A toothpaste for whitening teeth and inhibiting helicobacter pylori in oral cavity and a preparation method thereof

Abstract

This invention discloses a whitening toothpaste that inhibits oral Helicobacter pylori and its preparation method, belonging to the technical field of oral care products. Specifically, it relates to a whitening toothpaste that inhibits oral Helicobacter pylori, comprising the following components by weight: 2-4 parts of a microbial active ingredient complex, 5-10 parts of clove, 0.2-0.4 parts of comfrey oil, 0.04-0.06 parts of bisabolol, 30-50 parts of an abrasive, 0.4-0.6 parts of a thickener, 25-35 parts of a humectant, 4-6 parts of soapberry saponins, 0.05-0.15 parts of a sweetener, 0.2-0.4 parts of a preservative, and 10-15 parts of water. This invention utilizes the synergistic effect of the microbial active ingredient complex and the combination of clove, comfrey oil, and bisabolol to achieve the effect of inhibiting oral Helicobacter pylori. Combined with a specific amount of abrasive, it can simultaneously achieve a whitening effect.

Description

Technical Field

[0001] This invention belongs to the field of oral care products technology, and in particular relates to a whitening toothpaste that inhibits Helicobacter pylori in the oral cavity and its preparation method. Background Technology

[0002] Helicobacter pylori ( Helicobacter pylori Helicobacter pylori (H. pylori) is a Gram-negative bacterium that colonizes the human gastric mucosa and is a significant pathogenic factor in diseases such as chronic gastritis, peptic ulcers, and gastric cancer. In recent years, numerous studies have confirmed that the oral cavity, especially dental plaque, saliva, and the back of the tongue, is another important reservoir and potential source of infection for H. pylori besides the stomach. H. pylori in the oral cavity may not only be associated with local oral diseases such as periodontitis and halitosis, but its presence can also lead to recurrent gastric infections, severely affecting the efficacy of eradication therapy. Therefore, controlling oral H. pylori is of great significance for blocking its transmission routes, assisting in gastric eradication therapy, and maintaining oral health.

[0003] Currently, the main clinical treatment for Helicobacter pylori involves triple or quadruple therapy combining oral antibiotics with proton pump inhibitors. However, this therapy has certain limitations: firstly, systemic administration results in limited drug concentrations in the oral cavity, making it difficult to effectively eradicate hidden Helicobacter pylori in the mouth; secondly, long-term or frequent use of antibiotics can easily lead to bacterial resistance and intestinal flora imbalance, among other side effects; and thirdly, existing therapies are not designed for the oral environment and cannot be used long-term as routine oral care methods.

[0004] In the field of oral care, toothpaste, as the most commonly used daily cleaning product, has evolved from its single function of cleaning and stain removal to include multiple benefits such as preventing cavities, reducing sensitivity, whitening, inhibiting plaque, and addressing gum problems. Currently available whitening toothpastes generally lack the ability to inhibit specific oral pathogens, especially Helicobacter pylori, and their functions are relatively limited.

[0005] While some studies and products have attempted to add broad-spectrum antibacterial ingredients (such as triclosan and chlorhexidine) to toothpaste to inhibit plaque, these ingredients carry risks such as disrupting the oral flora balance, causing tooth discoloration, or irritating the oral mucosa, and are not specifically targeted at Helicobacter pylori. Furthermore, a few patents or publications have proposed adding specific extracts or ingredients to mouthwashes or oral sprays to inhibit oral Helicobacter pylori, but these formulations are generally used less frequently and have lower compliance rates than toothpaste, and similarly, may not be organically integrated with teeth whitening functions.

[0006] Therefore, there is a significant gap in the existing technology: a lack of daily oral care products that can effectively inhibit oral Helicobacter pylori and provide safe and reliable teeth whitening. Summary of the Invention

[0007] To address the aforementioned technical problems, this invention proposes a whitening toothpaste that inhibits oral Helicobacter pylori and its preparation method. The aim is to continuously intervene in the colonization of oral Helicobacter pylori through daily brushing, which is a high-frequency activity. This satisfies consumers' demand for teeth whitening while improving overall oral health and assisting in the prevention and treatment of Helicobacter pylori infection.

[0008] To achieve the above objectives, the present invention provides a whitening toothpaste that inhibits Helicobacter pylori in the oral cavity, comprising the following components by weight: 2-4 parts of microbial active ingredient complex, 5-10 parts of clove, 0.2-0.4 parts of comfrey oil, 0.04-0.06 parts of bisabolol, 30-50 parts of abrasive, 0.4-0.6 parts of thickener, 25-35 parts of humectant, 4-6 parts of soapberry saponin, 0.05-0.15 parts of sweetener, 0.2-0.4 parts of preservative, and 10-15 parts of water.

[0009] Preferably, the microbial active ingredient complex includes Enterococcus faecalis (… Enterococcus faecium CICC20089 and Acetobacter pasteurellosis ( Acetobacter pasteurianus Fermented products.

[0010] Preferably, the mass ratio of Enterococcus faecalis CICC 20089 to Acetobacter pasteurellium ferment is 1:1.

[0011] A further preferred method for preparing the *Acetobacter pasteurellium* ferment is as follows: *Acetobacter pasteurellium* CICC20001 is inoculated into an acetic acid bacteria liquid culture medium, aerobically cultured at 28-32°C for 12-36 hours, then centrifuged, the supernatant is collected, and freeze-dried under vacuum to obtain the *Acetobacter pasteurellium* ferment.

[0012] Preferably, the abrasive is calcium carbonate and / or silicon dioxide, the thickener is sodium carboxymethyl cellulose and / or gum arabic, the humectant is glycerin, the sweetener is sorbitol and / or xylitol, and the preservative is sodium benzoate.

[0013] The present invention also provides a method for preparing the whitening toothpaste, comprising the following steps: 1) Acetobacter pasteurellium CICC 20001 was inoculated into acetic acid bacteria liquid culture medium and cultured aerobically at 28~32℃ for 12~36h. Then, it was centrifuged, the supernatant was collected, and the product was freeze-dried under vacuum to obtain the Acetobacter pasteurellium fermentation product. 2) Mix Enterococcus faecalis CICC 20089 and the fermentation product of Acetobacter pasteurization obtained in step 1) to prepare a microbial active ingredient complex; 3) Clove, comfrey oil, and bisabolol are premixed to obtain component A; 4) Mix the abrasive, thickener, humectant, soapberry saponin, sweetener, preservative and water to obtain component B; 5) Add the microbial active ingredient complex obtained in step 2) and component A obtained in step 3) to component B obtained in step 4) to obtain whitening toothpaste.

[0014] Preferably, the formula of the acetic acid bacteria liquid culture medium in step 1) is: 90-110g glucose, 5-15g yeast extract, 15-25g calcium carbonate, 15-25mL ethanol, and 1000mL distilled water.

[0015] Preferably, in step 1), the vacuum degree of the vacuum freeze-drying is 10~50 Pa, the temperature of the vacuum freeze-drying is -25~-35℃, and the vacuum freezing time is 24~48h.

[0016] Compared with the prior art, the present invention has the following advantages and technical effects: This invention provides a whitening toothpaste that inhibits oral Helicobacter pylori and its preparation method. This invention utilizes a microbial active ingredient complex and the synergistic effect of clove, comfrey oil, and bisabolol to achieve the effect of inhibiting oral Helicobacter pylori. Combined with a specific amount of exfoliating agent, it can simultaneously achieve a whitening effect. In this invention, clove inhibits urease, comfrey oil provides broad-spectrum antibacterial and anti-inflammatory effects, and bisabolol further repairs and soothes the mucosa. This inhibits oral Helicobacter pylori through a direct bactericidal to anti-inflammatory repair pathway. The microbial active ingredient complex of this invention utilizes the synergistic effect of Enterococcus faecalis CICC20089 and Acetobacter pasteurization. Enterococcus faecalis competitively inhibits Helicobacter pylori colonization, while Acetobacter pasteurization disrupts the cell membrane and internal structure of Helicobacter pylori, inhibiting its urease activity. Combined with the direct bactericidal to anti-inflammatory repair pathway, this achieves the effect of inhibiting oral Helicobacter pylori. The formula of this invention is mild and effective. Attached Figure Description

[0017] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0018] Figure 1 These are dental photographs of subjects in Experiment 1, Experiment 2, Experiment 3, Control 1, Control 2, and Blank group before the start of the experiment. Among them, A is the subject of Experiment 1, B is the subject of Experiment 2, C is the subject of Experiment 3, D is the subject of Control 1, E is the subject of Control 2, and F is the subject of Blank group. Figure 2These are dental photographs of subjects in Experiment 1, Experiment 2, Experiment 3, Control 1, Control 2, and Blank group one week after the start of the experiment. Among them, A is the subject of Experiment 1, B is the subject of Experiment 2, C is the subject of Experiment 3, D is the subject of Control 1, E is the subject of Control 2, and F is the subject of Blank group. Figure 3 These are dental photographs of subjects in Experiment 1, Experiment 2, Experiment 3, Control 1, Control 2, and Blank group 4 weeks after the start of the experiment. Among them, A is the subject of Experiment 1, B is the subject of Experiment 2, C is the subject of Experiment 3, D is the subject of Control 1, E is the subject of Control 2, and F is the subject of Blank group. 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. Every smaller range between any stated value or intermediate value within a stated range, and 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] Unless otherwise specified, the term "parts" in this invention refers to parts by weight.

[0025] Example 1 The microbial active ingredient complex (Enterococcus faecalis CICC 20089 and Acetobacter pasteurization ferment in a 1:1 mass ratio) consists of 3 parts clove, 7.5 parts comfrey oil, 0.3 parts bisabolol, 40 parts calcium carbonate, 0.5 parts sodium carboxymethyl cellulose, 30 parts glycerin, 5 parts soapberry saponins, 0.10 parts xylitol, 0.3 parts sodium benzoate, and 13.25 parts water.

[0026] 1) Acetobacter pasteurellium CICC 20001 was inoculated into acetic acid bacteria liquid culture medium (the formula of acetic acid bacteria liquid culture medium is: glucose 100g, yeast extract 10g, calcium carbonate 20g, ethanol 20mL, distilled water 1000mL), and cultured aerobically at 30℃ for 24h. Then, it was centrifuged at 4℃, 10000rpm for 20min, and the supernatant was collected. It was then freeze-dried in vacuum at 30Pa, -30℃ for 36h to obtain the fermentation product of Acetobacter pasteurellium. 2) A microbial active ingredient complex was prepared by mixing Enterococcus faecalis CICC 20089 and Acetobacter pasteurization product; 3) Clove, comfrey oil, and bisabolol are premixed to obtain component A; 4) Calcium carbonate, sodium carboxymethyl cellulose, glycerol, soapberry saponins, xylitol, sodium benzoate and water are mixed to obtain component B; 5) Add the microbial active ingredient complex and component A to component B to obtain whitening toothpaste.

[0027] Example 2 The microbial active ingredient complex (Enterococcus faecalis CICC 20089 and Acetobacter pasteurization ferment in a 1:1 mass ratio) consists of 2 parts clove, 5 parts comfrey oil, 0.2 parts bisabolol, 30 parts silica, 0.4 parts gum arabic, 25 parts glycerin, 4 parts soapberry saponins, 0.05 parts sorbitol, 0.2 parts sodium benzoate, and 10 parts water.

[0028] 1) Acetobacter pasteurellium CICC 20001 was inoculated into acetic acid bacteria liquid culture medium (the formula of acetic acid bacteria liquid culture medium is: glucose 100g, yeast extract 10g, calcium carbonate 20g, ethanol 20mL, distilled water 1000mL), and cultured aerobically at 28℃ for 36h. Then, it was centrifuged at 4℃, 10000rpm for 20min, and the supernatant was collected. It was then freeze-dried in vacuum at 10Pa, -25℃ for 48h to obtain the fermentation product of Acetobacter pasteurellium. 2) A microbial active ingredient complex was prepared by mixing Enterococcus faecalis CICC 20089 and Acetobacter pasteurization product; 3) Clove, comfrey oil, and bisabolol are premixed to obtain component A; 4) Mix silica, gum arabic, glycerin, soapberry saponins, sorbitol, sodium benzoate and water to obtain component B; 5) Add the microbial active ingredient complex and component A to component B to obtain whitening toothpaste.

[0029] Example 3 The microbial active ingredient complex (Enterococcus faecalis CICC 20089 and Acetobacter pasteurization ferment in a 1:1 mass ratio) consisted of 4 parts clove, 10 parts comfrey oil, 0.4 parts bisabolol, 0.06 parts calcium carbonate, 0.6 parts sodium carboxymethyl cellulose, 35 parts glycerin, 6 parts soapberry saponins, 0.15 parts xylitol, 0.4 parts sodium benzoate, and 15 parts water.

[0030] 1) Acetobacter pasteurellium CICC 20001 was inoculated into acetic acid bacteria liquid culture medium (the formula of acetic acid bacteria liquid culture medium is: glucose 100g, yeast extract 10g, calcium carbonate 20g, ethanol 20mL, distilled water 1000mL), and cultured aerobically at 32℃ for 12h. Then, it was centrifuged at 4℃ and 10000rpm for 20min. The supernatant was collected and freeze-dried in vacuum at 50Pa and -35℃ for 24h to obtain the fermentation product of Acetobacter pasteurellium. 2) A microbial active ingredient complex was prepared by mixing Enterococcus faecalis CICC 20089 and Acetobacter pasteurization product; 3) Clove, comfrey oil, and bisabolol are premixed to obtain component A; 4) Calcium carbonate, sodium carboxymethyl cellulose, glycerol, soapberry saponins, xylitol, sodium benzoate and water are mixed to obtain component B; 5) Add the microbial active ingredient complex and component A to component B to obtain whitening toothpaste.

[0031] Comparative Example 1 The microbial active ingredient complex (Enterococcus faecalis CICC 20089 and Acetobacter pasteurization ferment in a 1:1 mass ratio) consisted of 3 parts, clove 7.7 parts, bisabolol 0.15 parts, calcium carbonate 40 parts, sodium carboxymethyl cellulose 0.5 parts, glycerol 30 parts, soapberry saponins 5 parts, xylitol 0.10 parts, sodium benzoate 0.3 parts, and water 13.25 parts.

[0032] 1) Acetobacter pasteurellium CICC 20001 was inoculated into acetic acid bacteria liquid culture medium (the formula of acetic acid bacteria liquid culture medium is: glucose 100g, yeast extract 10g, calcium carbonate 20g, ethanol 20mL, distilled water 1000mL), and cultured aerobically at 30℃ for 24h. Then, it was centrifuged at 4℃, 10000rpm for 20min, and the supernatant was collected. It was then freeze-dried in vacuum at 30Pa, -30℃ for 36h to obtain the fermentation product of Acetobacter pasteurellium. 2) A microbial active ingredient complex was prepared by mixing Enterococcus faecalis CICC 20089 and Acetobacter pasteurization product; 3) Clove and bisabolol are premixed to obtain component A; 4) Calcium carbonate, sodium carboxymethyl cellulose, glycerol, soapberry saponins, xylitol, sodium benzoate and water are mixed to obtain component B; 5) Add the microbial active ingredient complex and component A to component B to obtain whitening toothpaste.

[0033] Comparative Example 2 The microbial complex (Enterococcus faecalis CICC 20089 and Acetobacter pasteurellis CICC 20001 in a 1:1 mass ratio) consisted of 3 parts clove, 7.5 parts comfrey oil, 0.3 parts bisabolol, 0.05 parts calcium carbonate, 40 parts sodium carboxymethyl cellulose, 0.5 parts glycerol, 30 parts soapberry saponins, 5 parts xylitol, 0.10 parts sodium benzoate, and 13.25 parts water.

[0034] 1) A microbial complex was prepared by mixing Enterococcus faecalis CICC 20089 and Acetobacter pasteurellum CICC 20001; 2) Clove, comfrey oil, and bisabolol are premixed to obtain component A; 3) Calcium carbonate, sodium carboxymethyl cellulose, glycerol, soapberry saponins, xylitol, sodium benzoate and water are mixed to obtain component B; 4) Add the microbial complex and component A to component B to obtain whitening toothpaste.

[0035] Experimental Example 1 300 participants aged 20-40 with no smoking or other unhealthy habits were recruited and tested using a commercially available rapid urease test (RUT). HpVolunteer participants were eligible to participate if they met the following criteria: good general health with no other systemic diseases; a total of at least 24 natural teeth in their mouth, including at least 4 molars (excluding third molars); no antibiotics or stomach medications taken in the past 3 months; no periodontal treatment received in the past 12 months; and the ability to cooperate actively and master daily oral hygiene methods. Participants were divided into 6 groups of 50 each: Experimental Group 1, Experimental Group 2, Experimental Group 3, Control Group 1, Control Group 2, and Blank Group. Experimental Group 1: Patients used a soybean-sized amount of whitening toothpaste prepared in Example 1 for daily oral cleaning for 3 minutes within 30 minutes after each meal, for a period of 4 weeks; Experimental Group 2: Patients used a soybean-sized amount of whitening toothpaste prepared in Example 2 for daily oral cleaning for 3 minutes within 30 minutes after each meal, for a period of 4 weeks; Experimental Group 3: Patients used a soybean-sized amount of whitening toothpaste prepared in Example 3 for daily oral cleaning for 3 minutes within 30 minutes after each meal, for a period of 4 weeks; Control Group 1: Patients used a soybean-sized amount of whitening toothpaste prepared in Comparative Example 1 for daily oral cleaning for 3 minutes within 30 minutes after each meal, for a period of 4 weeks; Control Group 2: Patients used a soybean-sized amount of whitening toothpaste prepared in Comparative Example 2 for daily oral cleaning for 3 minutes within 30 minutes after each meal, for a period of 4 weeks; Blank Group: Patients used a soybean-sized amount of commercially available Shuke Enzyme Whitening Toothpaste for daily oral cleaning for 3 minutes within 30 minutes after each meal, for a period of 4 weeks.

[0036] One week and four weeks after the start of the experiment, all enrolled subjects underwent routine intraoral examinations. The molar with the most severe gingival inflammation was selected from each patient's oral cavity as the sampling site. After isolating the tooth with a cotton ball and drying the tooth surface, a plaque sample was scraped from the gingival margin using a sterilized curette, and Helicobacter pylori (Hp) was immediately detected using the rapid urease method.

[0037] Table 1. Rapid urease assay one week after the start of the experiment. Hp result

[0038] Table 2. Rapid urease assay 4 weeks after the start of the experiment Hp result

[0039] As shown in Tables 1 and 2, one week after the start of the experiment, in Experiment 1 group... Hp The highest percentage of patients tested negative, at 40%, was those who tested negative. The toothpaste prepared in this invention showed an average improvement after one week of use. Hp The negative conversion rate was 37.33%, significantly higher than that of control group 1 and control group 2; four weeks after the start of the experiment, the negative conversion rate in experimental group 1 was significantly higher than that in control group 2. HpThe percentage of people who tested negative was still the highest, reaching 88%, indicating that the whitening toothpaste prepared in Example 1 of this invention can effectively inhibit Helicobacter pylori in the oral cavity. This effect is achieved by the combination of all functional ingredients.

[0040] Experiment Example 2 One subject from each group in Experiment Example 1 was randomly selected, for a total of 6 subjects. Dental photographs were taken of the subjects before the start of the experiment, one week after the start of the experiment, and four weeks after the start of the experiment, while maintaining uniform lighting and location in the shooting environment.

[0041] Corresponding comparison Figure 1 China A~ Figure 1 China F and Figure 2 China A~ Figure 2 In the middle F, it can be seen that the yellow color of the teeth of the subjects in experimental group 1, experimental group 2, experimental group 3 and blank group was slightly lighter, and the color of dental plaque was slightly lighter. There was basically no change in control group 1, and the yellow color of the teeth of control group 2 was slightly lighter.

[0042] Corresponding comparison Figure 1 China A~ Figure 1 China F and Figure 3 China A~ Figure 3 In the middle F, it can be seen that the yellow color of the teeth of the subjects in experimental group 1, experimental group 2, experimental group 3 and blank group was significantly reduced and the dental plaque was improved. There was no significant change in the subjects in control group 1, and the yellow color of the teeth of the subjects in control group 2 was slightly reduced and the dental plaque color was slightly lighter.

[0043] 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 whitening toothpaste that inhibits oral Helicobacter pylori, characterized in that, Includes the following components by weight: Microbial active ingredient complex 2-4 parts, clove 5-10 parts, comfrey oil 0.2-0.4 parts, bisabolol 0.04-0.06 parts, exfoliant 30-50 parts, thickener 0.4-0.6 parts, moisturizer 25-35 parts, soapberry saponin 4-6 parts, sweetener 0.05-0.15 parts, preservative 0.2-0.4 parts, water 10-15 parts.

2. The whitening toothpaste according to claim 1, characterized in that, The microbial active ingredient complex includes Enterococcus faecalis ( Enterococcus faecium CICC 20089 and Acetobacter pasteurellosis ( Acetobacter pasteurianus Fermented products.

3. The whitening toothpaste according to claim 2, characterized in that, The mass ratio of Enterococcus faecalis CICC 20089 and Acetobacter pasteurellium fermentation product was 1:

1.

4. The whitening toothpaste according to claim 2, characterized in that, The preparation method of the *Acetobacter pasteurellium* ferment is as follows: Acetobacter pasteurellium CICC 20001 was inoculated into acetic acid bacteria liquid culture medium and cultured aerobically at 28-32℃ for 12-36 hours. Then, it was centrifuged, the supernatant was collected, and the product was freeze-dried under vacuum to obtain the Acetobacter pasteurellium fermentation product.

5. The whitening toothpaste according to claim 1, characterized in that, The abrasive is calcium carbonate and / or silicon dioxide, the thickener is sodium carboxymethyl cellulose and / or gum arabic, the humectant is glycerin, the sweetener is sorbitol and / or xylitol, and the preservative is sodium benzoate.

6. The method for preparing the whitening toothpaste according to any one of claims 1 to 5, characterized in that, Includes the following steps: 1) Acetobacter pasteurellium CICC 20001 was inoculated into acetic acid bacteria liquid culture medium and cultured aerobically at 28~32℃ for 12~36h. Then, it was centrifuged, the supernatant was collected, and the product was freeze-dried under vacuum to obtain the Acetobacter pasteurellium fermentation product. 2) Mix Enterococcus faecalis CICC 20089 and the fermentation product of Acetobacter pasteurization obtained in step 1) to prepare a microbial active ingredient complex; 3) Clove, comfrey oil, and bisabolol are premixed to obtain component A; 4) Mix the abrasive, thickener, humectant, soapberry saponin, sweetener, preservative and water to obtain component B; 5) Add the microbial active ingredient complex obtained in step 2) and component A obtained in step 3) to component B obtained in step 4) to obtain whitening toothpaste.

7. The preparation method according to claim 6, characterized in that, The formula for the acetic acid bacteria liquid culture medium in step 1) is: 90-110g glucose, 5-15g yeast extract, 15-25g calcium carbonate, 15-25mL ethanol, and 1000mL distilled water.

8. The preparation method according to claim 6, characterized in that, Step 1) The vacuum degree of the vacuum freeze-drying is 10~50Pa, the temperature of the vacuum freeze-drying is -25~-35℃, and the vacuum freezing time is 24~48h.

Images