation or testing of this invention. All references to this specification are incorporated by way of citation to disclose and describe methods and / or materials associated with those references. In the event of any conflict with any incorporated reference, the content of this specification shall prevail.

[0022] Various modifications and variations can be made to the specific embodiments described in this specification without departing from the scope or spirit of the invention, as will be apparent to those skilled in the art. Other embodiments derived from this specification will also be apparent to those skilled in the art. This specification and embodiments are merely exemplary.

[0023] The terms “include,” “including,” “have,” “contain,” etc., used in this article are all open-ended terms, meaning that they include but are not limited to.

[0024] Example 1

[0025] 1. Preparation of Flavonoid Extract from Hibiscus mutabilis

[0026] (1) Take 1 kg of dried golden sunflower petals, crush them to 60 mesh, and add 15 L of 70% ethanol solution.

[0027] (2) Extract twice at 55℃ (power 300W, frequency 40kHz), 45 minutes each time;

[0028] (3) Combine the extracts, concentrate under reduced pressure to obtain an extract, and freeze-dry to obtain crude flavonoids;

[0029] (4) The crude flavonoids were dissolved in deionized water and subjected to AB-8 macroporous resin column chromatography. The eluent was eluted with 60% ethanol by volume. The eluent was collected, concentrated, and freeze-dried to obtain the flavonoid extract.

[0030] 2. Preparation of Golden Sunflower Polysaccharide Extract

[0031] (1) Take 2 kg of golden sunflower stems and leaves, crush them and add 40 L of deionized water;

[0032] (2) Reflux extraction at 90℃ for 2.5 hours, followed by centrifugation to remove residue;

[0033] (3) The supernatant was deproteinized three times using the Sevage method (chloroform: n-butanol = 4:1);

[0034] (4) Add 3 times the volume of anhydrous ethanol to precipitate the polysaccharide, centrifuge to collect the precipitate, and freeze-dry to extract the polysaccharide.

[0035] 3. Preparation of decontamination gel

[0036] (1) Weigh 9403g of carbomer, disperse it in 30mL of deionized water, and let it stand to swell for 12 hours;

[0037] (2) Add 10g of glycerin and stir to obtain a transparent matrix;

[0038] (3) Take 15g of the flavonoid extract of *Hippophae rhamnoides* prepared in step 1 above, 25g of the polysaccharide extract of *Hippophae rhamnoides* prepared in step 2 above, 406g of polysorbate, and 0.4g of sodium benzoate, dissolve them in 40.6mL of deionized water, and disperse them by ultrasonication to obtain a solution;

[0039] (4) Slowly add the solution from step (3) into the transparent matrix from step (2) and homogenize at 4000 rpm for 25 minutes;

[0040] (5) Add triethanolamine to adjust the pH to 5.8, fill and sterilize to obtain the finished gel, and set aside for later use.

[0041] Example 2

[0042] The difference from Example 1 is that the preparation of the decontamination gel in step 3 is as follows: 1.5g of carbomer 940, 10g of glycerin, 3g of flavonoid extract of *Hippophae rhamnoides*, 10g of polysaccharide extract of *Hippophae rhamnoides*, 3g of polysorbate 80, and 0.3g of sodium benzoate. The remaining steps are the same as in Example 1.

[0043] Comparative Example 1

[0044] The difference from Example 1 is that the preparation of the golden hibiscus flavonoid extract in this comparative example is as follows:

[0045] (1) Take 1 kg of dried golden sunflower petals, crush them to 60 mesh, and add 15 L of 70% ethanol solution.

[0046] (2) Extract once with ultrasound (300W power, 40kHz frequency) at 65℃ for 45 minutes;

[0047] (3) The extract was concentrated under reduced pressure to a paste, and then freeze-dried to obtain crude flavonoids;

[0048] (4) The crude flavonoids were dissolved in deionized water and subjected to AB-8 macroporous resin column chromatography. The eluent was eluted with 60% ethanol by volume. The eluent was collected, concentrated, and freeze-dried to obtain the flavonoid extract.

[0049] The remaining steps are the same as in Example 1.

[0050] Comparative Example 2

[0051] The difference from Example 1 is that the preparation of the golden sunflower polysaccharide extract in this comparative example is as follows:

[0052] (1) Take 2 kg of golden sunflower stems and leaves, crush them and add 40 L of deionized water;

[0053] (2) Reflux extraction at 100℃ for 3.5 hours, followed by centrifugation to remove residue;

[0054] (3) The supernatant was deproteinized three times using the Sevage method (chloroform: n-butanol = 4:1);

[0055] (4) Add 3 times the volume of anhydrous ethanol to precipitate the polysaccharide, centrifuge to collect the precipitate, and freeze-dry to obtain polysaccharide extract (purity 88.3%).

[0056] The remaining steps are the same as in Example 1.

[0057] Comparative Example 3

[0058] The difference from Example 1 is that the preparation of the decontamination gel in this comparative example is as follows:

[0059] (1) Weigh 9404g of carbomer, disperse it in 30mL of deionized water, and let it stand to swell for 12 hours;

[0060] (2) Add 13g of glycerin and stir to obtain a transparent matrix;

[0061] (3) Take 35g of the flavonoid extract of *Hippophae rhamnoides* prepared in step 1 above, 9g of the polysaccharide extract of *Hippophae rhamnoides* prepared in step 2 above, 404g of polysorbate, and 1.4g of sodium benzoate, dissolve them in 33.6mL of deionized water, and disperse them by ultrasonication to obtain a solution;

[0062] (4) Slowly add the solution from step (3) into the transparent matrix from step (2) and homogenize at 4000 rpm for 25 minutes;

[0063] (5) Add triethanolamine to adjust the pH to 5.8, fill and sterilize to obtain the finished gel, and set aside for later use.

[0064] The remaining steps are the same as in Example 1.

[0065] Comparative Example 4

[0066] The difference from Example 1 is that in the preparation of the comparative example decontamination gel, 40g of *Hippophae rhamnoides* flavonoid extract was used, and no *Hippophae rhamnoides* polysaccharide extract was added. The remaining steps are the same as in Example 1.

[0067] Comparative Example 5

[0068] The difference from Example 1 is that in the preparation of the comparative example decontamination gel, 40g of *Hippophae rhamnoides* polysaccharide extract was used, and no *Hippophae rhamnoides* flavonoid extract was added. The remaining steps are the same as in Example 1.

[0069] Test Example 1

[0070] The gel products prepared in Examples 1, 2 and Comparative Examples 1-5 were stored at 55°C for 2 months and exposed to light for 2 months. The colloids of all the gel products remained stable and did not change color, indicating that the gels prepared by the method of the present invention have stable properties.

[0071] Test Example 2

[0072] The purity of the flavonoid extracts and polysaccharide extracts in Example 1, Comparative Example 1, and Comparative Example 2 was determined by high performance liquid chromatography (HPLC). The determination process is as follows:

[0073] Chromatographic conditions: The column was a ZORBAX Eclipse XDB-C18 (Agilent; 150 mm long × 4.6 mm inner diameter; 5 μm packed particle diameter); the mobile phase was acetonitrile-water (acetonitrile to water volume ratio of 77:23); the flow rate was 0.6 mL / min; the injection volume was 10 μL; the column temperature was 20 °C; and the detection wavelength was 254 nm.

[0074] Standard curve: Dissolve 5 mg of flavonoid extract or polysaccharide extract standard in 5 mL of methanol to prepare standard solutions with final concentrations of 500, 250, 125, 62.5, 31.25, and 0 μg / mL. Inject the solutions sequentially from low to high concentration, with an injection volume of 10 μL, and repeat each concentration three times. Analyze according to the above chromatographic conditions. Plot the mass concentration of flavonoid extract or polysaccharide extract as the ordinate (Y) and the peak area of ​​flavonoid extract or polysaccharide extract as the abscissa (X), and perform linear regression to obtain the regression equation. Based on the above chromatographic conditions and standard curve, determine the purity of the purified flavonoid extract or polysaccharide extract in Example 1, Comparative Example 1, and Comparative Example 2, and record the results in Table 1.

[0075] Table 1

[0076] Example 1 Comparative Example 1 Comparative Example 2 purity of flavonoid extract 81.5％ 66.4％ 81.5％ Polysaccharide extract purity 82.6％ 82.6％ 73.5％

[0077] As shown in Table 1, the extraction method of the present invention can obtain high-purity golden sunflower flavonoids and golden sunflower polysaccharides.

[0078] Test Example 3

[0079] The antibacterial properties of the gels prepared in Examples 1, 2, and 1-5 were tested, and the testing process is as follows:

[0080] Take 0.1 g of the gels prepared in Example 1, Example 2, and Comparative Examples 1-5 respectively, and mix them with 10 mL of 1×10 7 A mixture of CFU / mL *E. coli* and *Staphylococcus aureus* bacterial suspensions was placed in a test tube and incubated on a shaker at 37°C and 120 rpm for 4 hours. This was the experimental group, and the suspension without the antimicrobial gel was the control group. The bacterial suspensions from both the experimental and control groups were then diluted to 1×10⁻⁶. 5 CFU / mL, 100 μL of bacterial suspension was spread onto the surface of an agar plate and incubated in a shaking incubator at 37°C for 24 h. The antibacterial rate was calculated by plate count method. The formula for calculating the antibacterial rate is as follows: Antibacterial rate

[0081] = [(Na-Nb) / Na]×100%, where Na is the colony count in the blank group and Nb is the colony count in the experimental group. The calculation results are recorded in Table 2.

[0082] Table 2

[0083]

[0084] As shown in Table 2, the gel material prepared by adding the golden sunflower flavonoids and golden sunflower polysaccharides extracted in this invention has excellent antibacterial properties.

[0085] The embodiments described above are merely preferred embodiments of the present invention and are not intended to limit the scope of the present invention. Various modifications and improvements made by those skilled in the art to the technical solutions of the present invention without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.

Claims

1. A gel having an antibacterial and anti-inflammatory effect, characterized by comprising, The components include a malveira flavone extract and a malveira polysaccharide extract. The components include, by weight, 10-25 parts of a malveira flavone extract, 10-30 parts of a malveira polysaccharide extract, 1-3 parts of a gel base, 5-10 parts of a humectant, 5-10 parts of a surfactant, and 0.2-1 part of a preservative. The preparation method of the malveira flavone extract includes: ultrasonic extraction of the pulverized malveira petals with an ethanol solution with a volume concentration of 70% at 50-60°C for 2-3 times, each time for 45 minutes, combined extraction liquid, vacuum concentration, freeze-drying to obtain a flavone crude extract, and purification to obtain the malveira flavone extract. The preparation method of the malveira polysaccharide extract includes: reflux extraction of the pulverized malveira stems and leaves with deionized water at 85-95°C for 2-3 hours, centrifugation to obtain the supernatant, polysaccharide precipitation with anhydrous ethanol after protein elution, and freeze-drying to obtain the malveira polysaccharide extract.

2. The gel of claim 1, wherein, The gel base is one or more of carbomer 934, carbomer 940, carbomer 980, sodium carboxymethyl cellulose, sodium alginate, gelatin, and aluminum distearate; the humectant is one or more of glycerol and propylene glycol; the surfactant is one or more of polysorbate 40, polysorbate 60, polysorbate 80, and sodium dodecyl sulfate; and the preservative is one or more of sodium benzoate, potassium sorbate, and chlorobutanol.

3. The gel of claim 2, wherein, The gel base is carbomer 940, the humectant is glycerol, the surfactant is polysorbate 40, and the preservative is sodium benzoate.

4. The gel of claim 1, wherein, The pH value of the gel is 5.

8.

5. A process for the preparation of a gel according to any one of claims 1 to 4, characterised in that, The steps include: The gel base is dispersed in deionized water, and after swelling, the humectant is added and stirred uniformly to obtain a base solution; the malveira flavone extract, the malveira polysaccharide extract, the surfactant, and the preservative are dissolved in deionized water, and ultrasonic dispersion is performed to obtain an active ingredient solution; the obtained active ingredient solution is added to the base solution, and after homogenization, the pH value is adjusted to obtain the gel.

6. The production method according to claim 5, wherein The homogenization speed is 4000 rpm, and the homogenization time is 25 minutes.

7. Use of the gel of any one of claims 1-4 in the preparation of a decontamination product.

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