Chitosan-containing anti-allergic powder for nose and preparation method of chitosan-containing anti-allergic powder

Abstract

The invention relates to chitosan-containing nasal anti-allergic powder and a preparation method thereof, belongs to the technical field of medicines, and solves the problem that a barrier film formed by an existing nasal anti-allergic product is relatively short in residence time in a nasal cavity. The nasal antiallergic powder is prepared from modified chitosan containing-NH3 < + >, carboxymethyl chitosan, a soothing agent and a preservative, the anti-allergic powder for the nose is prepared from the following components in parts by weight: 30 to 70 parts of modified chitosan containing-NH < 3 + >, 30 to 50 parts of carboxymethyl chitosan, 0.1 to 2 parts of a soothing agent and 0.0001 to 0.1 part of a preservative. The nasal antiallergic powder can stay in a nasal cavity for a long time, and can instantly expand to form a film when being in contact with the moist nasal cavity.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of medicine, in particular to a chitosan-containing nasal antiallergic powder and a preparation method thereof. BACKGROUND

[0002] Nasal allergy is a common chronic inflammatory disease, which is characterized by the overreaction of nasal mucosa to allergens after the contact of atopic individuals with allergens, and is a type I allergic reaction of nasal mucosa mediated by IgE and involving multiple cytokines. Among them, dendritic cells (DCs) are the main antigen-presenting cells in the nasal mucosa, which can capture and process allergens and activate specific T cells, thereby triggering allergic inflammatory reactions such as sneezing, rhinorrhea, nasal mucosa redness, sensitivity, pain, and even life-threatening allergic asthma in severe cases. With the changes in people's lifestyle, combined with genetic and environmental factors, the incidence of allergic diseases is increasing. Allergic rhinitis can occur at any age, and the symptoms will gradually worsen after the onset, leading to a decrease in quality of life. Clinically, nasal direct medication combined with oral administration of corresponding drugs is usually used for treatment, which can greatly relieve the symptoms of allergic rhinitis during the medication period, but the symptoms of allergy will quickly appear again after the medication is stopped once the allergen is contacted. Moreover, the clinical administration usually uses antiallergic drugs such as mometasone furoate, budesonide, and loratadine, which have large side effects and cannot be used frequently.

[0003] Nasal local immune response plays a key role in the occurrence and development of nasal allergy, so nasal direct medication to block the contact of nasal mucosa with allergens can prevent the occurrence of allergic rhinitis. Chitosan is a natural polymer material with biocompatibility, biodegradability, and low toxicity, and its surface has a positive charge, which can produce strong electrostatic action with the negative nasal mucosa, so that chitosan is not easily removed by nasal cilia, thereby providing longer protection time for the nasal mucosa. Moreover, chitosan swells in the presence of water in the moist environment of the nasal cavity, forming a film-like material in the nasal cavity, which can prevent the combination of sensitizing substances in the external environment with receptors in the nasal cavity, thereby relieving the symptoms of allergic rhinitis.

[0004] Existing anti-nasal allergy products include gels, liquids, pastes, and powders in different dosage forms. However, the nasal mucosa is covered with numerous cilia, and its cleaning function makes the retention time of the drug in the nasal cavity only 15-30 min, and the residence time of the barrier film in the nasal cavity is also not long, so the user needs to administer the drug in time, which is inconvenient to operate, and forgetting to repeat the administration can easily cause allergy. Therefore, it is of great significance to develop an anti-allergic product with long retention time in the nasal cavity. SUMMARY

[0005] Based on the above analysis, the present invention aims to provide a chitosan-containing nasal anti-allergy powder and its preparation method, in order to solve the problem that the barrier film formed by existing nasal anti-allergy products has a short residence time in the nasal cavity.

[0006] On one hand, embodiments of the present invention provide a nasal anti-allergy powder containing chitosan, wherein the nasal anti-allergy powder comprises -NH3 + Modified chitosan, carboxymethyl chitosan, soothing agents, and preservatives; wherein, by weight, the nasal anti-allergy powder comprises: 30-70 parts containing -NH3 + Modified chitosan, 30-50 parts carboxymethyl chitosan, 0.1-2 parts soothing agent, 0.0001-0.1 parts preservative.

[0007] Preferably, the modified chitosan is at least one of chitosan acetate, chitosan hydrochloride, and chitosan lactate.

[0008] Preferably, the method for preparing the modified chitosan includes: dissolving chitosan in one of acetic acid, hydrochloric acid, and lactic acid, stirring until completely dissolved, adding a pH adjuster to cause chitosan gel to precipitate, redissolving the chitosan gel in an acid solution, and then preparing solid modified chitosan through post-treatment.

[0009] Preferably, the carboxymethyl chitosan is sodium carboxymethyl chitosan and / or potassium carboxymethyl chitosan.

[0010] Preferably, the preservative is at least one of benzalkonium chloride, benzalkonium bromide, and methylparaben.

[0011] Preferably, the soothing agent is at least one of ectoine, dipotassium glycyrrhizate, and glycyrrhetinic acid.

[0012] Preferably, the particle size of the nasal anti-allergy powder is 15-150 μm.

[0013] Preferably, the pH value of the nasal anti-allergy powder is 5.0-7.5.

[0014] Secondly, the present invention also provides a method for preparing the above-mentioned nasal anti-allergy powder, the method comprising: Chitosan was dissolved in acid and then post-treated to prepare solid modified chitosan. Modified chitosan, carboxymethyl chitosan, preservatives, and soothing agents were pulverized and sieved respectively, and particles with a particle size range of 15-150μm were collected respectively. Particles with a diameter in the range of 15-150μm are mixed according to their respective mass fractions and then filled into powder spray bottles.

[0015] Preferably, the post-treatment is one of drying, solvent precipitation / separation, or freeze-drying.

[0016] Compared with the prior art, the present invention can achieve at least one of the following beneficial effects: 1. In the chitosan-containing nasal anti-allergy powder of the present invention, the modified chitosan is hydrophilic, film-forming, positively charged, and can be adsorbed onto the negatively charged nasal mucosa; the molecular chain of carboxymethyl chitosan contains -COO - The modified chitosan molecular chain contains protonated amino groups -NH3. + After absorbing water, the two groups combine through electrostatic interaction to form a three-dimensional network structure. The appearance is a dense membrane structure that is insoluble in water. It adheres to the surface of the nasal cavity to form a physical protective layer. It will not be dissolved by nasal secretions and can only be cleared out of the nasal cavity by cilia, thus prolonging its residence time in the nasal cavity and thus effectively blocking allergens for a long time.

[0017] 2. The chitosan-containing nasal anti-allergy powder of the present invention rapidly absorbs water and swells upon contact with moisture in the moist nasal cavity, forming a water-insoluble physical protective film on the nasal mucosa surface within 5 seconds. This film can block external allergens such as pollen, dust, and animal dander for a long time, and continuously releases soothing and moisturizing agents such as ectoine, thereby moisturizing, reducing nasal mucosal edema and inflammation, and promoting the restoration of normal nasal function. The antibacterial effect of chitosan can improve the cleanliness of microorganisms in the nasal cavity, preventing the occurrence or aggravation of rhinitis due to bacterial proliferation.

[0018] In this invention, the above-described technical solutions can be combined with each other to achieve more preferred combinations. Other features and advantages of this invention will be set forth in the following description, and some advantages may become apparent from the description or be learned by practicing the invention. The objects and other advantages of this invention can be realized and obtained from what is particularly pointed out in the description and drawings. Attached Figure Description

[0019] The accompanying drawings are for illustrative purposes only and are not intended to limit the invention. Throughout the drawings, the same reference numerals denote the same parts.

[0020] Figure 1 This is a process flow diagram for preparing the chitosan-containing nasal anti-allergy powder of the present invention. Figure 2 This is a photograph of the chitosan-containing nasal anti-allergy powder prepared in Example 1. Figure 3 This is a water-based film morphology diagram of the chitosan-containing nasal anti-allergy powder prepared in Example 1. Figure 4 A photograph of the chitosan-containing nasal anti-allergy powder prepared in Comparative Example 2. Figure 5This is a water-based film morphology diagram of the chitosan-containing nasal anti-allergy powder prepared in Comparative Example 3. Detailed Implementation

[0021] Preferred embodiments of the present invention will now be described in detail with reference to the accompanying drawings, which form part of this application and are used together with the embodiments of the present invention to illustrate the principles of the present invention, but are not intended to limit the scope of the present invention.

[0022] The inventors discovered in their research that existing anti-nasal allergy products, when applied to the nasal cavity, form a barrier film on the nasal cavity surface that is soluble in water and can be miscible with nasal mucus. In addition, the cilia's wagging action cleanses the nasal cavity, resulting in the barrier film not staying in the nasal cavity for a long time.

[0023] Based on this, the present invention provides a nasal anti-allergy powder containing chitosan, wherein the nasal anti-allergy powder comprises -NH3 + Modified chitosan, carboxymethyl chitosan, soothing agents, and preservatives; wherein, by weight, the nasal anti-allergy powder comprises: 30-70 parts containing -NH3 + Modified chitosan (e.g., 30 parts, 40 parts, 50 parts, 60 parts, 70 parts), 30-50 parts carboxymethyl chitosan (e.g., 30 parts, 35 parts, 40 parts, 45 parts, 50 parts), 0.1-2 parts soothing agent (e.g., 0.1 parts, 0.5 parts, 1 part, 1.5 parts, 2 parts), 0.0001-0.1 parts preservative (e.g., 0.0001 parts, 0.001 parts, 0.01 parts, 0.1 parts).

[0024] In practice, the chitosan-containing nasal anti-allergy powder is placed in a powder spray bottle. When needed, the nasal anti-allergy powder is sprayed into the nasal cavity through the spray bottle.

[0025] Compared with the prior art, the chitosan-containing nasal anti-allergy powder of the present invention can rapidly absorb moisture and swell upon contact with moist nasal mucosa, forming a water-insoluble physical barrier on the nasal mucosa and releasing soothing agents, thereby exerting a long-lasting barrier, protective and anti-inflammatory effect.

[0026] For example, the mass ratio of modified chitosan to carboxymethyl chitosan is 1.1-1.5:1, more preferably 1.33:1. At this ratio, the modified chitosan and carboxymethyl chitosan can react completely.

[0027] For example, the modified chitosan is at least one of chitosan acetate, chitosan hydrochloride, and chitosan lactate, more preferably chitosan lactate. The modified chitosan is hydrophilic, film-forming, and positively charged, allowing it to adsorb onto the negatively charged nasal mucosa. Furthermore, the modified chitosan is water-soluble, and its amino groups are protonated, enabling it to complex with carboxymethyl chitosan.

[0028] For example, the method for preparing the modified chitosan includes: dissolving chitosan in an acid (e.g., acetic acid, hydrochloric acid, or lactic acid), stirring until completely dissolved, adding a pH adjuster to precipitate the chitosan gel, redissolving the chitosan gel in an acid solution (acetic acid solution, hydrochloric acid solution, or lactic acid solution), and then preparing solid modified chitosan through post-treatment.

[0029] For example, during the initial chitosan dissolution stage, the acid is added in the form of an acid solution with a mass concentration of 0.2-1%.

[0030] For example, in the initial chitosan dissolution stage, the mass-to-volume ratio of chitosan to acid solution is 1g:30-150mL.

[0031] For example, the stirring speed is 500-1000 rpm.

[0032] For example, the mass concentration of the pH adjuster is 0.4-1%.

[0033] For example, the pH adjuster adjusts the pH of the chitosan solution to 7.5-9, and chitosan gel is visible precipitating out.

[0034] For example, the pH adjuster is at least one of sodium hydroxide solution and potassium hydroxide solution.

[0035] For example, during the reconstitution stage, the mass-to-volume ratio of chitosan to acid solution is 1 g: 60-100 mL.

[0036] For example, during the reconstitution stage, the mass concentration of the acid solution is 0.1-0.2%, resulting in a chitosan reconstituted solution with a pH value of 5-6.5. When the modified chitosan obtained from this pH reconstituted solution is mixed with other components in the nasal anti-allergy powder, the nasal anti-allergy powder can possess a pH level that is non-irritating to the nasal mucosa.

[0037] For example, the post-processing is one of drying, solvent precipitation / separation, or freeze-drying, and more preferably freeze-drying.

[0038] For example, the solvent precipitation / separation includes using ethanol to precipitate the modified chitosan from the solution followed by filtration.

[0039] For example, the freeze-drying process includes: pre-freezing the chitosan solution at -20 to -80°C for 2-4 hours, and then freeze-drying it at -10 to -25°C for 4-8 hours.

[0040] For example, the carboxymethyl chitosan is sodium carboxymethyl chitosan and / or potassium carboxymethyl chitosan, more preferably sodium carboxymethyl chitosan.

[0041] For example, the preservative is at least one of benzalkonium chloride, benzalkonium bromide, and methylparaben, and more preferably benzalkonium chloride.

[0042] For example, the soothing agent is at least one of ectoine, dipotassium glycyrrhizate, and glycyrrhetinic acid, more preferably ectoine. Ectoine is derived from highly halophilic bacteria and is a strong hydrophilic substance that can calm and soothe irritated and damaged tissues. It has excellent anti-inflammatory properties and can be used to treat atopic dermatitis (neurodermatitis) or allergic skin diseases without side effects.

[0043] For example, the particle size of the nasal anti-allergy powder is 15-150μm, more preferably 45-74μm. Powder in this particle size range is easily sprayed continuously and evenly from the packaging bottle and will not enter the respiratory tract and lungs, thus ensuring safety.

[0044] For example, the pH value of the nasal anti-allergy powder is 5.0-7.5, more preferably 5.5-7.5. This pH value is non-irritating to the nasal mucosa.

[0045] Secondly, the present invention also provides a method for preparing the above-mentioned chitosan-containing nasal anti-allergy powder, such as... Figure 1 As shown, the preparation method includes: Chitosan was dissolved in acid and then post-treated to prepare solid modified chitosan. Modified chitosan, carboxymethyl chitosan, preservatives, and soothing agents were pulverized and sieved respectively, and particles with a particle size range of 15-150μm were collected respectively. Particles with a diameter in the range of 15-150μm are mixed according to their respective mass fractions and then filled into powder spray bottles.

[0046] Furthermore, the post-processing is one of drying, solvent precipitation / separation, or freeze-drying.

[0047] The nasal anti-allergy powder prepared by the method of the present invention can form a film rapidly on the nasal mucosa, and the physical barrier film formed is a non-water-soluble film that will not be dissolved by nasal secretions. It can stay in the nasal cavity for a long time, release soothing agents, reduce inflammatory reactions, and achieve a long-lasting anti-allergy effect.

[0048] The following specific embodiments further illustrate the chitosan-containing nasal anti-allergy powder and its preparation method of the present invention.

[0049] The film formation time and etching time detection methods in the following examples and comparative examples are as follows: Take a 50ml clean beaker, add an appropriate amount of physiological saline to wet the bottom of the beaker, quickly use a powder spray bottle to evenly spray 0.03g of powder onto the bottom of the beaker, add 7.5ml of physiological saline to fully wet the powder, observe the film formation time and record it; measure 20ml of physiological saline, cover the gel film, keep it at 37℃, shake it in a shaker (100 rpm), and observe the etching time of the gel film.

[0050] Example 1 (1) Dissolve 16g of chitosan in 480ml of acetic acid solution with a mass fraction of 1wt%, stir at 800rpm for 4h to completely dissolve it, add 1% sodium hydroxide pH adjuster to make the pH value of the solution 7.83, chitosan gel precipitates, filter out the chitosan gel, add 0.2% lactic acid solution to the total volume of 1300ml, stir until completely dissolved, so that the pH value of the chitosan redissolved solution is 5.95; pour the solution into the sample cell, pre-freeze at -50℃ for 2h, and then freeze-dry at -20℃ for 8h to obtain modified chitosan (i.e. chitosan lactate) solid, which is light yellow in color.

[0051] (2) The modified chitosan, sodium carboxymethyl chitosan, ectoine and benzalkonium chloride obtained are crushed and sieved in a pulverizer, and the powder particles that pass through the 200-mesh sieve but cannot pass through the 300-mesh sieve are taken for later use.

[0052] (3) Take the sieved particles according to the following mass proportions: 56.51 parts modified chitosan, 42.48 parts sodium carboxymethyl chitosan, 1 part ectoine, and 0.01 parts benzalkonium chloride. Mix them evenly to obtain a chitosan-containing nasal anti-allergy powder. Pack it into a powder spray bottle, as shown below. Figure 2 As shown.

[0053] The chitosan-containing nasal anti-allergy powder prepared in Example 1 has a pH of 6.91, a film-forming time of <5s, a microbial limit of 0 CFU / g, a dissolution time of >24h, and can be continuously and uniformly sprayed from a spray bottle. Furthermore, the nasal anti-allergy powder prepared in Example 1 forms a tough and uniform film upon contact with water, such as... Figure 3 As shown.

[0054] Example 2 (1) Dissolve 16g of chitosan in 480ml of acetic acid solution with a mass fraction of 1wt%, stir at 800rpm for 4h to completely dissolve it, add 1% sodium hydroxide pH adjuster to make the pH value of the solution 7.83, chitosan gel precipitates, filter out the chitosan gel, add 0.2% lactic acid solution to the total volume of 1300ml, stir until completely dissolved, so that the pH value of the chitosan redissolved solution is 5.95; pour the solution into the sample cell, pre-freeze at -50℃ for 2h, and then freeze-dry at -20℃ for 8h to obtain modified chitosan (i.e. chitosan lactate) solid.

[0055] (2) The modified chitosan, sodium carboxymethyl chitosan, ectoine and benzalkonium chloride obtained are crushed and sieved in a pulverizer, and the powder particles that pass through the 200-mesh sieve but cannot pass through the 300-mesh sieve are taken for later use.

[0056] (3) Take the sieved particles according to the mass fractions, 56.97 parts of modified chitosan, 42.82 parts of sodium carboxymethyl chitosan, 0.2 parts of dipotassium glycyrrhizate, and 0.01 parts of benzalkonium chloride, mix them evenly, and put them into a powder spray bottle.

[0057] The chitosan-containing nasal anti-allergy powder prepared in Example 2 has a pH value of 6.78, a film-forming time of <5s, a microbial limit of 0CFU / g, a dissolution time of >24h, and can be continuously and uniformly sprayed from the spray bottle. Furthermore, the nasal anti-allergy powder prepared in Example 2 can form a tough and uniform film when it comes into contact with water.

[0058] Comparative Example 1 The preparation method of this comparative example is similar to that of Example 1. The difference is that in step (1), the post-treatment of the chitosan solution is drying, and the acid solution used in the chitosan resolution stage is acetic acid solution. That is, step (1) is as follows: 16g of chitosan is dissolved in 480ml of acetic acid solution with a mass fraction of 1wt%, and stirred at 800rpm for 4h to make it completely dissolved. 1% sodium hydroxide is added as a pH adjuster to make the pH value of the solution 7.83. Chitosan gel is precipitated, and the chitosan gel is filtered out. 0.18% acetic acid solution is added to a total volume of 1300ml, and stirred until completely dissolved to make the pH value of the chitosan resolution solution 5.95. The solution is poured into the sample cell, dried at 40℃ for 24h, and then dried at 60℃ for 8h to obtain modified chitosan (chitosan acetate) solid, which is dark yellow in color.

[0059] The chitosan-containing nasal anti-allergy powder prepared in Comparative Example 1 had a pH of 8.03, a film-forming time of 8 seconds, a microbial limit of 0 CFU / g, a dissolution time of 4 hours, and could be continuously and uniformly sprayed from the spray bottle. In Comparative Example 1, the modified chitosan prepared by the drying method was darker in color because the high temperature triggered the Maillard reaction of chitosan. This reaction should be avoided to maintain the activity of chitosan. Furthermore, the modified chitosan after drying was slightly alkaline because acetic acid volatilized during the drying process. The resulting anti-allergy powder was alkaline, which could easily irritate the nasal mucosa and deteriorate the nasal environment.

[0060] Comparative Example 2 The preparation method of this comparative example is similar to that of Example 1. The difference is that step (2) is: the modified chitosan, sodium carboxymethyl chitosan, ectoine and benzalkonium chloride are crushed and sieved in a pulverizer, and the powder particles that pass through a 100-mesh sieve but cannot pass through a 200-mesh sieve are taken for later use.

[0061] The chitosan-containing nasal anti-allergy powder prepared in Comparative Example 2 was placed in a spray bottle, but the spray could not be continuously and evenly dispensed. Figure 4 As shown.

[0062] Comparative Example 3 (1) Dissolve 16g of chitosan in 480ml of acetic acid solution with a mass fraction of 1wt%, stir at 800rpm for 4h to completely dissolve it, add 1% sodium hydroxide pH adjuster to make the pH value of the solution 7.83, chitosan gel precipitates, filter out the chitosan gel, add 0.2% lactic acid solution to the total volume of 1300ml, stir until completely dissolved, so that the pH value of the chitosan redissolved solution is 5.95; pour the solution into the sample cell, pre-freeze at -50℃ for 2h, and then freeze-dry at -20℃ for 8h to obtain modified chitosan (i.e. chitosan lactate) solid.

[0063] (2) The modified chitosan, hydroxypropyl methylcellulose, ectoine and benzalkonium chloride obtained are crushed and sieved in a pulverizer, and the powder particles that pass through the 200-mesh sieve but not the 300-mesh sieve are taken for later use.

[0064] (3) Take the sieved particles according to the mass fractions, 56.51 parts of modified chitosan, 42.48 parts of hydroxypropyl methylcellulose, 1 part of ectoine, and 0.01 parts of benzalkonium chloride, mix them evenly, and put them into a powder spray bottle.

[0065] The chitosan-containing nasal anti-allergy powder prepared in Comparative Example 3 had a pH of 5.98, a film-forming time of <5s, a dissolution time of 6h, and the powder could be continuously and uniformly sprayed from the spray bottle. In Comparative Example 3, because the film-forming agent used was the non-ionic compound hydroxypropyl methylcellulose, it could not complex with the modified chitosan to form an insoluble substance. The resulting film was a water-soluble gel film, which would dissolve in nasal secretions and be cleared from the nasal cavity by cilia or nasal cleaning, and could not remain on the nasal mucosa for an extended period. Figure 5 As shown, (a) is the state of Comparative Example 3 immediately after water was added, and (b) is the state of Comparative Example 3 30 minutes after water was added.

[0066] Comparative Example 4 The preparation method of this comparative example is similar to that of Example 1, except that the same weight parts of sodium carboxymethyl chitosan salt are used instead of modified chitosan, that is, the nasal anti-allergy powder does not contain modified chitosan, and the weight parts of sodium carboxymethyl chitosan salt are 98.99 parts.

[0067] The anti-allergy nasal powder prepared in Comparative Example 4 had a pH of 7.58, a film-forming time of <5s, a microbial limit of 0 CFU / g, a dissolution time of 4.5h, and could be continuously and uniformly sprayed from the spray bottle.

[0068] Comparative Example 5 The preparation method of this comparative example is similar to that of Example 1, except that the same amount of modified chitosan is used instead of sodium carboxymethyl chitosan, that is, the nasal anti-allergy powder does not contain sodium carboxymethyl chitosan, and the amount of modified chitosan is 98.99 parts by weight.

[0069] The anti-allergy nasal powder prepared in Comparative Example 5 had a pH of 5.57, a film-forming time of <5s, a microbial limit of 0 CFU / g, a dissolution time of 3.5h, and could be continuously and uniformly sprayed from the spray bottle.

[0070] Comparative Example 6 The preparation method of this comparative example is similar to that of Example 1, except that chitosan is not modified, i.e., step (1) is omitted, and chitosan is used instead of modified chitosan in step (2).

[0071] The anti-allergy nasal powder prepared in Comparative Example 6 had a pH of 7.51, a film-forming time of <5s, a microbial limit of 0CFU / g, a dissolution time of 4h, and could be continuously and uniformly sprayed from the spray bottle.

[0072] Comparative Example 7 (1) Dissolve 16g of chitosan in 480ml of acetic acid solution with a mass fraction of 1wt%, stir at 800rpm for 4h to completely dissolve it, add 1% sodium hydroxide pH adjuster to make the pH value of the solution 7.83, chitosan gel precipitates, filter out the chitosan gel, add 0.2% lactic acid solution to the total volume of 1300ml, stir until completely dissolved, so that the pH value of the chitosan redissolved solution is 5.95; pour the solution into the sample cell, pre-freeze at -50℃ for 2h, and then freeze-dry at -20℃ for 8h to obtain modified chitosan (i.e. chitosan lactate) solid.

[0073] (2) The modified chitosan, sodium carboxymethyl chitosan, ectoine and benzalkonium chloride obtained are crushed and sieved in a pulverizer, and the powder particles that pass through the 200-mesh sieve but cannot pass through the 300-mesh sieve are taken for later use.

[0074] (3) Take the sieved particles according to the mass fraction, 35 parts of modified chitosan, 63.99 parts of sodium carboxymethyl chitosan, 1 part of ectoine, and 0.01 parts of benzalkonium chloride, mix them evenly, and put them into a powder spray bottle.

[0075] The chitosan-containing nasal anti-allergy powder prepared in Comparative Example 7 had a pH of 6.95, a film-forming time of <5s, a microbial limit of 0 CFU / g, a dissolution time of >24h, and the powder could be continuously and uniformly sprayed from the spray bottle. However, the nasal anti-allergy powder prepared in Comparative Example 7 formed a broken and uneven film upon contact with water, which is presumably due to an unsuitable weight ratio of carboxymethyl chitosan and modified chitosan. Compared with Example 1, the carboxymethyl chitosan and modified chitosan in Example 1 could react completely, forming a denser and thicker film, with better coverage of the nasal cavity and correspondingly longer coverage time.

[0076] Application Example 1 An in vitro cytotoxicity test (MTT method) was performed on the nasal anti-allergy powder of Example 1. The specific test method is as follows: (1) Take the chitosan-containing nasal anti-allergy powder prepared in Example 1, spread it thinly on the bottom of the petri dish, slowly add physiological saline, and after it forms a film, take out the film-like substance as the sample to be tested.

[0077] (2) The test was conducted in accordance with GB / T 16886.5-2017 Biological Evaluation of Medical Devices Part 5: In Vitro Cytotoxicity Tests. The extraction ratio of the test sample group was 0.2 g / ml. The results are shown in Table 1.

[0078] Table 1 Results of in vitro cytotoxicity test in Example 1

[0079] As can be seen from Table 1, the chitosan-containing nasal anti-allergy powder of Example 1 does not have potential cytotoxicity.

[0080] Application Example 2 The chitosan-containing nasal anti-allergy powders prepared in Examples 1 and 2 were tested on humans. The specific testing methods are as follows: 30 volunteers aged 18-55 years were selected for each experimental group. All volunteers were diagnosed with allergic rhinitis and had a clear allergen. They had experienced a recurrence of allergic rhinitis within the past six months. The anti-allergy powders prepared in Examples 1 and 2 were used respectively. The method of use was as follows: after cleaning the nasal cavity, the anti-allergy powder was sprayed into the left and right nasal cavities respectively. The dosage was 2-4 sprays per nasal cavity, once in the morning and once in the evening. The allergen could be exposed 10 minutes to 12 hours after using the anti-allergy powder. The use was continued for 15 days, and the results were recorded and archived. Evaluation method: (1) Efficacy: Inquire about the recurrence / relief of allergic rhinitis in volunteers. Significant effect is defined as a significant reduction in the number of allergic reactions or a significant reduction in allergic symptoms; effective effect is defined as a reduction in the number of allergic reactions or a reduction in allergic symptoms; ineffective effect is defined as no improvement in the number of allergic reactions or allergic symptoms. (2) User experience: If more than 80% of people feel no obvious discomfort in their nasal cavity after use, it is considered a good experience and is rated as "superior". If 60%-80% of people feel no discomfort after use, it is rated as "medium" and if less than 60% of people feel no discomfort, it is rated as "inferior".

[0081] The specific test results are shown in Table 2 below: Table 2. Results of Effect Evaluation and Performance Testing

[0082] As shown in Table 2, the chitosan-containing nasal anti-allergy powders prepared in Examples 1 and 2 can effectively prevent or relieve allergic rhinitis. Compared with Example 2, the soothing agent used in Example 1 is ectoine, and the anti-allergy powder prepared in Example 1 has a relatively better anti-allergy effect.

[0083] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any changes or substitutions that can be easily conceived by those skilled in the art within the scope of the technology disclosed in the present invention should be included within the scope of protection of the present invention.

Claims

1. A nasal anti-allergy powder containing chitosan, characterized in that, The nasal anti-allergy powder includes: containing -NH3 + Modified chitosan, carboxymethyl chitosan, soothing agents, and preservatives; wherein, by weight, the nasal anti-allergy powder comprises: 30-70 parts containing -NH3 + Modified chitosan, 30-50 parts carboxymethyl chitosan, 0.1-2 parts soothing agent, 0.0001-0.1 parts preservative.

2. The nasal anti-allergy powder according to claim 1, characterized in that, The modified chitosan is at least one of chitosan acetate, chitosan hydrochloride, and chitosan lactate.

3. The nasal anti-allergy powder according to claim 1, characterized in that, The method for preparing the modified chitosan includes: dissolving chitosan in one of acetic acid, hydrochloric acid, and lactic acid, stirring until completely dissolved, adding a pH adjuster to cause chitosan gel to precipitate, redissolving the chitosan gel in an acid solution, and then preparing solid modified chitosan through post-treatment.

4. The nasal anti-allergy powder according to claim 1, characterized in that, The carboxymethyl chitosan is sodium carboxymethyl chitosan and / or potassium carboxymethyl chitosan.

5. The nasal anti-allergy powder according to claim 1, characterized in that, The preservative is at least one of benzalkonium chloride, benzalkonium bromide, and methylparaben.

6. The nasal anti-allergy powder according to claim 1, characterized in that, The soothing agent is at least one of ectoine, dipotassium glycyrrhizate, and glycyrrhetinic acid.

7. The nasal anti-allergy powder according to claim 1, characterized in that, The particle size of the nasal anti-allergy powder is 15-150 μm.

8. The nasal anti-allergy powder according to claim 1, characterized in that, The pH value of the nasal anti-allergy powder is 5.0-7.

5.

9. The method for preparing nasal anti-allergy powder according to any one of claims 1 to 8, characterized in that, The preparation method includes: Chitosan was dissolved in acid and then post-treated to prepare solid modified chitosan. Modified chitosan, carboxymethyl chitosan, preservatives, and soothing agents were pulverized and sieved respectively, and particles with a particle size range of 15-150μm were collected respectively. Particles with a diameter in the range of 15-150μm are mixed according to their respective mass fractions and then filled into powder spray bottles.

10. The method for preparing the nasal anti-allergy powder according to claim 9, characterized in that, The post-processing is one of drying, solvent precipitation / separation, or freeze-drying.

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