Preparation process of low-irritation anti-mite antibacterial disinfectant powder

Abstract

The present application belongs to the technical field of disinfecting powder, and particularly relates to a preparation process of low-irritation anti-mite and antibacterial disinfecting powder. The process comprises the following steps: enzymatic hydrolysis and fermentation of callerya nitida leaf and sequoia sempervirens leaf; enzymatic hydrolysis and purification of helix pompejana gum; preparation of phosphate-PAMAM bacterial membrane disruptor; and compounding of antibacterial disinfecting powder. The callerya nitida leaf and sequoia sempervirens leaf are subjected to enzymatic hydrolysis by using beta-glucosidase, and then the obtained callerya nitida leaf-sequoia sempervirens leaf enzyme-treated substrate is subjected to mixed fermentation of lactobacillus plantarum and pediococcus pentosaceus to obtain callerya nitida leaf-sequoia sempervirens leaf anti-mite and antibacterial liquid. The anti-mite and antibacterial disinfecting powder prepared by using the callerya nitida leaf-sequoia sempervirens leaf anti-mite and antibacterial liquid as the main component has good anti-mite and antibacterial effect, and has extremely low irritation to human body, so that harm caused by contact with skin after anti-mite and sterilization of close-fitting fabrics such as clothes and bedclothes can be avoided.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of disinfecting powder, and particularly relates to a preparation process of low-irritation anti-mite and antibacterial disinfecting powder. BACKGROUND

[0002] The current market disinfecting powder generally relies on hypochlorite, quaternary ammonium salt and peroxide as the core bactericidal component, and the strong oxidizing property and alkaline property can inactivate pathogenic microorganisms efficiently, but there are significant application defects, research shows that the free chlorine and volatile organic compounds released after dilution of the conventional disinfecting powder can easily cause respiratory mucosa irritation, skin barrier function damage and even induce allergic contact dermatitis.

[0003] Especially in the fabric disinfection scene, the residual chemical active substances can migrate to the skin surface through the clothes fibers, causing erythema, itching and other adverse reactions in infants and sensitive groups, in order to solve the problem of high irritation of the existing chemical disinfecting powder, it is urgent to develop a new disinfecting system with high efficient anti-mite and antibacterial performance, low biological toxicity and excellent environmental compatibility. SUMMARY

[0004] In order to solve the above technical defects, the application researches a preparation process of low-irritation anti-mite and antibacterial disinfecting powder, and the prepared product has low irritation, good anti-mite effect and excellent bactericidal capacity.

[0005] A preparation process of low-irritation anti-mite and antibacterial disinfecting powder, comprising the following steps:

[0006] S1: Enzymatic fermentation of yellow poplar leaves and north American red cedar leaves

[0007] Yellow poplar leaves and north American red cedar leaves are taken for drying and crushing, then mixed enzymolysis is carried out by beta-glucosidase, and after adding glucose, yeast extract, inulin and salt, mixed fermentation is carried out by using lactobacillus plantarum and pediococcus pentosaceus, the supernatant is taken by centrifugation, and yellow poplar leaf-north American red cedar leaf anti-mite and antibacterial liquid is obtained;

[0008] S2: Enzymatic purification of chrysozooid colloidal substance

[0009] The chrysozooid is treated and then subjected to alkaline treatment, and then subjected to enzymatic hydrolysis by pepsin, the supernatant is taken by centrifugation, NaCl is added for precipitation, and then the chrysozooid collagen peptide solution is obtained by dissolving in acetic acid aqueous solution and dialysis with distilled water;

[0010] S3: Preparation of phosphate ester-PAMAM bacterial membrane disruptant and compounding of antibacterial disinfecting powder

[0011] O-phospho-L-serine is dissolved in deionized water, after adjusting pH, 1-ethyl-(3-dimethylaminopropyl) carbonyl diimide and N-hydroxysuccinimide are added and mixed uniformly, then fifth generation dendrimer polyamide amine interface amino and 4-dimethylamino pyridine are added, after stirring and rotary evaporation, clean and dry to obtain phosphate-PAMAM bacterial membrane disruptant, mix the mesquite leaf-northern red cedar leaf mite-killing antibacterial solution, jellyfish collagen peptide solution and phosphate-PAMAM bacterial membrane disruptant, and freeze-dry to obtain low-irritation mite-killing antibacterial disinfectant powder.

[0012] Further, the step S1 mesquite leaf-northern red cedar leaf enzymatic fermentation includes the following steps:

[0013] S1.1: Take the mesquite leaf and northern red cedar leaf with a mass ratio of 1: (1-1.5), dry to a moisture content of 4-8%, then crush to pass through an 80-100 mesh sieve to obtain mixed leaf powder, add the mixed leaf powder to distilled water at a temperature of 45-50℃ at a solid-liquid ratio of 1: (12-15) g / mL, adjust the pH to 5-5.5, then add 0.3-0.5wt% of β-glucosidase, and oscillate at 45-50℃, 150-180rpm for 8-10 hours to obtain mesquite leaf-northern red cedar leaf enzyme-treated substrate;

[0014] S1.2: Adjust the pH of 1-1.2 parts by weight of mesquite leaf-northern red cedar 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 to 7-7.5, sterilize at 121℃ for 15-20 minutes to obtain a fermentation substrate, activate the culture of Lactobacillus plantarum and Pediococcus pentosaceus, inoculate into the fermentation substrate at a total inoculation amount of 4-5%, oscillate at 28-30℃, 150-180rpm for 55-60 hours, then sterilize at 80-85℃ for 20-25 minutes, centrifuge at 10000-12000rpm for 3-4 minutes, collect the supernatant, and obtain mesquite leaf-northern red cedar leaf mite-killing antibacterial solution.

[0015] Further, the step S2 jellyfish collagenase enzymatic purification includes the following steps:

[0016] S2.1: Fresh and live Physaliae tentaculum is washed clean, and after cutting off the edge of the umbrella part, it is cut into small pieces to obtain the Physaliae gelatin, which is added into 3-5 times volume of 0.4-0.5 mol / L sodium hydroxide solution, and then is homogenized in a homogenizer at a speed of 8000-11000 rpm for 10-15 seconds. After repeating the homogenization 4-5 times under the same conditions, it is placed at 3-4℃ for 20-24 hours, and then is centrifuged at 3-4℃ and a speed of 10000-12000 rpm for 10-12 minutes. The precipitate is washed to neutral, and then is filtered to obtain the pretreated Physaliae gelatin;

[0017] S2.2: The pretreated Physaliae gelatin and acetic acid aqueous solution are mixed uniformly at a solid-liquid ratio of 1: (6-8) g / mL, and then 4-5 wt% of pepsin is added to the pretreated Physaliae gelatin. The mixture is oscillated at 3-4℃ and a speed of 120-140 rpm for 45-48 hours, and then is centrifuged at a speed of 10000-12000 rpm for 10-12 minutes. The supernatant is collected, and NaCl is added until the concentration of NaCl is 2-2.5 mol / L. The mixture is continuously incubated and placed for 24-30 hours, and then is filtered. The precipitate is dissolved in 3-4 times mass of acetic acid aqueous solution, and then is loaded into a dialysis bag for dialysis against distilled water for 42-48 hours. The solution in the dialysis bag is collected to obtain a Physaliae collagen peptide solution.

[0018] Further, the preparation of the phosphate-PAMAM bacterial membrane disruptant and the compounding of the antibacterial disinfectant powder in step S3 include the following steps:

[0019] S3.1: 3-5 parts by weight of O-phospho-L-serine is dissolved in 30-40 parts by weight of deionized water under the condition of a water bath at 45-50℃, and 1 mol / L HCl is added dropwise to adjust the pH to 5.5-6. Then, 0.6-0.8 parts by weight of 1-ethyl-(3-dimethylaminopropyl) carbodiimide and 0.4-0.5 parts by weight of N-hydroxysuccinimide are added. The mixture is stirred at 25-30℃ and a speed of 250-300 rpm for 30-40 minutes to obtain a phosphate esterification active solution;

[0020] S3.2: 5-7 parts by weight of a fifth-generation dendritic polyamidoamine is added to the phosphate esterification active solution prepared in step S3.1, and 0.1-0.15 parts by weight of 4-dimethylaminopyridine is further added. The mixture is stirred at room temperature for 20-24 hours under a nitrogen atmosphere at a speed of 200-250 rpm. Then, the mixture is rotary evaporated at 0.08-0.1 MPa and 60-65℃ for 2-3 hours, and then is washed clean with deionized water and dried to obtain a phosphate-PAMAM bacterial membrane disruptant.

[0021] S3.3: The yellow poplar leaf-northern red cedar leaf mite-killing antibacterial liquid and the jellyfish collagen peptide solution are mixed uniformly at a mass ratio of 1: (0.3-0.5), then 4-6 wt% of the phosphate-PAMAM bacterial membrane disruptor, 0.8-1 wt% of cetylpyridinium chloride and 2-3 wt% of trehalose are added and stirred uniformly, and then the mixture is freeze-dried at-50℃ to-40℃, crushed and sieved through an 80-100 mesh sieve to obtain the low-irritation mite-killing antibacterial disinfectant powder.

[0022] Further, the mass ratio of Lactobacillus plantarum and Pediococcus pentosaceus in the total inoculum in step S1.2 is 2:1.

[0023] Further, the concentration of the aqueous acetic acid solution in step S2.2 is 0.5-0.55 mol / L.

[0024] Further, during the dialysis process of step S2.2, the distilled water is replaced every 10-12 hours.

[0025] Beneficial effects are: 1. The present application first uses beta-glucosidase to enzymatically hydrolyze the yellow poplar leaves and the northern red cedar leaves, and then carries out mixed fermentation of Lactobacillus plantarum and Pediococcus pentosaceus on the obtained yellow poplar leaf-northern red cedar leaf enzyme-treated substrate to prepare the yellow poplar leaf-northern red cedar leaf mite-killing antibacterial liquid. The mite-killing antibacterial disinfectant powder prepared by taking the yellow poplar leaf-northern red cedar leaf mite-killing antibacterial liquid as the main component has good mite-killing antibacterial effect and extremely low irritation to the human body, and can avoid damage to the skin after killing mites and bacteria on clothes, bedclothes and other close-fitting fabrics.

[0026] 2. The present application extracts collagen peptides from the jellyfish collagen by the enzymatic hydrolysis method. The collagen peptides have high content of glycine, as well as histidine, tyrosine, lysine and methionine, etc. amino acids, which can improve the SOD activity of bacterial cells and reduce the content of malondialdehyde. When the prepared mite-killing antibacterial disinfectant powder contacts bacteria, it can improve the activity of the bacteria and strengthen the speed of bacterial metabolism, so that the subsequent phosphate-PAMAM bacterial membrane disruptor can more easily combine with the bacterial membrane and destroy the structure of the bacterial membrane, so that the effective components of the yellow poplar leaf-northern red cedar leaf mite-killing antibacterial liquid can better penetrate into the bacteria to kill bacteria and improve the bactericidal effect.

[0027] 3. The present application prepares the phosphate-PAMAM bacterial membrane disruptor. Since phosphate is the main component of the cell membrane of bacteria, it can enhance the affinity of PAMAM dendrimers with the cell membrane, so as to better penetrate and destroy the cell membrane, and cooperate with the effective components of the yellow poplar leaf-northern red cedar leaf mite-killing antibacterial liquid to better kill bacteria and improve the bactericidal effect. BRIEF DESCRIPTION OF DRAWINGS

[0028] Figure 1The preparation process flow chart of the low-irritation acarid-removing antibacterial disinfectant powder used in the embodiments of the present application is shown in the following. DETAILED DESCRIPTION

[0029] The technical solutions in the embodiments of the present application will be clearly and completely described in combination with the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all the other embodiments obtained by those skilled in the art without creative labor fall within the protection scope of the present application.

[0030] Embodiment 1: The preparation process of a low-irritation acarid-removing antibacterial disinfectant powder is shown in the following, which comprises the following steps: Figure 1

[0031] S1: Enzymolysis fermentation of pistacia chinensis leaves and sequoia sempervirens leaves

[0032] S1.1: Take the pistacia chinensis leaves and sequoia sempervirens leaves with a mass ratio of 1:1, dry them to a water content of 4%, then crush them through an 80-mesh sieve, obtain mixed leaf powder, add the mixed leaf powder into distilled water with a temperature of 45℃ at a solid-liquid ratio of 1:12 g / mL, adjust the pH to 5, then add 0.3wt% of β-glucosidase, oscillate at 45℃ and 150rpm for 8 hours, and obtain the pistacia chinensis leaf-sequoia sempervirens leaf enzyme-treated substrate;

[0033] S1.2: Take 1 part by weight of the pistacia chinensis leaf-sequoia sempervirens 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, adjust the pH to 7, sterilize at 121℃ for 15 minutes to obtain a fermentation substrate, inoculate Lactobacillus plantarum and Pediococcus pentosaceus into the fermentation substrate at a total inoculation amount of 4% after activating culture, the mass ratio of Lactobacillus plantarum and Pediococcus pentosaceus is 2:1, oscillate and ferment at 28℃ and 150rpm for 55 hours, then sterilize at 80℃ for 20 minutes, centrifuge at a speed of 10000rpm for 3 minutes in a centrifuge to collect the supernatant, and obtain the pistacia chinensis leaf-sequoia sempervirens leaf acarid-removing antibacterial liquid.

[0034] S2: Enzymolysis purification of halistemma gelatinosum

[0035] ​S2.1: Fresh and live pennatula nipponica is washed clean, and after the umbrella edge of pennatula nipponica is removed by cutting, pennatula nipponica is cut into small pieces to obtain medusoid, the medusoid is added into 3 times volume of 0.4 mol / L sodium hydroxide solution, and then is homogenized in a homogenizer at a speed of 8000 rpm for 10 seconds, and is homogenized for 4 times under the same conditions, and then is placed at 3℃ for 20 hours, and then is centrifuged at 3℃ and a speed of 10000 rpm for 10 minutes, and the precipitate is washed to neutral, and filtration is performed to obtain pretreated medusoid;

[0036] S2.2: The pretreated medusoid and 0.5 mol / L acetic acid aqueous solution are uniformly mixed at a solid-liquid ratio of 1:6 g / mL, and then 4 wt% of pepsin is added to the pretreated medusoid, and the mixture is oscillated at 3℃ and a speed of 120 rpm for 45 hours, and then is centrifuged at a speed of 10000 rpm for 10 minutes, and the supernatant is added with NaCl until the concentration of NaCl is 2 mol / L, and the mixture is continuously incubated and placed for 24 hours, and then filtration is performed, and the precipitate is dissolved in 3 times mass concentration of 0.5 mol / L acetic acid aqueous solution, and then is loaded into a dialysis bag, and is dialyzed against distilled water for 42 hours, and the distilled water is replaced every 10 hours, and the solution in the dialysis bag is collected to obtain a pennatula nipponica collagen peptide solution.

[0037] S3: Preparation of phosphate-PAMAM bacterial membrane disruptant and compounding of antibacterial disinfectant powder

[0038] S3.1: 3 parts by weight of O-phospho-L-serine is dissolved in 30 parts by weight of deionized water under the condition of a water bath at 45℃, 1 mol / L HCl is added dropwise to adjust the pH to 5.5, and then 0.6 parts by weight of 1-ethyl-(3-dimethylaminopropyl) carbonyl diimide and 0.4 parts by weight of N-hydroxysuccinimide are added, and the mixture is stirred at 25℃ and a speed of 250 rpm for 30 minutes to obtain a phosphate esterification active solution;

[0039] S3.2: 5 parts by weight of five-generation dendritic polyamide amine is added to the phosphate esterification active solution prepared in step S3.1, and then 0.1 parts by weight of 4-dimethylaminopyridine is added, and the mixture is stirred at room temperature for 20 hours under a nitrogen atmosphere, and the stirring speed is 200 rpm, and then the mixture is rotary evaporated at 0.08 MPa and 60℃ for 2 hours, and then is washed clean with deionized water, and is dried to obtain a phosphate-PAMAM bacterial membrane disruptant;

[0040] S3.3: The yellow poplar leaf-northern red cedar leaf mite-killing antibacterial solution and the jellyfish collagen peptide solution were mixed uniformly at a mass ratio of 1:0.3, then 4wt% of the phosphate-PAMAM bacterial membrane disruptor, 0.8wt% of cetylpyridinium chloride, and 2wt% of trehalose were added and stirred uniformly, and then freeze-drying was performed at -50℃, and after crushing, the product was sieved through an 80-mesh sieve to obtain a low-irritation mite-killing antibacterial disinfectant powder.

[0041] Example 2: A preparation process of a low-irritation mite-killing antibacterial disinfectant powder, as shown in Figure 1 , includes the following steps:

[0042] S1: Enzymatic fermentation of yellow poplar leaf-northern red cedar leaf

[0043] S1.1: Yellow poplar leaves and northern red cedar leaves were taken at a mass ratio of 1:1.5, dried to a moisture content of 4%, then crushed and sieved through an 80-mesh sieve to obtain mixed leaf powder, and the mixed leaf powder was added to distilled water at a temperature of 45℃ at a solid-liquid ratio of 1:12g / mL, the pH was adjusted to 5, then 0.5wt% of β-glucosidase was added, and the mixture was oscillated at 45℃ and 150rpm for 8 hours to obtain a yellow poplar leaf-northern red cedar leaf enzyme-treated substrate;

[0044] S1.2: 1.2 parts by weight of the yellow poplar leaf-northern red cedar 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 mixed, the pH was adjusted to 7, and sterilization was performed at 121℃ for 15 minutes to obtain a fermentation substrate, and after activation culture, Lactobacillus plantarum and Pediococcus pentosaceus were inoculated into the fermentation substrate at a total inoculation amount of 5%, and the mass ratio of Lactobacillus plantarum to Pediococcus pentosaceus was 2:1, and then the mixture was oscillated at 28℃ and 150rpm for 55 hours, and then sterilization was performed at 80℃ for 20 minutes, and then the mixture was centrifuged at a speed of 10000rpm for 3 minutes, and then the supernatant was collected to obtain a yellow poplar leaf-northern red cedar leaf mite-killing antibacterial solution.

[0045] S2: Enzymatic purification of jellyfish collagen

[0046] S2.1: Fresh and live jellyfish were washed clean, and after cutting off the umbrella edge of the jellyfish, the jellyfish were cut into small pieces to obtain jellyfish collagen, and then the jellyfish collagen was added to 5 times the volume of a 0.4mol / L sodium hydroxide solution, and then the mixture was homogenized in a homogenizer at a speed of 8000rpm for 10 seconds, and then the homogenization was repeated 4 times under the same conditions, and then the mixture was placed at 3℃ for 20 hours, and then the mixture was centrifuged at 3℃ and 10000rpm for 10 minutes, and then the precipitate was washed to neutral, and then the mixture was filtered to obtain pretreated jellyfish collagen;

[0047] S2.2: The pretreated jellyfish mucilage and the aqueous acetic acid solution with a concentration of 0.5 mol / L were mixed uniformly at a solid-liquid ratio of 1:6 g / mL, then pepsin was added at 5 wt% of the pretreated jellyfish mucilage, and oscillation was carried out at 3°C and 120 rpm for 45 hours, then centrifugation was carried out at a rotation speed of 10000 rpm for 10 minutes to obtain supernatant, NaCl was added until the concentration of NaCl was 2 mol / L, and incubation was continued for 24 hours, then the precipitate was filtered and dissolved in 4 times the mass concentration of 0.5 mol / L aqueous acetic acid solution, then the solution was loaded into a dialysis bag and dialyzed against distilled water for 42 hours, the distilled water was replaced every 10 hours, the solution in the dialysis bag was collected, and a jellyfish collagen peptide solution was obtained.

[0048] S3: Preparation of phosphate ester-PAMAM bacterial membrane disruptor and compounding of low-irritation anti-mite and antibacterial disinfectant powder

[0049] S3.1: 5 parts by weight of O-phospho-L-serine were dissolved in 40 parts by weight of deionized water under the condition of a water bath at 45°C, 1 mol / L HCl was added dropwise to adjust the pH to 5.5, then 0.8 parts by weight of 1-ethyl-(3-dimethylaminopropyl) carbonyl diimide and 0.5 parts by weight of N-hydroxysuccinimide were added, and stirring was carried out at 25°C and 250 rpm for 30 minutes to obtain a phosphatized active solution;

[0050] S3.2: 7 parts by weight of a fifth-generation dendritic polyamide amine were added to the phosphatized active solution prepared in step S3.1, then 0.15 parts by weight of 4-dimethylaminopyridine were added, stirring was carried out at room temperature for 20 hours under a nitrogen atmosphere at a stirring speed of 200 rpm, then rotary evaporation was carried out at 0.08 MPa and 60°C for 2 hours, then the product was washed with deionized water until clean, and drying was carried out to obtain a phosphate ester-PAMAM bacterial membrane disruptor;

[0051] S3.3: The yellow poplar leaf-northern red cedar leaf anti-mite and antibacterial solution and the jellyfish collagen peptide solution were mixed uniformly at a mass ratio of 1:0.5, then 6 wt% of the phosphate ester-PAMAM bacterial membrane disruptor, 1 wt% of cetylpyridinium chloride and 3 wt% of trehalose were added and stirred uniformly, cold drying was carried out at -50°C, the product was crushed and sieved through an 80-mesh sieve, and a low-irritation anti-mite and antibacterial disinfectant powder was obtained.

[0052] Example 3, a preparation process of a low-irritation anti-mite and antibacterial disinfectant powder, as shown in Figure 1 , includes the following steps:

[0053] S1: Enzymatic fermentation of yellow poplar leaf-northern red cedar leaf

[0054] S1.1: Take the leaves of Pistacia chinensis Bunge and Pseudotsuga taxifolia in a mass ratio of 1:1, dry them to a moisture content of 8%, then crush them through a 100-mesh sieve to obtain a mixed leaf powder. Add the mixed leaf powder to distilled water at a temperature of 50°C at a solid-liquid ratio of 1:15 g / mL, adjust the pH to 5.5, then add 0.3wt% of β-glucosidase, and oscillate at 50°C and 180 rpm for 10 hours to obtain a Pistacia chinensis Bunge-Pseudotsuga taxifolia enzyme-treated substrate;

[0055] S1.2: Take 1 part by weight of the Pistacia chinensis Bunge-Pseudotsuga taxifolia enzyme-treated substrate, 0.1 parts by weight of glucose, 0.1 parts by weight of yeast extract, 0.06 parts by weight of inulin, and 0.02 parts by weight of salt, adjust the pH to 7.5, and sterilize at 121°C for 20 minutes to obtain a fermentation substrate. After activating the cultures of Lactobacillus plantarum and Pediococcus pentosaceus, inoculate them into the fermentation substrate at a total inoculum of 4%, with a mass ratio of Lactobacillus plantarum to Pediococcus pentosaceus of 2:1. Oscillate the fermentation at 30°C and 180 rpm for 60 hours, then sterilize at 85°C for 25 minutes, and centrifuge at 12,000 rpm for 4 minutes to collect the supernatant, thereby obtaining a Pistacia chinensis Bunge-Pseudotsuga taxifolia acarid-repelling and antibacterial liquid.

[0056] S2: Enzymatic extraction and purification of Halistemma gelatinosa

[0057] S2.1: Wash fresh Halistemma gelatinosa thoroughly, cut off the edge of the umbrella part, and then cut into small pieces to obtain jellyfish gelatin. Add the jellyfish gelatin to 3 times its volume of a 0.5 mol / L sodium hydroxide solution, and then homogenize in a homogenizer at a speed of 11,000 rpm for 15 seconds. Repeat the homogenization 5 times under the same conditions, and then let stand at 4°C for 24 hours. Centrifuge at 4°C and 12,000 rpm for 12 minutes, wash the precipitate with water until it is neutral, and then filter to obtain pretreated jellyfish gelatin.

[0058] S2.2: Mix the pretreated jellyfish gelatin with an aqueous acetic acid solution at a concentration of 0.55 mol / L at a solid-liquid ratio of 1:8 g / mL, and then add pepsin at 5wt% of the pretreated jellyfish gelatin. Oscillate at 4°C and 140 rpm for 48 hours, and then centrifuge at a speed of 12,000 rpm for 12 minutes to obtain the supernatant. Add NaCl to the supernatant until the concentration of NaCl is 2.5 mol / L, and then continue to incubate for 30 hours. Filter to collect the precipitate, and then dissolve it in 3 times its mass of an aqueous acetic acid solution at a concentration of 0.55 mol / L. Place the solution in a dialysis bag, and dialyze against distilled water for 48 hours. Replace the distilled water every 12 hours. Collect the solution in the dialysis bag to obtain a Halistemma gelatinosa collagen peptide solution.

[0059] S3: Preparation of phosphate-PAMAM bacterial membrane disruptant and compounding of antibacterial and disinfectant powder

[0060] S3.1: 3 parts by weight of O-phospho-L-serine was dissolved in 30 parts by weight of deionized water at 50°C in a water bath, 1 mol / L HCl was added dropwise to adjust the pH to 6, then 0.6 parts by weight of 1-ethyl-(3-dimethylaminopropyl) carbodiimide and 0.4 parts by weight of N-hydroxysuccinimide were added, and stirred at 30°C and 300 rpm for 40 minutes to obtain a phosphonate active solution;

[0061] S3.2: 5 parts by weight of fifth-generation dendritic polyamidoamine was added to the phosphonate active solution prepared in step S3.1, and 0.1 parts by weight of 4-dimethylaminopyridine was added, stirred at room temperature for 24 hours under nitrogen atmosphere, the stirring speed was 250 rpm, then rotary evaporation was carried out at 0.1 MPa and 65°C for 3 hours, then washed with deionized water until clean, and dried to obtain a phosphonate-PAMAM cell membrane disruptant;

[0062] S3.3: The yellow poplar leaf-northern red cedar leaf mite-killing antibacterial solution and the chrysaora collagen peptide solution were mixed uniformly at a mass ratio of 1:0.3, then 4wt% of the phosphonate-PAMAM cell membrane disruptant, 0.8wt% of cetylpyridinium chloride and 2wt% of trehalose were added and stirred uniformly, then freeze-dried at -40°C, crushed and sieved through a 100-mesh sieve to obtain a low-irritation mite-killing antibacterial disinfectant powder.

[0063] Comparative Example 1 differs from the embodiment of Example 1 in that Comparative Example 1 replaces the yellow poplar leaves in step S1.1 with equal mass of northern red cedar leaves to prepare a northern red cedar leaf mite-killing antibacterial solution, and replaces the subsequent yellow poplar leaf-northern red cedar leaf mite-killing antibacterial solution with the northern red cedar leaf mite-killing antibacterial solution, and the remaining specific embodiments are the same as those of Example 1.

[0064] Comparative Example 2 differs from the embodiment of Example 1 in that Comparative Example 2 replaces the northern red cedar leaves in step S1.1 with equal mass of yellow poplar leaves to prepare a yellow poplar leaf mite-killing antibacterial solution, and replaces the subsequent yellow poplar leaf-northern red cedar leaf mite-killing antibacterial solution with the yellow poplar leaf mite-killing antibacterial solution, and the remaining specific embodiments are the same as those of Example 1.

[0065] Comparative Example 3 differs from the embodiment of Example 1 in that Comparative Example 3 removes step S2, and replaces the chrysaora collagen peptide solution in step S3.3 with equal mass of distilled water, and the remaining specific embodiments are the same as those of Example 1.

[0066] Comparative Example 4 differs from the embodiment of Example 1 in that Comparative Example 4 removes steps S3.1 and S3.2, and does not add the phosphonate-PAMAM cell membrane disruptant in step S3.3, and the remaining specific embodiments are the same as those of Example 1.

[0067] The low-irritation anti-mite antibacterial disinfectant powder prepared in Examples 1-3 was selected and configured into a disinfectant solution with a concentration of 30% with water as a sample to perform acute oral toxicity test and multiple complete skin irritation test.

[0068] Acute oral toxicity test: 20 healthy Kunming mice with a body weight of (20±0.2) g were selected, half male and half female, and divided into 4 groups, 5 mice in each group, corresponding to the samples of Examples 1-3 and a blank group (without gavage), the night before gavage, the animals were not allowed to eat but allowed to drink, the sample dose of the tested substance was 5000 mg / kg of body weight, after gavage, the animals were allowed to eat and drink normally, the clinical performance of the experimental animals was observed and the number of dead animals was recorded, the observation was continuously performed for 14 days, the average value was calculated after the body weight was measured at the end of the test, the mice were sacrificed and pathological observation was performed, and the test results are shown in Table 1.

[0069] Table 1: Results of mouse acute oral toxicity test of example samples

[0070]

[0071] Multiple complete skin irritation test: 15 healthy New Zealand rabbits were selected and divided into 3 groups, the hair on both sides of the dorsal spine was removed about 3 cm x 3 cm on each side 24 hours before the test without damaging the epidermis, different samples were applied to the right side of the skin removed of hair the next day, and the left side of the skin removed of hair was applied with normal saline as a blank control, after 4 hours of application, the residual was washed off with warm water, the application was performed once a day for 14 consecutive days, the skin irritation reaction was observed and scored 24 hours after each application, and the results are shown in Table 2.

[0072] Table 2: Results of multiple complete skin irritation test of example samples

[0073]

[0074] From the results of the mouse acute oral toxicity test in Table 1, no animal poisoning symptoms and death occurred during the 14-day continuous observation, which can prove that the low-irritation anti-mite antibacterial disinfectant powder prepared in the examples is actually non-toxic, and from the results of the multiple complete skin irritation test of the example samples in Table 2, after 14 days of repeated contact stimulation, the test skin of the rabbits in the sample group and the control skin were both normal, according to the scoring standard, the average score was 0, the multiple skin irritation index was 0, and the irritation intensity was non-irritating.

[0075] The low-irritation anti-mite antibacterial disinfectant powder prepared in Examples 1-3 and Comparative Examples 1-4 were selected and configured into a disinfectant solution with a concentration of 5% with water as a sample to perform anti-mite and sterilization test.

[0076] Mite removal test: 18 pieces of circular cloth with a diameter of 10 cm were prepared, high-temperature steamed and dried, then divided into 6 groups, 3 pieces in each group, placed in a culture dish, 0.1 g of mite feed was spread on each piece of cloth, then 100 live mites were put in, and the live mites were wrapped up by folding, after 10 minutes, immersed in the samples prepared in Examples 1-3, Comparative Examples 1-2 and distilled water, distilled water as a blank group, for 5 minutes, then take out and open the folded cloth, immerse in distilled water and stir at a speed of 200 rpm for 5 minutes, record the number of mites on the cloth, denoted as N, the mite removal rate% = (100-N) / 100x100%, the results are shown in Table 3.

[0077] Table 3: Mite removal rate of 5% concentration disinfectant

[0078]

[0079] Bactericidal test: Escherichia coli, Staphylococcus aureus and Candida albicans strains were inoculated on the required nutrient agar medium plate, single typical colonies were isolated and inoculated for enrichment culture, then the colonies were eluted with TPS diluent to prepare a bacterial suspension with a bacterial content of (1x10 8 ~5x10 8 ) cfu / mL, 4 mL of samples prepared in Examples 1-3, Comparative Examples 1-4 and distilled water were taken and mixed with 1 mL of bacterial suspension at 20°C water bath, after 5 minutes of action, placed on a sterile filter membrane and washed with sterile hard water, then the filter membrane was pasted on an agar medium plate and incubated at 37°C for 48 h, the number of colonies was counted, the average killing logarithm was calculated, the test was repeated three times, and the average killing logarithm was taken as the test result, which is shown in Table 4.

[0080] Table 4: Average killing logarithm of 5% concentration disinfectant on each bacterial species

[0081]

[0082] As can be seen from Table 3, the mite removal rates of Examples 1-3 all reached more than 97%, which can prove that the low-irritation mite removal antibacterial disinfectant powder prepared in the application has good mite removal effect, and the mite removal rate of Comparative Example 1-2 has a significant decrease, which proves that there is a synergistic effect of pistacia chinensis leaf and sequoia sempervirens leaf on mite removal effect.

[0083] As can be seen from Table 4, the killing logarithm values of Examples 1-3 to E. coli, S. aureus and C. albicans all reached the standard requirements of disinfectants (≥5 to E. coli, ≥5 to S. aureus, and ≥4 to C. albicans), which proved that the present application has excellent bactericidal effect, while the killing logarithm values of Comparative Examples 1-4 decreased significantly, which proved that there is a synergistic effect between the leaves of V. fordii and the leaves of P. taxifolia in the bactericidal effect, and the addition of jellyfish collagen peptide and phosphate-PAMAM bacterial membrane disruptor can enhance the bactericidal effect.

[0084] The above examples only illustrate the principles and effects of the present application, and are not used to limit the present application. Any person skilled in the art can modify or change the above examples without departing from the spirit and scope of the present application. Therefore, all equivalent modifications or changes completed by those skilled in the art without departing from the spirit and technical ideas disclosed by the present application should be covered by the claims of the present application.

Claims

1. A preparation process for a low-irritation mite-removing and antibacterial disinfectant powder, characterized in that, Includes the following steps: S1 Enzymatic hydrolysis and fermentation of Pistacia chinensis leaves and redwood leaves: Pistacia chinensis leaves and redwood leaves are dried and crushed, then enzymatically hydrolyzed by β-glucosidase mixture. After adding glucose, yeast extract, inulin and salt, fermentation is carried out by mixed fermentation of Lactobacillus plantarum and Pediococcus pentosus. The supernatant is collected by centrifugation to obtain Pistacia chinensis leaves and redwood leaves anti-mite and antibacterial liquid. Enzymatic hydrolysis and purification of S2 whiptail jellyfish gelatinous bodies: After processing the whiptail jellyfish, it was treated with alkali, then hydrolyzed with pepsin, the supernatant was collected by centrifugation, NaCl was added for precipitation, and then dissolved in acetic acid aqueous solution and dialyzed with distilled water to obtain whiptail jellyfish collagen peptide solution. Preparation of S3 phosphate ester-PAMAM biofilm destroyer and compounding of antibacterial disinfectant powder: O-phospho-L-serine was dissolved in deionized water, and after adjusting the pH, 1-ethyl-(3-dimethylaminopropyl)carbodiimide and N-hydroxysuccinimide were added and mixed evenly. Then, fifth-generation dendritic polyamide amine-linked amino and 4-dimethylaminopyridine were added. After stirring and rotary evaporation, the mixture was washed clean and dried to obtain phosphate ester-PAMAM biofilm destroyer. The anti-mite and antibacterial liquid of Pistacia chinensis leaf-North American redwood leaf, collagen peptide solution of Trichoderma variegata, and phosphate ester-PAMAM biofilm destroyer were mixed, freeze-dried, and pulverized to obtain low-irritant anti-mite and antibacterial disinfectant powder. Step S3 specifically includes 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 under a water bath at 45-50℃, adjust the pH to 5.5-6 by adding 1 mol / L HCl dropwise, 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 for 30-40 minutes at 25-30℃ and 250-300 rpm to obtain a phosphorylation active solution; S3.2: Add 5-7 parts by weight of fifth-generation dendritic polyamide amine to the phosphate esterification 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 under a nitrogen atmosphere at a stirring speed of 200-250 rpm. Then, rotary evaporate at 0.08-0.1 MPa and 60-65℃ for 2-3 hours. Then, wash with deionized water and dry to obtain phosphate ester-PAMAM biofilm destroyer. S3.3: Mix the Pistacia chinensis leaf-Redwood leaf anti-mite and antibacterial solution and the Collagen peptide solution of Trichoderma variegata at a mass ratio of 1:(0.3-0.5). Then add 4-6wt% of phosphate ester-PAMAM bacterial film destroyer, 0.8-1wt% of cetylpyridinium chloride and 2-3wt% of trehalose and stir evenly. Freeze-dry at -50℃ to -40℃, pulverize and pass through an 80-100 mesh sieve to obtain a low-irritant anti-mite and antibacterial disinfectant powder.

2. The preparation process of a low-irritation anti-mite and antibacterial disinfectant powder according to claim 1, characterized in that, Step S1, enzymatic fermentation of *Pistacia chinensis* leaves and *Sequoia glyptostroboides* leaves, includes the following steps: S1.1: Take Chinese pistache leaves and North American redwood leaves in a mass ratio of 1:(1-1.5), dry them to a moisture content of 4-8%, then pulverize them through an 80-100 mesh sieve to obtain mixed leaf powder. Add the mixed leaf powder to distilled water at a temperature of 45-50℃ at a material-to-liquid ratio of 1:(12-15) g / mL, adjust the pH to 5-5.5, then add 0.3-0.5wt% β-glucosidase, and shake for 8-10 hours at 45-50℃ and 150-180 rpm to obtain the Chinese pistache leaf-North American redwood leaf enzyme-treated substrate. S1.2: Mix 1-1.2 parts by weight of the enzyme-treated substrate of *Pistacia chinensis* leaves and *Sequoia glyptostroboides* leaves, 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, adjust the pH to 7-7.5, and sterilize at 121℃ for 15-20 minutes to obtain the fermentation substrate. After activating and culturing *Lactobacillus plantarum* and *Pediococcus pentosaceus*, inoculate them into the fermentation substrate at a total inoculum of 4-5%. Ferment at 28-30℃ and 150-180 rpm for 55-60 hours with shaking. Then, heat to 80-85℃ for sterilization for 20-25 minutes, centrifuge at 10000-12000 rpm for 3-4 minutes, and collect the supernatant to obtain the anti-mite and antibacterial solution of *Pistacia chinensis* leaves and *Sequoia glyptostroboides* leaves.

3. The preparation process of a low-irritation mite-removing and antibacterial disinfectant powder according to claim 2, characterized in that, Step S2, enzymatic hydrolysis and purification of the gelatinous body of *Tetracentron sinense*, includes the following steps: S2.1: Clean the live flagellated jellyfish, trim off the edge of the bell, and cut into small pieces to obtain the jellyfish gelatinous body. Add the jellyfish gelatinous body to 3-5 times the volume of sodium hydroxide solution with a concentration of 0.4-0.5 mol / L, and then place it in a homogenizer and homogenize at 8000-11000 rpm for 10-15 seconds. Repeat the homogenization under the same conditions 4-5 times, and then let it stand at 3-4℃ for 20-24 hours. Then centrifuge at 3-4℃ and 10000-12000 rpm for 10-12 minutes. Take the precipitate, wash it with water until neutral, and filter to obtain the pretreated jellyfish gelatinous body. S2.2: Mix the pretreated jellyfish gelatinous body and acetic acid aqueous solution at a material-to-liquid ratio of 1:(6-8) g / mL. Then add 4-5 wt% pepsin to the pretreated jellyfish gelatinous body and shake at 3-4℃ and 120-140 rpm for 45-48 hours. Then maintain the temperature and centrifuge at 10000-12000 rpm for 10-12 minutes. Take the supernatant and add NaCl until the NaCl concentration is 2-2.5 mol / L. Continue to keep warm and stand for 24-30 hours. Filter and dissolve the precipitate in 3-4 times the mass of acetic acid aqueous solution. Then put it into a dialysis bag and dialyze it with distilled water for 42-48 hours. Collect the solution in the dialysis bag to obtain the jellyfish collagen peptide solution.

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

1.

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

6. The preparation process of a low-irritation anti-mite and antibacterial disinfectant powder according to claim 3, characterized in that, During the dialysis process in step S2.2, the distilled water is changed every 10-12 hours.

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