A pet ear cleaning composition and a method of making the same

Abstract

The application discloses a pet ear cleaning liquid composition and a preparation method thereof, and belongs to the field of cleaning and nursing agents for pets. The composition comprises 1-10 parts of polylysine, 1-5 parts of hydroxyethyl cellulose, 1-5 parts of allantoin, 1-8 parts of hydrochloric acid and 90-100 parts of purified water in terms of weight fraction. The polylysine is alkylated modified polylysine. The ear cleaning liquid composition can soften and dissolve pet earwax, remove peculiar smell, prevent and assist in treating inflammation of ear canals caused by infection of Malassezia and the like, relieve itching symptoms, continuously play a role and nourish skin due to the addition of allantoin and cellulose derivative components, and has the characteristics of simple components, mild raw materials, no stimulation and low cytotoxicity due to the weak acid formula, and can be used for daily cleaning of ear canals of pets and auxiliary treatment of otitis of pets.

Description

Technical Field

[0001] This invention belongs to the field of pet cleaning and care products, specifically relating to a pet ear cleaning solution composition and its preparation method. Background Technology

[0002] Pets are man's most loyal and reliable friends, and an important part of our daily lives. They play a positive role in providing emotional companionship, relieving stress, and improving physical and mental health. However, improper care can also have negative effects on human health. Therefore, it is essential to practice proper care when living with pets.

[0003] In the process of scientific pet ownership, the cleaning and management of pets, especially the cleaning and care of the ear canals, is an indispensable part. This is mainly because the unique "L-shaped" ear canal structure of pets, especially dogs and cats, makes it difficult for earwax to be expelled, leading to the accumulation of earwax, earwax, and necrotic keratinocytes. If not cleaned in time, this can cause bacterial infections in the ear canal, resulting in diseases such as otitis externa and otitis media. Pet otitis often manifests as itching in the ear, redness of the auricle and ear canal, excessive discharge with an unpleasant odor, and in severe cases, suppuration with a foul odor, or even hyperplasia and blockage of the ear canal. Repeated inflammation can also cause thickening of the ear canal tissue, and even tumors, leading to thickened auricle skin, auricle deformation, and hearing impairment, seriously endangering the pet's health. Furthermore, since owners and pets are inseparable, neglecting the owner's hygiene and protection, or having a weakened immune system, can also harm the owner's health. For example, Malassezia, a pathogenic fungus in the ear canal, can cause pityriasis versicolor, seborrheic dermatitis, and Malassezia folliculitis in humans, while mites can easily cause allergic reactions in their owners. Therefore, when keeping pets, we need to pay close attention to their hygiene, especially the cleaning and care of their ear canals, to protect the health and safety of both the pet and its owner.

[0004] Current methods for cleaning and caring for pet ears primarily rely on topical ear cleaning solutions. These solutions are categorized into two types based on their cleaning agents: oil-based and water-based. Pure oil-based solutions mainly provide lubrication and soften the surface, requiring a second rinse afterward to prevent bacterial growth from residual oil, making them inconvenient to use. Water-based ear cleaning solutions, some primarily using H2O2 or NaHCO3, release gas to create bubbles that break up earwax, thus achieving cleaning. However, the sound of these bubbles breaking can easily frighten pets, leading to low acceptance. Other solutions use surfactants such as sodium docusate as the main cleaning ingredient, supplemented by boric acid and salicylic acid, resulting in significant cleaning effects, but with drawbacks such as high cytotoxicity and strong irritation. Therefore, developing a gentle, non-irritating, safe, and effective pet ear cleaning solution is essential for maintaining the health of both pets and their owners. Summary of the Invention

[0005] The purpose of this invention is to address the shortcomings of existing technologies by providing a pet ear cleaning solution composition, its preparation method, and its application. This composition can soften and dissolve excess earwax, earwax, and necrotic keratinocytes in pet ears, preventing and assisting in the treatment of ear canal inflammation caused by infections such as Malassezia. It also contains allantoin, hydroxyethyl cellulose, and other ingredients that nourish the skin while forming a long-lasting protective film, continuously protecting ear canal health. The weakly acidic formula is more suitable for the pet ear canal environment and is safe, gentle, and has low cytotoxicity. It is suitable for daily cleaning of pet ear canals, prevention of ear canal inflammation, and adjunctive treatment.

[0006] The technical solution adopted in this invention is implemented as follows:

[0007] This invention provides an alkylated modified polylysine, the structural formula of which is:

[0008]

[0009] It is a polymeric surfactant, and its preparation process is as follows:

[0010] (1) Stearic acid was dispersed in deionized water, and EDC (1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride) and NHS (N-hydroxysuccinimide) were added with stirring. The mixture was allowed to react fully at room temperature.

[0011] (2) Slowly add polylysine dissolved in deionized water and continue stirring the reaction.

[0012] (3) After the above reaction is completed, the reaction mixture is purified by dialysis with a molecular weight cutoff of 3400 for 8-24 hours to remove unreacted small molecule impurities.

[0013] (4) After reaching the end of dialysis, the liquid in the dialysis bag is filtered and then freeze-dried to obtain alkylated modified polylysine.

[0014] This invention provides a pet ear cleaning solution composition, comprising, by weight, 1-10 parts of polylysine, 1-5 parts of cellulose derivative, 1-5 parts of allantoin, 1-8 parts of hydrochloric acid, and 90-100 parts of purified water.

[0015] Preferably, the composition comprises, by weight ratio, the following raw materials: 5 parts polylysine, 1 part hydroxyethyl cellulose, 2 parts allantoin, 2.4 parts hydrochloric acid, and the remainder being purified water.

[0016] This invention provides a method for preparing a pet ear cleaning solution composition, comprising the following steps:

[0017] 1) Preparation of alkylated polylysine;

[0018] 2) Add poly-L-lysine to purified water and stir at room temperature until completely dissolved to prepare a stock solution for later use;

[0019] 3) Add allantoin to purified water and heat in a water bath at 48°C for 30-90 minutes until completely dissolved to prepare a stock solution for later use;

[0020] 4) Add hydroxyethyl cellulose to purified water and heat in a water bath at 48°C for 30-60 minutes until completely dissolved to prepare a stock solution for later use;

[0021] 5) Mix the mother liquors obtained in steps 2), 3), and 4) in the required proportions, stir well, and finally add hydrochloric acid to adjust the pH value of the pet ear cleaning solution.

[0022] The ear cleaning solution has a final pH value of 6.2-6.8, which is consistent with the slightly acidic environment of a pet's ear canal.

[0023] In summary, due to the adoption of the above technical solution, the beneficial effects of the present invention are:

[0024] 1. By modifying polylysine with stearic acid, a hydrophobic polylysine was prepared, which simultaneously possesses hydrophilic and hydrophobic groups, exhibiting typical structural characteristics of surfactants. In addition, it has both hydrophilic and lipophilic properties, making it more suitable for cleaning oily secretions in pet ear canals.

[0025] 2. The ear cleaning solution prepared by this invention does not contain irritating substances such as salicylic acid and sodium docusate. It uses polylysine as a cleaning agent and is safe, non-toxic, and non-irritating. It can soften and dissolve excess earwax and necrotic keratinocytes in pets' ears, and can be used for daily cleaning of pets' ear canals. At the same time, it can prevent and assist in the treatment of ear canal inflammation caused by bacteria such as Malassezia, and provide long-lasting protection for ear canal health.

[0026] Instruction manual illustrations

[0027] Figure 1 This is a schematic diagram of the preparation method of alkylated modified polylysine in this invention;

[0028] Figure 2 The hydrogen spectrum of the alkylated modified polylysine obtained;

[0029] Figure 3 This is a comparison chart of the cleaning capabilities of various examples of the present invention; Detailed Implementation

[0030] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0031] Example 1

[0032] A pet ear cleaning solution composition, by weight fraction, comprises the following components: 10 parts polylysine, 1 part hydroxyethyl cellulose, 2 parts allantoin, 3.6 parts hydrochloric acid, and the remainder being purified water.

[0033] The polyamino acid is alkylated modified polylysine.

[0034] The preparation method of the pet ear cleaning solution composition is as follows:

[0035] 1) Preparation of alkylated modified polylysine: Step 1: Stearic acid is dispersed in deionized water, and EDC (1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride) and NHS (N-hydroxysuccinimide) are added under stirring. The reaction is allowed to proceed fully at room temperature. Step 2: Polylysine dissolved in deionized water is slowly added, and the reaction is continued with stirring. Step 3: The reaction mixture is purified by dialyzing with a dialysis bag with a molecular weight cutoff of 3400 for 8-24 hours to remove unreacted small molecule impurities. Step 4: After reaching the dialysis endpoint, the liquid in the dialysis bag is filtered and freeze-dried to obtain stearic acid-functionalized polylysine.

[0036] 2) Add 80 parts of alkylated polylysine to a centrifuge tube, add 500 parts of purified water, stir at room temperature until completely dissolved, and prepare a stock solution for later use.

[0037] 3) Place 4 parts of allantoin into a flask, add 400 parts of purified water, and heat in a water bath at 48°C for 30-90 minutes until completely dissolved to prepare a stock solution for later use.

[0038] 4) Place 12 parts of hydroxyethyl cellulose in a flask, add 300 parts of purified water, and heat in a water bath at 48°C for 30-60 minutes until completely dissolved to prepare a stock solution for later use.

[0039] 5) Mix the mother liquors obtained in steps 2), 3), and 4) in the above proportions, stir well, and finally add hydrochloric acid to adjust the pH value of the pet ear cleaning solution.

[0040] Example 2

[0041] A pet ear cleaning solution composition, by weight fraction, comprises the following components: 5 parts polylysine, 1 part hydroxyethyl cellulose, 2 parts allantoin, 2.4 parts hydrochloric acid, and the remainder being purified water.

[0042] The polyamino acid is alkylated modified polylysine.

[0043] The preparation method of the pet ear cleaning solution composition is as follows:

[0044] 1) Preparation of alkylated modified polylysine: Step 1: Stearic acid is dispersed in deionized water, and EDC (1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride) and NHS (N-hydroxysuccinimide) are added under stirring. The reaction is allowed to proceed fully at room temperature. Step 2: Polylysine dissolved in deionized water is slowly added, and the reaction is continued with stirring. Step 3: The reaction mixture is purified by dialyzing with a dialysis bag with a molecular weight cutoff of 3400 for 8-24 hours to remove unreacted small molecule impurities. Step 4: After reaching the dialysis endpoint, the liquid in the dialysis bag is filtered and freeze-dried to obtain stearic acid-functionalized polylysine.

[0045] 2) Add 80 parts of alkylated polylysine to a centrifuge tube, add 500 parts of purified water, stir at room temperature until completely dissolved, and prepare a stock solution for later use.

[0046] 3) Place 4 parts of allantoin into a flask, add 400 parts of purified water, and heat in a water bath at 48°C for 30-90 minutes until completely dissolved to prepare a stock solution for later use.

[0047] 4) Place 12 parts of hydroxyethyl cellulose in a flask, add 300 parts of purified water, and heat in a water bath at 48°C for 30-60 minutes until completely dissolved to prepare a stock solution for later use.

[0048] 5) Mix the mother liquors obtained in steps 2), 3), and 4) in the above proportions, stir well, and finally add hydrochloric acid to adjust the pH value of the pet ear cleaning solution.

[0049] Example 3

[0050] A pet ear cleaning solution composition, by weight fraction, comprises the following components: 3 parts polylysine, 1 part hydroxyethyl cellulose, 2 parts allantoin, 1.8 parts hydrochloric acid, and the remainder being purified water.

[0051] The polyamino acid is alkylated modified polylysine.

[0052] The preparation method of the pet ear cleaning solution composition is as follows:

[0053] 1) Preparation of alkylated modified polylysine: Step 1: Stearic acid is dispersed in deionized water, and EDC (1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride) and NHS (N-hydroxysuccinimide) are added under stirring. The reaction is allowed to proceed fully at room temperature. Step 2: Polylysine dissolved in deionized water is slowly added, and the reaction is continued with stirring. Step 3: The reaction mixture is purified by dialyzing with a dialysis bag with a molecular weight cutoff of 3400 for 8-24 hours to remove unreacted small molecule impurities. Step 4: After reaching the dialysis endpoint, the liquid in the dialysis bag is filtered and freeze-dried to obtain stearic acid-functionalized polylysine.

[0054] 2) Add 80 parts of alkylated polylysine to a centrifuge tube, add 500 parts of purified water, stir at room temperature until completely dissolved, and prepare a stock solution for later use.

[0055] 3) Place 4 parts of allantoin into a flask, add 400 parts of purified water, and heat in a water bath at 48°C for 30-90 minutes until completely dissolved to prepare a stock solution for later use.

[0056] 4) Place 12 parts of hydroxyethyl cellulose in a flask, add 300 parts of purified water, and heat in a water bath at 48°C for 30-60 minutes until completely dissolved to prepare a stock solution for later use.

[0057] 5) Mix the mother liquors obtained in steps 2), 3), and 4) in the above proportions, stir well, and finally add hydrochloric acid to adjust the pH value of the pet ear cleaning solution.

[0058] Comparative Example 1

[0059] A pet ear cleaning solution composition, by weight fraction, comprises the following components: 10 parts polylysine, 1 part hydroxyethyl cellulose, 2 parts allantoin, 3.3 parts hydrochloric acid, and the remainder being purified water.

[0060] The polylysine was not alkylated.

[0061] The preparation method of the pet ear cleaning solution composition is as follows:

[0062] 1) Add 80 parts of poly-L-lysine to a centrifuge tube, add 500 parts of purified water, stir at room temperature until completely dissolved, and prepare a stock solution for later use.

[0063] 2) Place 4 parts of allantoin into a flask, add 400 parts of purified water, and heat in a water bath at 48°C for 30-90 minutes until completely dissolved to prepare a stock solution for later use.

[0064] 3) Place 12 parts of hydroxyethyl cellulose in a flask, add 300 parts of purified water, and heat in a water bath at 48°C for 30-60 minutes until completely dissolved to prepare a stock solution for later use.

[0065] 4) Mix the mother liquors obtained in steps 2), 3), and 4) in the above proportions, stir well, and finally add hydrochloric acid to adjust the pH value of the pet ear cleaning solution.

[0066] Comparative Example 2

[0067] A pet ear cleaning solution composition, by weight fraction, comprises the following components: 5 parts polylysine, 1 part hydroxyethyl cellulose, 2 parts allantoin, 2 parts hydrochloric acid, and the remainder being purified water.

[0068] The polylysine was not alkylated.

[0069] The preparation method of the pet ear cleaning solution composition is as follows:

[0070] 1) Add 80 parts of poly-L-lysine to a centrifuge tube, add 500 parts of purified water, stir at room temperature until completely dissolved, and prepare a stock solution for later use.

[0071] 2) Place 4 parts of allantoin into a flask, add 400 parts of purified water, and heat in a water bath at 48°C for 30-90 minutes until completely dissolved to prepare a stock solution for later use.

[0072] 3) Place 12 parts of hydroxyethyl cellulose in a flask, add 300 parts of purified water, and heat in a water bath at 48°C for 30-60 minutes until completely dissolved to prepare a stock solution for later use.

[0073] 4) Mix the mother liquors obtained in steps 2), 3), and 4) according to the above proportions, stir well, and finally add hydrochloric acid to adjust the pH value of the pet ear cleaning solution.

[0074] Comparative Example 3

[0075] A pet ear cleaning solution has the following ingredients: water, EDTA, PCMX, sodium docusate, salicylic acid, rhamnose, galactose, mannose, meadowsweet extract, belandro leaf extract, pigments, etc.

[0076] Test Example 1: Nuclear Magnetic Resonance Spectroscopy Analysis of Alkylated Polylysine Structure

[0077] Weigh approximately 10 mg of alkylated polylysine and dissolve it thoroughly in 600 μL of deuterium water. Filter the solution through a 0.22 μm aqueous filter and place it in an NMR tube. Perform proton NMR spectroscopy using a 500 MHz NMR instrument (Bruker DMX500). 1 Chemical structures were analyzed using 1H NMR.

[0078] See results Figure 2 .

[0079] Test Example 2: Surface Tension Measurement

[0080] Using deionized water as a solvent, alkylated modified polylysine and unalkylated polylysine were prepared into solutions of different concentrations. The surface tension of the liquids was measured using a DSA100 contact angle meter at 23°C, and the changes in IFT (mN / m) values ​​of the two solutions were compared.

[0081] The results are shown in Table 1.

[0082] Table 1

[0083]

[0084] As shown in Table 1, the surface tension of polylysine modified by alkylation is significantly reduced compared with that of the original polylysine at the same concentration, and the performance of its surfactant is significantly improved.

[0085] Test Example 3 Cleaning Ability Test

[0086] To more clearly illustrate the present invention, the cleaning abilities of the pet ear canal cleaners described in Examples 1-3 and Comparative Examples 1-3 of the present invention were tested and compared.

[0087] Weigh 0.5g of artificial earwax into a transparent bottle, add 1.5mL of the pet ear cleaning solution described in Examples 1-3 and Comparative Examples 1-3 respectively, and incubate in a 38℃ water bath for 30 minutes. Use an ELISA reader to read the absorbance value of each group at 350-400nm. Repeat the test 3 times and observe the liquid of each group to compare the cleaning ability of each group.

[0088] See results Figure 3

[0089] The results are as follows Figure 3 As shown, the absorbance value of the pet ear cleaner using alkylated polylysine as a cleaning agent was significantly higher than that of the unmodified polylysine group, indicating that its ability to dissolve earwax was significantly enhanced. It was also slightly better than commercially available ear cleaners using sodium docusate as the main cleaning ingredient.

[0090] Test Example 4: Antibacterial Capacity Test

[0091] To more clearly illustrate the present invention, the antibacterial ability of the pet ear canal cleaners described in Examples 1-3 and Comparative Examples 1-3 against Malassezia, a common bacterium in pet ear canals, was tested.

[0092] The results are shown in Table 2.

[0093] Table 2

[0094] Example 1 99.94％ Example 2 98.83％ Example 3 99.72％ Comparative Example 1 99.97％ Comparative Example 2 98.87％ Comparative Example 3 98.48％

[0095] The results are shown in Table 3. The ear washing solutions in Examples 1-3 and Comparative Examples 1-3 all showed good antibacterial effects against Malassezia, with antibacterial rates all exceeding 98%.

[0096] Test Example 5: Cytotoxicity Detection of Ear Wash Solution

[0097] To more clearly illustrate the present invention, the pet ear cleaning solutions described in Examples 1-3 and Comparative Examples 1-3 of the present invention were subjected to cytotoxicity testing using the CCK8 method.

[0098] The results are shown in Table 3.

[0099] Table 3

[0100] Example 1 >75％ Example 2 >75％ Example 3 >75％ Comparative Example 1 >75％ Comparative Example 2 >75％ Comparative Example 3 11.3％

[0101] The results are shown in Table 3. The cell survival rate of the ear cleaning solutions in Examples 1-3 and Comparative Examples 1-2 was over 75%, with low cytotoxicity. In contrast, a commercially available ear cleaning solution with sodium docusate as the cleaning ingredient had a cell survival rate of only 11.3%, with high cytotoxicity. The embodiments of the present invention are significantly superior to Comparative Example 3.

[0102] Test Example 6: Stability Test of Ear Wash Solution

[0103] To more clearly illustrate the present invention, the stability of Examples 1-3 was tested. Examples 1-3 were placed at 40℃ and -20℃ for 24 hours respectively, and after returning to room temperature, they were compared with the room temperature group to observe whether there were any significant changes in the state of the ear washing solution.

[0104] The samples from Examples 1-3 were placed at 40℃ and -20℃ for 24 hours respectively. After returning to room temperature, compared with the original liquid placed at room temperature, the liquid color did not change, and no substance precipitated or separated, proving that its stability is reliable.

[0105] Finally, it should be noted that the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A pet ear cleaning solution composition, characterized in that: The product comprises, by weight parts, the following components: 1-10 parts poly-L-lysine, 1-5 parts hydroxyethyl cellulose, 1-5 parts allantoin, 1-8 parts hydrochloric acid, and 90-100 parts purified water; wherein the poly-L-lysine is alkylated modified poly-L-lysine; the structural formula of the alkylated modified poly-L-lysine is: 。 2. The composition according to claim 1, characterized in that, The preparation method of the alkylated modified polylysine is as follows: (1) Disperse stearic acid in deionized water, add EDC (1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride) and NHS (N-hydroxysuccinimide) while stirring, and react fully at room temperature; (2) Slowly add polylysine dissolved in deionized water and continue stirring the reaction; (3) After the reaction is complete, the reaction mixture is purified by dialysis with a molecular weight cutoff of 3400 for 8-24 hours to remove unreacted small molecule impurities. (4) After reaching the end of dialysis, the liquid in the dialysis bag is filtered and then freeze-dried to obtain alkylated modified polylysine.

3. The method for preparing a pet ear-cleaning solution composition as described in claim 1, characterized in that, The preparation process includes the following steps: 1) Preparation of alkylated modified polylysine; 2) Add the prepared alkylated modified polylysine to purified water and stir at room temperature until completely dissolved to prepare a mother liquor for later use; 3) Add allantoin to purified water and heat in a water bath at 48°C for 30-90 minutes until completely dissolved to prepare a stock solution for later use; 4) Add hydroxyethyl cellulose to purified water and heat in a water bath at 48°C for 30-60 minutes until completely dissolved to prepare a stock solution for later use; 5) Mix the mother liquors obtained in steps 2), 3), and 4) in the required proportions, stir well, and finally add hydrochloric acid to adjust the pH value of the solution.

4. A method for preparing a pet ear-cleaning solution composition as described in claim 3, characterized in that, Add hydrochloric acid to adjust the pH of the solution to 6.2-6.8.

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