Preparation process of low-irritation acarus-killing antibacterial disinfection powder

Through enzymatic fermentation of Pistacia chinensis leaves and North American redwood leaves and purification of jellyfish colloids, combined with phosphate-PAMAM biofilm disruptor, a low-irritation mite-removing and antibacterial disinfectant powder is prepared, which solves the problem of high irritation of existing disinfectant powders and achieves efficient sterilization and mite removal effects.

CN120642860AActive Publication Date: 2025-09-16SENCON GUARD (SHANDONG) MEDICAL TECH CO LTD
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Patent Information

Application Number
CN202510781991.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-06-12
Publication Date
2025-09-16
Estimated Expiration
2045-06-12

AI Technical Summary

Technical Problem

Existing disinfectant powders are highly irritating due to the highly active compounds they contain, which may cause adverse reactions in the human body, especially after disinfecting fabrics, and their bactericidal effects are limited.

Method used

A low-irritation mite-removing and antibacterial disinfectant powder is prepared by enzymatic fermentation of Pistacia chinensis leaves and North American redwood leaves, enzymatic purification of jellyfish colloids, and compounding with phosphate-PAMAM biofilm disruptor. Collagen peptides are extracted by fermentation of Lactobacillus plantarum and Pediococcus pentosaceus, followed by pepsin treatment and dialysis technology, and the bactericidal effect is enhanced by combining phosphate-PAMAM biofilm disruptor.

Benefits of technology

The low-irritation mite-removing and antibacterial disinfectant powder prepared has excellent bactericidal effect, significantly reduces irritation to the skin, and has good mite removal ability, avoiding the adverse reactions of chemical disinfectant powders.

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Abstract

The invention belongs to the technical field of disinfection powder, and particularly relates to a preparation process of low-irritation acarus-killing antibacterial disinfection powder. Comprising the following steps: performing enzymolysis fermentation on pistacia chinensis bunge leaves and sequoia sempervirens leaves; carrying out enzymolysis and purification on colloid of jellyfish; preparing a phosphate-PAMAM mycoderm breaking agent; and compounding the antibacterial and disinfection powder. The preparation method comprises the following steps: performing enzymolysis on pistacia chinensis bunge leaves and sequoia sempervirens leaves by using beta-glucosidase, and then performing mixed fermentation of lactobacillus plantarum and pediococcus pentosaceus on an obtained pistacia chinensis bunge leaf-sequoia sempervirens leaf enzyme treatment substrate to prepare the pistacia chinensis bunge leaf-sequoia sempervirens leaf mite-killing antibacterial liquid. The acarus-killing antibacterial disinfection powder prepared by taking the pistacia chinensis leaf-sequoia sempervirens leaf acarus-killing antibacterial liquid as a main component has a good acarus-killing antibacterial effect, is extremely low in irritation to a human body, and can avoid injury caused by contact with skin after acarus-killing and sterilization are performed on close-fitting fabrics such as clothes, beds and quilts.
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Description

Technical Field

[0001] The invention belongs to the technical field of disinfectant powders, and in particular relates to a preparation process of a low-irritation mite-removing and antibacterial disinfectant powder. Background Art

[0002] Currently, commercially available disinfectant powders generally rely on highly active compounds such as hypochlorite, quaternary ammonium salts and peroxides as core bactericidal ingredients. Although their strong oxidizing and alkaline properties can effectively inactivate pathogenic microorganisms, they have significant application defects. Studies have shown that the free chlorine and volatile organic compounds released after conventional disinfectant powders are diluted can easily cause irritation of the human respiratory mucosa, damage to the skin barrier function, and even induce allergic contact dermatitis.

[0003] Especially in the fabric disinfection scenario, residual chemical active substances may migrate to the skin surface through clothing fibers, causing adverse reactions such as erythema and itching in infants and sensitive people. In order to solve the problem of high irritation of existing chemical disinfectant powders, it is urgent to develop a new type of disinfection system that has high efficiency in removing mites and antibacterial properties, low biological toxicity and excellent environmental compatibility. Summary of the Invention

[0004] In order to solve the above technical defects, the present invention has developed a preparation process for a low-irritation mite removal and antibacterial disinfectant powder. The prepared product is not only low in irritation, but also has good mite removal effect and excellent bactericidal ability.

[0005] A preparation process of a low-irritation mite-removing and antibacterial disinfectant powder comprises the following steps: S1: Enzymatic fermentation of Pistacia chinensis leaves and Sequoia chinensis leaves Pistacia chinensis leaves and redwood leaves are dried and crushed, then enzymatically hydrolyzed with β-glucosidase, and then fermented with Lactobacillus plantarum and Pediococcus pentosaceus after adding glucose, yeast extract, inulin, and salt. The supernatant is collected by centrifugation to obtain a Pistacia chinensis leaf-redwood leaf mite removal and antibacterial liquid. S2: Enzymatic purification of jellyfish colloids The jellyfish is treated with alkali and then enzymatically hydrolyzed with pepsin. The supernatant is centrifuged and added with NaCl for precipitation. The supernatant is then dissolved in an acetic acid aqueous solution and dialyzed against distilled water to obtain a jellyfish collagen peptide solution. S3: Preparation of phosphate-PAMAM biofilm disruptor and compounding of antibacterial disinfectant powder O-phospho-L-serine is dissolved in deionized water, and after adjusting the pH, 1-ethyl-(3-dimethylaminopropyl)carbodiimide and N-hydroxysuccinimide are added and mixed evenly. Then, fifth-generation dendritic polyamidoamine with amino groups and 4-dimethylaminopyridine are added, and the mixture is stirred, rotary evaporated, cleaned, and dried to obtain a phosphate-PAMAM biofilm disruptor. A Pistacia chinensis leaf-North American redwood leaf mite and antibacterial liquid, a whip-breasted jellyfish collagen peptide solution, and the phosphate-PAMAM biofilm disruptor are mixed, freeze-dried, and pulverized to obtain a low-irritation mite and antibacterial disinfectant powder.

[0006] Furthermore, step S1 of enzymatic fermentation of Pistacia chinensis leaves and Sequoia chinensis leaves comprises the following steps: S1.1: Pistacia chinensis leaves and redwood leaves in a mass ratio of 1:(1-1.5) are dried to a moisture content of 4-8%, and then pulverized through an 80-100 mesh sieve to obtain a mixed leaf powder. The mixed leaf powder is added to distilled water at a temperature of 45-50°C at a material-liquid ratio of 1:(12-15) g / mL, and the pH is adjusted to 5-5.5. 0.3-0.5 wt% of β-glucosidase is then added, and the mixture is shaken at 45-50°C and 150-180 rpm for 8-10 hours to obtain a Pistacia chinensis leaf-redwood leaf enzyme-treated substrate. S1.2: 1-1.2 parts by weight of a Pistacia chinensis leaf-Northern redwood leaf enzyme-treated substrate, 0.1-0.2 parts by weight of glucose, 0.1-0.2 parts by weight of yeast extract, 0.06-0.08 parts by weight of inulin and 0.02-0.03 parts by weight of salt are adjusted to a pH of 7-7.5, and sterilized at 121°C for 15-20 minutes to obtain a fermentation substrate. After activation culture of Lactobacillus plantarum and Pediococcus pentosaceus, they are inoculated into the fermentation substrate at a total inoculum amount of 4-5%, and fermented with shaking at 28-30°C and 150-180 rpm for 55-60 hours. The mixture is then heated to 80-85°C and sterilized for 20-25 minutes. The mixture is placed in a centrifuge and centrifuged at a speed of 10,000-12,000 rpm for 3-4 minutes. The supernatant is collected to obtain a Pistacia chinensis leaf-Northern redwood leaf mite removal and antibacterial liquid.

[0007] Furthermore, step S2 of enzymatic purification of jellyfish colloids comprises the following steps: S2.1: Clean fresh jellyfish, trim the edges of the umbrella, and then cut into small pieces to obtain jellyfish colloids. Add the jellyfish colloids to 3-5 times the volume of a 0.4-0.5 mol / L sodium hydroxide solution. Then, homogenize the jellyfish colloids in a homogenizer at 8000-11000 rpm for 10-15 seconds. Repeat the homogenization process 4-5 times under the same conditions, let it stand at 3-4°C for 20-24 hours, and then centrifuge at 3-4°C and 10000-12000 rpm for 10-12 minutes. Wash the precipitate with water until it is neutral, and filter it to obtain the pretreated jellyfish colloids. S2.2: The pretreated jellyfish colloid and acetic acid aqueous solution are mixed evenly at a material-liquid ratio of 1: (6-8) g / mL, and then 4-5wt% pepsin of the pretreated jellyfish colloid is added. The mixture is shaken at 3-4°C and 120-140rpm for 45-48 hours, and then centrifuged for 10-12 minutes while maintaining the temperature at 10000-12000rpm. NaCl is added to the supernatant until the NaCl concentration is 2-2.5mol / L. The mixture is kept warm and allowed to stand for 24-30 hours. The precipitate is filtered and dissolved in 3-4 times the mass of acetic acid aqueous solution, and then placed in a dialysis bag and dialyzed with distilled water for 42-48 hours. The solution in the dialysis bag is collected to obtain the whip-arm jellyfish collagen peptide solution.

[0008] Furthermore, step S3 of preparing the phosphate-PAMAM biofilm disruptor and compounding the antibacterial disinfectant powder comprises the following steps: S3.1: Dissolve 3-5 parts by weight of O-phospho-L-serine in 30-40 parts by weight of deionized water in a water bath at 45-50°C, add 1 mol / L HCl dropwise to adjust the pH to 5.5-6, then add 0.6-0.8 parts by weight of 1-ethyl-(3-dimethylaminopropyl)carbodiimide and 0.4-0.5 parts by weight of N-hydroxysuccinimide, and stir at 25-30°C and 250-300 rpm for 30-40 minutes to obtain a phosphation active solution; S3.2: Add 5-7 parts by weight of the fifth-generation dendritic polyamidoamine with amino groups to the phosphated active solution prepared in step S3.1, and then add 0.1-0.15 parts by weight of 4-dimethylaminopyridine. Stir at room temperature for 20-24 hours at a stirring speed of 200-250 rpm under a nitrogen atmosphere. Then, rotary evaporate at 0.08-0.1 MPa and 60-65°C for 2-3 hours. Then, rinse with deionized water and dry to obtain the phosphate-PAMAM biofilm disruptor. S3.3: Mix the Pistacia chinensis leaf-North American redwood leaf mite removal and antibacterial liquid and the whip-arm jellyfish collagen peptide solution in a mass ratio of 1: (0.3-0.5), then add 4-6wt% of phosphate-PAMAM biofilm disruptor, 0.8-1wt% of cetylpyridinium chloride and 2-3wt% of trehalose and stir evenly, freeze-dry at -50℃ to -40℃, crush and pass through an 80-100 mesh sieve to obtain a low-irritation mite removal and antibacterial disinfectant powder.

[0009] Furthermore, the mass ratio of Lactobacillus plantarum to Pediococcus pentosaceus in the total inoculation amount in step S1.2 is 2:1.

[0010] Furthermore, the concentration of the acetic acid aqueous solution in step S2.2 is 0.5-0.55 mol / L.

[0011] Furthermore, during the dialysis process of step S2.2, distilled water is replaced every 10-12 hours.

[0012] The beneficial effects are as follows: 1. The present invention first uses β-glucosidase to enzymolyze the Pistacia chinensis leaves and the North American redwood leaves, and then carries out mixed fermentation of Lactobacillus plantarum and Pediococcus pentosaceus on the obtained Pistacia chinensis leaf-North American redwood leaf enzyme-treated substrate to prepare the Pistacia chinensis leaf-North American redwood leaf mite removal and antibacterial liquid. The mite removal and antibacterial disinfectant powder prepared with the Pistacia chinensis leaf-North American redwood leaf mite removal and antibacterial liquid as the main component has good mite removal and antibacterial effect, and is extremely low in irritation to the human body, and can avoid damage to the skin caused by contact with close-fitting fabrics such as clothes and bedding after mite removal and sterilization.

[0013] 2. The present invention extracts collagen peptides from the jellyfish colloid by enzymatic hydrolysis. The collagen peptides have a high content of glycine, as well as amino acids such as histidine, tyrosine, lysine and methionine, which can improve the SOD activity of bacterial cells and reduce the malondialdehyde content. The prepared mite-removing and antibacterial disinfectant powder can improve the activity of bacteria and enhance the rate of bacterial metabolism when it comes into contact with bacteria, thereby enabling the subsequent phosphate-PAMAM biofilm disruptor to more easily bind to the bacterial biofilm and destroy the structure of the biofilm, thereby allowing the effective ingredients of the Pistacia chinensis leaf-North American redwood leaf mite-removing and antibacterial liquid to better penetrate into the bacteria for sterilization, thereby improving the sterilization effect.

[0014] 3. The present invention prepares a phosphate-PAMAM biofilm disruptor. Since phosphate is the main component of bacterial cell membranes, it can enhance the affinity of PAMAM dendrimers to cell membranes, thereby better penetrating and destroying the cell membranes. Combined with the active ingredients of the Pistacia chinensis leaf-North American redwood leaf mite removal and antibacterial liquid, it can better kill bacteria and improve the bactericidal effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1This is a flow chart of the preparation process of the low-irritation mite-removing and antibacterial disinfectant powder used in the embodiments of the present invention. DETAILED DESCRIPTION

[0016] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0017] Example 1 A preparation process of a low-irritation mite-removing and antibacterial disinfectant powder, such as Figure 1 As shown, the following steps are included: S1: Enzymatic fermentation of Pistacia chinensis leaves and Sequoia chinensis leaves S1.1: Pistacia chinensis leaves and redwood leaves in a 1:1 mass ratio were dried to a moisture content of 4%, then pulverized through an 80-mesh sieve to obtain a mixed leaf powder. The mixed leaf powder was added to distilled water at 45°C at a material-liquid ratio of 1:12 g / mL. The pH was adjusted to 5, and 0.3 wt% β-glucosidase was added. The mixture was shaken at 45°C and 150 rpm for 8 hours to obtain a Pistacia chinensis leaf-redwood leaf enzyme-treated substrate. S1.2: 1 part by weight of Pistacia chinensis leaf-North American redwood leaf enzyme-treated substrate, 0.1 part by weight of glucose, 0.1 part by weight of yeast extract, 0.06 part by weight of inulin and 0.02 part by weight of salt were adjusted to pH 7, and sterilized at 121°C for 15 minutes to obtain a fermentation substrate. After activation culture, Lactobacillus plantarum and Pediococcus pentosaceus were inoculated into the fermentation substrate at a total inoculum amount of 4%, with a mass ratio of Lactobacillus plantarum to Pediococcus pentosaceus of 2:1. The mixture was shaken and fermented at 28°C and 150rpm for 55 hours, then heated to 80°C and sterilized for 20 minutes. The mixture was placed in a centrifuge and centrifuged at 10,000rpm for 3 minutes. The supernatant was collected to obtain Pistacia chinensis leaf-North American redwood leaf mite removal and antibacterial liquid.

[0018] S2: Enzymatic purification of jellyfish colloids S2.1: Clean fresh jellyfish, trim the edges of the umbrella, and then cut into small pieces to obtain jellyfish colloids. Add the jellyfish colloids to 3 times the volume of 0.4 mol / L sodium hydroxide solution. Then, homogenize them in a homogenizer at 8000 rpm for 10 seconds. Repeat the homogenization four times under the same conditions, let it stand at 3°C ​​for 20 hours, and then centrifuge it at 3°C ​​and 10000 rpm for 10 minutes. Wash the precipitate with water until it is neutral, and filter it to obtain the pretreated jellyfish colloids. S2.2: The pretreated jellyfish colloid and an acetic acid aqueous solution with a concentration of 0.5 mol / L were mixed evenly at a solid-liquid ratio of 1:6 g / mL, and then 4 wt% pepsin of the pretreated jellyfish colloid was added, and the mixture was shaken at 3°C ​​and 120 rpm for 45 hours, and then centrifuged at a speed of 10000 rpm for 10 minutes, and the supernatant was added with NaCl until the NaCl concentration reached 2 mol / L. The mixture was kept warm and allowed to stand for 24 hours. The precipitate was filtered and dissolved in an acetic acid aqueous solution with a concentration of 3 times the mass of 0.5 mol / L, and then placed in a dialysis bag and dialyzed with distilled water for 42 hours. The distilled water was replaced every 10 hours. The solution in the dialysis bag was collected to obtain a whip-arm jellyfish collagen peptide solution.

[0019] S3: Preparation of phosphate-PAMAM biofilm disruptor and compounding of antibacterial disinfectant powder S3.1: Dissolve 3 parts by weight of O-phospho-L-serine in 30 parts by weight of deionized water in a 45°C water bath. Add 1 mol / L HCl dropwise to adjust the pH to 5.5. Then, add 0.6 parts by weight of 1-ethyl-(3-dimethylaminopropyl)carbodiimide and 0.4 parts by weight of N-hydroxysuccinimide. Stir at 25°C and 250 rpm for 30 minutes to obtain a phospho-active solution. S3.2: Add 5 parts by weight of the fifth-generation dendritic polyamidoamine with amino groups to the phosphated active solution prepared in step S3.1, followed by 0.1 parts by weight of 4-dimethylaminopyridine. Stir at room temperature for 20 hours at a stirring speed of 200 rpm under a nitrogen atmosphere. Rotary evaporate the mixture at 0.08 MPa and 60°C for 2 hours. Rinse with deionized water and dry to obtain the phosphate-PAMAM biofilm disruptor. S3.3: Mix the Pistacia chinensis leaf-North American redwood leaf mite removal and antibacterial liquid and the whip-arm jellyfish collagen peptide solution in a mass ratio of 1:0.3, then add 4wt% of phosphate-PAMAM biofilm disruptor, 0.8wt% of cetylpyridinium chloride and 2wt% of trehalose and stir evenly, freeze-dry at -50℃, crush and pass through an 80-mesh sieve to obtain a low-irritation mite removal and antibacterial disinfectant powder.

[0020] Example 2 A preparation process of a low-irritation mite-removing and antibacterial disinfectant powder, such as Figure 1 As shown, the following steps are included: S1: Enzymatic fermentation of Pistacia chinensis leaves and Sequoia chinensis leaves S1.1: Pistacia chinensis leaves and redwood leaves in a mass ratio of 1:1.5 were dried to a moisture content of 4%, then pulverized through an 80-mesh sieve to obtain a mixed leaf powder. The mixed leaf powder was added to distilled water at 45°C at a material-liquid ratio of 1:12 g / mL. The pH was adjusted to 5, and 0.5 wt% β-glucosidase was added. The mixture was shaken at 45°C and 150 rpm for 8 hours to obtain a Pistacia chinensis leaf-redwood leaf enzyme-treated substrate. S1.2: 1.2 parts by weight of Pistacia chinensis leaf-North American redwood leaf enzyme-treated substrate, 0.2 parts by weight of glucose, 0.2 parts by weight of yeast extract, 0.08 parts by weight of inulin and 0.03 parts by weight of salt were adjusted to pH 7, and sterilized at 121°C for 15 minutes to obtain a fermentation substrate. Lactobacillus plantarum and Pediococcus pentosaceus were activated and cultured, and then inoculated into the fermentation substrate at a total inoculum amount of 5%, with a mass ratio of Lactobacillus plantarum to Pediococcus pentosaceus of 2:1. The mixture was shaken and fermented at 28°C and 150rpm for 55 hours, then heated to 80°C and sterilized for 20 minutes. The mixture was placed in a centrifuge and centrifuged at 10,000rpm for 3 minutes. The supernatant was collected to obtain Pistacia chinensis leaf-North American redwood leaf mite removal and antibacterial liquid.

[0021] S2: Enzymatic purification of jellyfish colloids S2.1: Clean fresh jellyfish, trim the edges of the umbrella, and then cut into small pieces to obtain jellyfish colloids. Add the jellyfish colloids to 5 times the volume of 0.4 mol / L sodium hydroxide solution. Then, homogenize them in a homogenizer at 8000 rpm for 10 seconds. Repeat the homogenization four times under the same conditions, let it stand at 3°C ​​for 20 hours, and then centrifuge it at 3°C ​​and 10000 rpm for 10 minutes. Wash the precipitate with water until it is neutral, and filter it to obtain the pretreated jellyfish colloids. S2.2: The pretreated jellyfish colloid and an acetic acid aqueous solution with a concentration of 0.5 mol / L were mixed evenly at a solid-liquid ratio of 1:6 g / mL, and then 5 wt% pepsin of the pretreated jellyfish colloid was added, and the mixture was shaken at 3°C ​​and 120 rpm for 45 hours, and then centrifuged at a speed of 10000 rpm for 10 minutes, and the supernatant was added with NaCl until the NaCl concentration reached 2 mol / L. The mixture was kept warm and allowed to stand for 24 hours. The precipitate was filtered and dissolved in an acetic acid aqueous solution with a concentration of 4 times the mass of 0.5 mol / L, and then placed in a dialysis bag and dialyzed with distilled water for 42 hours. The distilled water was replaced every 10 hours. The solution in the dialysis bag was collected to obtain a whip-arm jellyfish collagen peptide solution.

[0022] S3: Preparation of phosphate-PAMAM biofilm disruptor and compounding of antibacterial disinfectant powder S3.1: Dissolve 5 parts by weight of O-phospho-L-serine in 40 parts by weight of deionized water in a 45°C water bath. Add 1 mol / L HCl dropwise to adjust the pH to 5.5. Then, add 0.8 parts by weight of 1-ethyl-(3-dimethylaminopropyl)carbodiimide and 0.5 parts by weight of N-hydroxysuccinimide. Stir at 25°C and 250 rpm for 30 minutes to obtain a phospho-active solution. S3.2: Add 7 parts by weight of the fifth-generation dendritic polyamidoamine to the phosphated active solution prepared in step S3.1, followed by 0.15 parts by weight of 4-dimethylaminopyridine. Stir at room temperature for 20 hours at 200 rpm under a nitrogen atmosphere. Rotary evaporate the mixture at 0.08 MPa and 60°C for 2 hours. Rinse with deionized water and dry to obtain the phosphate-PAMAM biofilm disruptor. S3.3: Mix the Pistacia chinensis leaf-North American redwood leaf mite removal and antibacterial liquid and the whip-arm jellyfish collagen peptide solution in a mass ratio of 1:0.5, then add 6wt% of phosphate-PAMAM biofilm disruptor, 1wt% of cetylpyridinium chloride and 3wt% of trehalose and stir evenly, freeze-dry at -50℃, crush and pass through an 80-mesh sieve to obtain a low-irritation mite removal and antibacterial disinfectant powder.

[0023] Example 3 A preparation process of a low-irritation mite-removing and antibacterial disinfectant powder, such as Figure 1 As shown, the following steps are included: S1: Enzymatic fermentation of Pistacia chinensis leaves and Sequoia chinensis leaves S1.1: Pistacia chinensis leaves and redwood leaves in a 1:1 mass ratio were dried to a moisture content of 8%, then pulverized through a 100-mesh sieve to obtain a mixed leaf powder. The mixed leaf powder was added to distilled water at 50°C at a material-liquid ratio of 1:15 g / mL. The pH was adjusted to 5.5, and 0.3 wt% β-glucosidase was added. The mixture was shaken at 50°C and 180 rpm for 10 hours to obtain a Pistacia chinensis leaf-redwood leaf enzyme-treated substrate. S1.2: 1 part by weight of a Pistacia chinensis leaf-North American redwood leaf enzyme-treated substrate, 0.1 part by weight of glucose, 0.1 part by weight of yeast extract, 0.06 part by weight of inulin and 0.02 part by weight of salt were adjusted to pH 7.5, and sterilized at 121°C for 20 minutes to obtain a fermentation substrate. After activation culture of Lactobacillus plantarum and Pediococcus pentosaceus, they were inoculated into the fermentation substrate at a total inoculum amount of 4%, with a mass ratio of Lactobacillus plantarum to Pediococcus pentosaceus of 2:1. The mixture was shaken and fermented at 30°C and 180 rpm for 60 hours, then heated to 85°C and sterilized for 25 minutes. The mixture was placed in a centrifuge and centrifuged at 12,000 rpm for 4 minutes. The supernatant was collected to obtain a Pistacia chinensis leaf-North American redwood leaf mite removal and antibacterial liquid.

[0024] S2: Enzymatic purification of jellyfish colloids S2.1: Clean fresh jellyfish, trim the edges of the umbrella, and then cut into small pieces to obtain jellyfish colloids. Add the jellyfish colloids to 3 times the volume of 0.5 mol / L sodium hydroxide solution. Then, homogenize them in a homogenizer at 11,000 rpm for 15 seconds. Repeat the homogenization process five times under the same conditions, let them stand at 4°C for 24 hours, and then centrifuge them at 4°C and 12,000 rpm for 12 minutes. Wash the precipitate with water until it is neutral, and filter it to obtain the pretreated jellyfish colloids. S2.2: The pretreated jellyfish colloid and an acetic acid aqueous solution with a concentration of 0.55 mol / L were mixed evenly at a solid-liquid ratio of 1:8 g / mL, and then 5 wt% pepsin of the pretreated jellyfish colloid was added. The mixture was shaken at 4°C and 140 rpm for 48 hours, and then centrifuged at 12000 rpm for 12 minutes. The supernatant was added with NaCl until the NaCl concentration reached 2.5 mol / L. The mixture was kept warm and allowed to stand for 30 hours. The precipitate was filtered and dissolved in an acetic acid aqueous solution with a concentration of 3 times the mass of 0.55 mol / L. The precipitate was then placed in a dialysis bag and dialyzed with distilled water for 48 hours. The distilled water was replaced every 12 hours. The solution in the dialysis bag was collected to obtain a whip-arm jellyfish collagen peptide solution.

[0025] S3: Preparation of phosphate-PAMAM biofilm disruptor and compounding of antibacterial disinfectant powder S3.1: Dissolve 3 parts by weight of O-phospho-L-serine in 30 parts by weight of deionized water in a 50°C water bath. Add 1 mol / L HCl dropwise to adjust the pH to 6. Then, add 0.6 parts by weight of 1-ethyl-(3-dimethylaminopropyl)carbodiimide and 0.4 parts by weight of N-hydroxysuccinimide. Stir at 30°C and 300 rpm for 40 minutes to obtain a phospho-active solution. S3.2: Add 5 parts by weight of a fifth-generation dendritic polyamidoamine with amino groups to the phosphated active solution prepared in step S3.1, followed by 0.1 parts by weight of 4-dimethylaminopyridine. Stir at room temperature for 24 hours at 250 rpm under a nitrogen atmosphere. Rotary evaporate the mixture at 0.1 MPa and 65°C for 3 hours. Rinse with deionized water and dry to obtain a phosphate-PAMAM biofilm disruptor. S3.3: Mix the Pistacia chinensis leaf-North American redwood leaf mite removal and antibacterial liquid and the whip-arm jellyfish collagen peptide solution in a mass ratio of 1:0.3, then add 4wt% of phosphate-PAMAM biofilm disruptor, 0.8wt% of cetylpyridinium chloride and 2wt% of trehalose and stir evenly, freeze-dry at -40°C, crush and pass through a 100-mesh sieve to obtain a low-irritation mite removal and antibacterial disinfectant powder.

[0026] The difference between Comparative Example 1 and Example 1 is that, in Comparative Example 1, the Pistacia chinensis leaves in step S1.1 are replaced with equal mass of North American redwood leaves to prepare North American redwood leaf mite removal and antibacterial liquid, and the subsequent Pistacia chinensis leaf-North American redwood leaf mite removal and antibacterial liquid is replaced with North American redwood leaf mite removal and antibacterial liquid. The remaining specific implementation methods are the same as Example 1.

[0027] The difference between Comparative Example 2 and Example 1 is that Comparative Example 2 replaces the North American redwood leaves in step S1.1 with equal mass of Pistacia leaves to prepare Pistacia leaf mite removal and antibacterial liquid, and replaces the subsequent Pistacia leaf-North American redwood leaf mite removal and antibacterial liquid with Pistacia leaf mite removal and antibacterial liquid. The remaining specific implementation methods are the same as Example 1.

[0028] Comparative Example 3 is different from Example 1 in that step S2 is removed in Comparative Example 3, and the jellyfish collagen peptide solution in step S3.3 is replaced with distilled water of equal mass. The rest of the specific implementations are the same as those in Example 1.

[0029] Comparative Example 4 differs from Example 1 in that step S3.1 and step S3.2 are omitted, and the phosphate-PAMAM biofilm disruptor is not added in step S3.3. The remaining specific embodiments are the same as those in Example 1.

[0030] The low-irritation mite-removing and antibacterial disinfectant powder prepared in Examples 1-3 was selected and mixed with water to prepare a disinfectant with a concentration of 30% as a sample for acute oral toxicity test and multiple intact skin irritation tests.

[0031] Acute oral toxicity test: 20 healthy Kunming mice weighing (20±0.2) g, half male and half female, were selected and divided into 4 groups, 5 mice in each group, corresponding to the samples of Examples 1-3 and a blank group (no gavage). The night before gavage, the mice were fasted but not watered. The dose of the test sample was 5000 mg / kg body weight. After gavage, they ate and drank normally. The clinical manifestations of the experimental animals were observed and the number of deaths was recorded. The observation was continued for 14 consecutive days. After the end of the test, the weight was weighed and the average value was calculated. The mice were sacrificed and pathological observation was performed. The test results are shown in Table 1.

[0032] Table 1: Results of acute oral toxicity test on mice of the samples of the examples

[0033] Multiple intact skin irritation test: Fifteen New Zealand rabbits with healthy skin were selected and divided into three groups. 24 hours before the test, the hair on both sides of the back spine was trimmed, approximately 3 cm × 3 cm on each side, without damaging the epidermis. The next day, different samples were applied to the hairless skin on the right side of different groups, and physiological saline was applied to the hairless skin on the left side as a blank control. After 4 hours of application, the residue was washed off with warm water. The application was repeated once a day for 14 consecutive days. The skin irritation reaction was observed and scored 24 hours after each application. The results are shown in Table 2.

[0034] Table 2: Results of multiple intact skin irritation tests on samples from the examples

[0035] As shown in Table 1, the results of the acute oral toxicity test on mice showed no symptoms of poisoning or death in animals after 14 consecutive days of observation, which proves that the low-irritation mite-removing and antibacterial disinfectant powder prepared in the example is actually non-toxic. As shown in Table 2, the results of the multiple intact skin irritation test on the example samples showed no abnormalities in the test skin of the rabbits in the sample group compared with the skin on the control side after repeated contact stimulation for 14 consecutive days. According to the scoring standard, the mean score was 0, the multiple skin irritation index was 0, and the irritation intensity was non-irritating.

[0036] The low-irritation mite removal and antibacterial disinfectant powders prepared in Examples 1-3 and Comparative Examples 1-4 were selected and mixed with water to prepare disinfectants with a concentration of 5% as samples for mite removal and sterilization tests.

[0037] Mite removal test: 18 round pieces of cloth with a diameter of 10 cm were prepared, steamed at high temperature and dried, and then divided into 6 groups, with three pieces in each group, and placed in a culture dish. 0.1 g of mite feed was sprinkled on each piece of cloth, and then 100 live mites were put in. The cloth was folded to wrap the live mites. After 10 minutes, it was immersed in the samples prepared in Examples 1-3 and Comparative Examples 1-2 and in distilled water, with distilled water serving as a blank group, for 5 minutes. Then, the folded cloth was taken out and opened, immersed in distilled water and stirred at 200 rpm for 5 minutes. The number of mites on the cloth was recorded, recorded as N, and the mite removal rate% = (100-N) / 100×100%. The results are shown in Table 3.

[0038] Table 3: Mite removal rate of 5% concentration disinfectant

[0039] Bactericidal test: Escherichia coli, Staphylococcus aureus and Candida albicans were inoculated on the required nutrient agar medium plates, and a single typical colony was isolated and inoculated for bacterial enrichment culture. The colony was then eluted with TPS diluent to prepare a plate with a bacterial count of (1×10 8 ~5×10 8) cfu / mL bacterial suspension, take 4 mL of the samples prepared in Examples 1-3 and Comparative Examples 1-4 and distilled water, and mix them with 1 mL of the bacterial suspension respectively in a water bath at 20°C. After acting for 5 minutes, place them on a sterile filter membrane and filter them, then rinse and filter them with sterile hard water, then stick the filter membrane on an agar medium plate, place it at 37°C and culture it for 48 hours, count the number of colonies, and calculate the killing logarithm. The test was repeated three times, and the killing logarithm average was taken. The test results are shown in Table 4.

[0040] Table 4: Average killing logarithms of various bacteria by 5% concentration disinfectant

[0041] It can be seen from Table 3 that the mite removal rates of Examples 1-3 all reached more than 97%, which can prove that the low-irritation mite removal and antibacterial disinfectant powder prepared in the present application has a good mite removal effect, while the mite removal rate of Comparative Examples 1-2 was significantly reduced, proving that the leaves of Pistacia chinensis and the leaves of North American redwood have a synergistic effect in the mite removal effect.

[0042] It can be seen from Table 4 that the killing logarithmic values ​​of Examples 1-3 against Escherichia coli, Staphylococcus aureus and Candida albicans all meet the standard requirements of disinfectants (≥5 for Escherichia coli, ≥5 for Staphylococcus aureus, ≥4 for Candida albicans), which can prove that the present application has excellent bactericidal effects, while the killing logarithmic values ​​of Comparative Examples 1-4 are significantly reduced, proving that the leaves of Pistacia chinensis and the leaves of North American redwood also have a synergistic effect in the bactericidal effect, and the addition of whip-arm jellyfish collagen peptide and phosphate-PAMAM biofilm disruptor can enhance the bactericidal effect.

[0043] The above embodiments are merely illustrative of the principles and effects of the present invention and are not intended to limit the present invention. Any person skilled in the art may modify or alter the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or alterations made by persons skilled in the art without departing from the spirit and technical concepts disclosed herein are intended to be covered by the claims of the present invention.

Claims

1. A preparation process for a low-irritation mite-removing and antibacterial disinfectant powder, characterized in that: The following steps are involved: S1. Enzymatic hydrolysis and fermentation of Pistacia chinensis leaves and North American redwood leaves: Pistacia chinensis leaves and North American redwood leaves are dried and crushed, then mixed and hydrolyzed with β-glucosidase, and then fermented with Lactobacillus plantarum and Pediococcus pentosaceus after adding glucose, yeast extract, inulin, and salt. The supernatant is collected by centrifugation to obtain a Pistacia chinensis leaf-North American redwood leaf mite removal and antibacterial liquid; S2 Enzymatic purification of jellyfish colloids: The jellyfish is treated with alkali and then enzymatically hydrolyzed with pepsin. The supernatant is centrifuged and added with NaCl for precipitation. The supernatant is then dissolved in acetic acid aqueous solution and dialyzed against distilled water to obtain a jellyfish collagen peptide solution. Preparation of S3 phosphate-PAMAM biofilm disruptor and compounding of antibacterial disinfectant powder: O-phospho-L-serine was dissolved in deionized water, 1-ethyl-(3-dimethylaminopropyl)carbodiimide and N-hydroxysuccinimide were added and mixed evenly after adjusting the pH, and then the fifth-generation dendritic polyamide amine with amino group and 4-dimethylaminopyridine were added, stirred and rotary evaporated, and then cleaned and dried to obtain phosphate-PAMAM biofilm disruptor. The Pistacia chinensis leaf-North American redwood leaf mite removal and antibacterial liquid, whip-arm jellyfish collagen peptide solution and phosphate-PAMAM biofilm disruptor were mixed and freeze-dried, and crushed to obtain low-irritation mite removal and antibacterial disinfectant powder.

2. The preparation process of a low-irritation mite-removing and antibacterial disinfectant powder according to claim 1, characterized in that: Step S1: enzymatic fermentation of Pistacia chinensis leaves and Sequoia chinensis leaves, comprising the following steps: S1.1: Pistacia chinensis leaves and redwood leaves in a mass ratio of 1:(1-1.5) are dried to a moisture content of 4-8%, and then pulverized through an 80-100 mesh sieve to obtain a mixed leaf powder. The mixed leaf powder is added to distilled water at a temperature of 45-50°C at a material-liquid ratio of 1:(12-15) g / mL, and the pH is adjusted to 5-5.

5. 0.3-0.5 wt% of β-glucosidase is then added, and the mixture is shaken at 45-50°C and 150-180 rpm for 8-10 hours to obtain a Pistacia chinensis leaf-redwood leaf enzyme-treated substrate. S1.2: 1-1.2 parts by weight of a Pistacia chinensis leaf-Northern redwood leaf enzyme-treated substrate, 0.1-0.2 parts by weight of glucose, 0.1-0.2 parts by weight of yeast extract, 0.06-0.08 parts by weight of inulin and 0.02-0.03 parts by weight of salt are adjusted to a pH of 7-7.5, and sterilized at 121°C for 15-20 minutes to obtain a fermentation substrate. After activation culture of Lactobacillus plantarum and Pediococcus pentosaceus, they are inoculated into the fermentation substrate at a total inoculum amount of 4-5%, and fermented with shaking at 28-30°C and 150-180 rpm for 55-60 hours. The mixture is then heated to 80-85°C and sterilized for 20-25 minutes. The mixture is placed in a centrifuge and centrifuged at a speed of 10,000-12,000 rpm for 3-4 minutes. The supernatant is collected to obtain a Pistacia chinensis leaf-Northern redwood leaf mite removal and antibacterial liquid.

3. The preparation process of a low-irritation mite-removing and antibacterial disinfectant powder according to claim 2, characterized in that: Step S2, enzymatic purification of jellyfish colloids, comprises the following steps: S2.1: Clean fresh jellyfish, trim the edges of the umbrella, and then cut into small pieces to obtain jellyfish colloids. Add the jellyfish colloids to 3-5 times the volume of a 0.4-0.5 mol / L sodium hydroxide solution. Then, homogenize the jellyfish colloids in a homogenizer at 8000-11000 rpm for 10-15 seconds. Repeat the homogenization process 4-5 times under the same conditions, let it stand at 3-4°C for 20-24 hours, and then centrifuge at 3-4°C and 10000-12000 rpm for 10-12 minutes. Wash the precipitate with water until it is neutral, and filter it to obtain the pretreated jellyfish colloids. S2.2: The pretreated jellyfish colloid and the acetic acid aqueous solution are mixed evenly at a material-liquid ratio of 1: (6-8) g / mL, and then 4-5wt% pepsin of the pretreated jellyfish colloid is added. The mixture is shaken at 3-4°C and 120-140rpm for 45-48 hours, and then the temperature is maintained at 10000-12000rpm for centrifugation for 10-12 minutes. The supernatant is added with NaCl until the NaCl concentration is 2-2.5mol / L. The mixture is kept warm and allowed to stand for 24-30 hours. The precipitate is filtered and dissolved in 3-4 times the mass of the acetic acid aqueous solution. The precipitate is then placed in a dialysis bag and dialyzed with distilled water for 42-48 hours. The solution in the dialysis bag is collected to obtain the whip-arm jellyfish collagen peptide solution.

4. The preparation process of a low-irritation mite-removing and antibacterial disinfectant powder according to claim 3, characterized in that: Step S3, the preparation of the phosphate-PAMAM biofilm disruptor and the compounding of the antibacterial disinfectant powder, comprises the following steps: S3.1: Dissolve 3-5 parts by weight of O-phospho-L-serine in 30-40 parts by weight of deionized water in a water bath at 45-50°C, add 1 mol / L HCl dropwise to adjust the pH to 5.5-6, then add 0.6-0.8 parts by weight of 1-ethyl-(3-dimethylaminopropyl)carbodiimide and 0.4-0.5 parts by weight of N-hydroxysuccinimide, and stir at 25-30°C and 250-300 rpm for 30-40 minutes to obtain a phosphation active solution; S3.2: Add 5-7 parts by weight of the fifth-generation dendritic polyamidoamine with amino groups to the phosphated active solution prepared in step S3.1, and then add 0.1-0.15 parts by weight of 4-dimethylaminopyridine. Stir at room temperature for 20-24 hours at a stirring speed of 200-250 rpm under a nitrogen atmosphere. Then, rotary evaporate at 0.08-0.1 MPa and 60-65°C for 2-3 hours. Then, rinse with deionized water and dry to obtain the phosphate-PAMAM biofilm disruptor. S3.3: Mix the Pistacia chinensis leaf-North American redwood leaf mite removal and antibacterial liquid and the whip-arm jellyfish collagen peptide solution in a mass ratio of 1: (0.3-0.5), then add 4-6wt% of phosphate-PAMAM biofilm disruptor, 0.8-1wt% of cetylpyridinium chloride and 2-3wt% of trehalose and stir evenly, freeze-dry at -50℃ to -40℃, crush and pass through an 80-100 mesh sieve to obtain a low-irritation mite removal and antibacterial disinfectant powder.

5. The preparation process of a low-irritation mite-removing and antibacterial disinfectant powder according to claim 2, characterized in that: The mass ratio of Lactobacillus plantarum to Pediococcus pentosaceus in the total inoculum in step S1.2 is 2:

1.

6. The preparation process of a low-irritation mite-removing and antibacterial disinfectant powder according to claim 3, characterized in that: The concentration of the acetic acid aqueous solution in step S2.2 is 0.5-0.55 mol / L.

7. The preparation process of a low-irritation mite-removing and antibacterial disinfectant powder according to claim 3, characterized in that: During the dialysis process in step S2.2, distilled water was replaced every 10-12 hours.

Citation Information

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