CN117653703A - Preparation method of polyphenol liquid for sterilization, disinfection and deodorization - Google Patents
Preparation method of polyphenol liquid for sterilization, disinfection and deodorization Download PDFInfo
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- CN117653703A CN117653703A CN202410083177.6A CN202410083177A CN117653703A CN 117653703 A CN117653703 A CN 117653703A CN 202410083177 A CN202410083177 A CN 202410083177A CN 117653703 A CN117653703 A CN 117653703A
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- Prior art keywords
- liquid
- solution
- sterilization
- stirring
- polyphenol
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- 239000007788 liquid Substances 0.000 title claims abstract description 113
- 235000013824 polyphenols Nutrition 0.000 title claims abstract description 105
- 150000008442 polyphenolic compounds Chemical class 0.000 title claims abstract description 92
- 238000004659 sterilization and disinfection Methods 0.000 title claims abstract description 79
- 230000001954 sterilising effect Effects 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 238000004332 deodorization Methods 0.000 title claims abstract description 24
- 235000005487 catechin Nutrition 0.000 claims abstract description 81
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 claims abstract description 81
- 229950001002 cianidanol Drugs 0.000 claims abstract description 75
- PFTAWBLQPZVEMU-DZGCQCFKSA-N (+)-catechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-DZGCQCFKSA-N 0.000 claims abstract description 74
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- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 24
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims abstract description 24
- 230000001681 protective effect Effects 0.000 claims abstract description 24
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- SNPLKNRPJHDVJA-ZETCQYMHSA-N D-panthenol Chemical compound OCC(C)(C)[C@@H](O)C(=O)NCCCO SNPLKNRPJHDVJA-ZETCQYMHSA-N 0.000 claims abstract description 8
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- 238000003756 stirring Methods 0.000 claims description 75
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 63
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 20
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Abstract
The invention discloses a preparation method of polyphenol liquid for sterilization, disinfection and deodorization, belonging to the technical field of catechin composition preparation showing sterilization activity. The polyphenol liquid of the invention comprises 20 to 40 percent of catechin extracting solution, 5 to 10 percent of antioxidant protective solution B phase, 2.0 to 4.0 percent of glycine, 2.0 to 5.0 percent of neroli hydrosol, 0.5 to 2.0 percent of panthenol, 2.0 to 5.0 percent of glycerol and 3.0 to 6.0 percent of bamboo charcoal liquid. The synergistic effect of the components can promote the overall excellent disinfection and sterilization effect, and has no irritation to skin. The novel form of the disinfecting and deodorizing liquid is developed, and the disinfecting and deodorizing liquid can be used for disinfecting and sterilizing mucous membranes of mouth, nose, eyes and oral cavity.
Description
Technical Field
The invention belongs to the technical field of catechin composition preparation showing bactericidal activity, and particularly relates to a preparation method of polyphenol liquid for sterilizing, disinfecting and deodorizing skin.
Background
At present, the demand of the sterilizing products with antibacterial and bactericidal effects on the market is quite large, various sterilizing and bactericidal products on the market are layered endlessly, but most of sterilizing and disinfecting components are chemical components, and commonly used iodine-containing preparations, such as 75% alcohol, diethyl ether, chloroform, formaldehyde, chlorine-containing disinfectant, peracetic acid and the like, are generally adopted. Moreover, the preparations have strong irritation to human skin, can not be used for disinfection in the oral cavity, and also cause certain damage to the human body while killing bacteria, and the harm caused by aspiration or miseating of people is larger,
according to the disinfectant guideline issued by 19 days 2 and 2 in 2020, the alcohol disinfectant contains 70-80% of ethanol and the alcohol disinfectant contains more than 60% of ethanol, but the alcohol disinfectant has short disinfection effect and cannot be disinfected and antibacterial for a long time. Therefore, development of an antibacterial ingredient which is natural, green, harmless to the human body and can be disinfected for a long time is an urgent problem to be solved in the industry.
The Chinese patent publication No. CN102349992B discloses a medical skin disinfectant which is prepared by mixing purslane, fructus cnidii, clove, star anise, dried ginger, toad, white peony root, honeysuckle and saffron, adding water, decocting, and matching with polyvinyl chloride nonylphenol ether, glycerol, available iodine and metronidazole.
The Chinese patent publication No. CN103494745B discloses a tea polyphenol antibacterial wet tissue and a preparation method thereof, and refers to loading a liquid medicine containing tea polyphenol on a base material non-woven fabric, so that the tea polyphenol antibacterial wet tissue has the effects of cleaning, moisturizing, disinfecting and sterilizing the skin. However, in order to enhance the sterilization effect, the bactericide is compounded, and the bactericide consists of cetylpyridinium chloride and benzethonium chloride, so that the chlorine-containing bactericide increases the risk of skin allergy, and the skin becomes dry and tight due to the frequent use of the chlorine-containing bactericide, and becomes rough due to the long-term use of the chlorine-containing bactericide.
Polyphenols are the sum of polyphenols extracted from green tea, and the main component in the tea polyphenols is catechin, accounting for 70-80%. Catechin is a plant secondary metabolite containing a plurality of phenolic hydroxyl groups and having a plurality of biological activities, and is widely studied and paid attention to because of the outstanding antioxidant, anti-inflammatory and antibacterial effects and the like. Catechin is a high-efficiency natural antioxidant which is free from toxic and side effects and is found and utilized at present, and is white crystalline at normal temperature, but is easy to oxidize or polymerize in the extraction process, so that the catechin is usually light yellow to brown, has astringency and is slightly fragrant; catechin has a plurality of hydroxyl groups, is easy to dissolve in water, and after tea polyphenol is dissolved in water, but according to Wang Liqing and the like, in the experiment of stability of tea polyphenol aqueous solution, the validity period of the tea polyphenol in the aqueous solution is only 17-18 hours. This is because catechin is unstable in water and is easily deteriorated by strong alkali, strong acid, light and the like. Catechins are readily oxidized by oxygen in air or water to form o-quinones, or oxidized and polymerized in the presence of alkaline or acidic oxidants to form theaflavins.
The Chinese patent with publication number of CN108653713B discloses a preparation method of a natural composite antibacterial composition containing tea saponin, which has broad-spectrum antibacterial effect after compounding tea polyphenol, tea saponin, purslane extract and tea dreg antibacterial peptide, and can kill various bacteria rapidly.
Therefore, how to prepare a natural and safe polyphenol liquid with lasting activity and excellent sterilization and disinfection effects is a difficult problem which needs to be solved at present.
Disclosure of Invention
In order to solve the above problems, the present invention provides a method for preparing a polyphenol liquid for sterilization, disinfection and deodorization, which solves one or more technical problems existing in the prior art, and at least provides a beneficial selection or creation condition.
Aiming at the defects and shortcomings in the background technology, the invention provides the polyphenol liquid for sterilization, disinfection and deodorization and the preparation method thereof, and the polyphenol liquid has good sterilization and deodorization effects, simple components and no irritation to skin; meanwhile, the preparation method can keep the activity of each component for a long time, so that catechin in the tea polyphenol can exist in the aqueous solution stably, and the sterilization and disinfection effects can be continuously exerted for a long time.
According to one aspect of the invention, water-soluble catechins are first extracted from tea leaves in order to avoid oxidation of catechins in aqueous solution to form o-quinones during extraction or oxidative polymerization in the presence of an acidic oxidant to form theaflavins. The antioxidant protective liquid comprises a phase A and a phase B, wherein the phase A plays a role in protecting activity during catechin extraction, and the phase B plays a role in synergistically protecting activity in polyphenol liquid, and the preparation method is as follows:
s001, selecting spherical sodium-based montmorillonite with the nano diameter of 10-30 nm, adding deionized water into the spherical sodium-based montmorillonite, adding hydrochloric acid, stirring uniformly to ensure that the pH value is 3.2-3.8, fully dispersing the spherical sodium-based montmorillonite in a dilute hydrochloric acid solution, heating to 60 ℃, adding glutamic acid, fully stirring, and reacting for 1-2 hours to ensure that sodium in the montmorillonite is released by NH of the glutamic acid 3 + Substitution, according to the amphoteric characteristic of glutamic acid, under the action of pH greater than 3.2, NH is released 3 + Protons to make the spherical montmorillonite in the suspension become COO in the inner layer - A group, the outer layer is NH 3 + Spherical charge groups of protons. Taking out the montmorillonite suspension, centrifuging at 3500rpm, washing with deionized water for 2-3 times to remove hydrochloric acid, centrifuging, taking out the solid mixture at the bottom, oven drying at 60deg.C, and grinding to obtain COO as inner layer - A group, the outer layer is NH 3 + The spherical montmorillonite of proton is marked as active positive charge particle.
Wherein, the mass percentage of the spherical sodium-based montmorillonite is 1-3%, and the mass ratio of the spherical sodium-based montmorillonite to the glutamic acid is 1:3-8.
S002, selecting spherical sodium montmorillonite with the nano diameter of 10-30 nm, adding deionized water into the spherical sodium montmorillonite in a reaction kettle, adding sodium carbonate, stirring uniformly to ensure that the pH value is 9.0-9.5, fully dispersing the sodium montmorillonite in alkaline solution, continuously adding lysine, fully stirring, reacting for 1-2 hours, and ensuring that sodium groups in the montmorillonite are released by NH of the lysine 3 + Substitution, according to the amphoteric characteristic of lysine, under the action of pH less than 9.6, COO is released - Radicals which make montmorillonite in suspension as NH as inner layer 3 + Proton, with COO as outer layer - Spherical charge groups of the groups. Taking out the montmorillonite suspension, and making the montmorillonite suspension at 3500rpmCentrifugal separation, washing with deionized water for 2-3 times to remove sodium carbonate, centrifugal separation, taking out bottom solid mixture, oven drying at 60deg.C, grinding to obtain inner layer of NH 3 + Proton, with COO as outer layer - The spherical montmorillonite of the group is marked as an active negative charge particle group.
Wherein, the mass percentage of the spherical sodium-based montmorillonite is 1-3%, and the mass ratio of the spherical sodium-based montmorillonite to the lysine is 1:3-8.
S003, adding bamboo vinegar and deionized water into a reaction kettle, uniformly stirring, and then adding active positive charge particles to enable the active positive charge particles to be fully dispersed in the bamboo vinegar solution, wherein the pH value is 4.5-5.0. Stirring and reacting for 1-2 hours, and taking out the mixed solution to obtain the phase A of the antioxidant protection solution. The bamboo vinegar accounts for 3 to 5 mass percent, wherein the active positive charge grain groups account for 3 to 5 mass percent.
S004, deionized water is added into a reaction kettle, then active negative charge particles are added, and the mixed solution obtained after full dispersion is the B phase of the antioxidant protection solution, wherein the active negative charge particles are 2-4%.
Glutamic acid and lysine are a typical class of amphoteric molecules, i.e. with a proton-releasing NH on the same molecule 3 + Positive ions and COO capable of accepting protons - The negative ions have acidic and basic functional groups at the same time, are strong electrolytes in aqueous solution, and have high solubility in strong polar solvents. By adjusting the acid-base of the aqueous solution, the aqueous solution can be made to take on different molecular states. When the tendency or degree of dissociation of glutamic acid or lysine into cations and anions is the same in a solution at a certain pH, the amino acid is electrically neutral, and the pH of the solution is the isoelectric point of glutamic acid or lysine. When the pH of the solution is higher than the isoelectric point, glutamic acid or lysine releases protons to be negatively charged; when the pH of the solution is less than the isoelectric point, glutamic acid or lysine is protonated to be positively charged, so that the control of the charge of the solution can be realized by changing the pH value of the system. Glutamic acid has an isoelectric point of 3.2 and lysine has an isoelectric point of 9.6. The entire system is in a dynamic equilibrium by a low pH and a high pH difference.
Further, catechin is extracted by using an antioxidant protection solution at a low temperature, and the extraction method comprises the following steps:
s101, cleaning tea, freeze-drying, pulverizing to obtain pulverized mixture,
s102, adding an antioxidant protection liquid A phase with the mass 1-3 times of that of the mixture into the crushed mixture, extracting in an ultrasonic extractor at the temperature of 5-10 ℃, uniformly stirring, standing for reaction for 40-60 minutes, and filtering by a filter screen with 800 meshes to obtain a first-stage extraction liquid and first-stage filter residues for later use;
s103, in order to extract more fully, extracting the first-stage filter residue again, adding 1-3 times of antioxidant protection liquid A phase into the first-stage filter residue in the step S102, placing the first-stage filter residue in an ultrasonic extractor for secondary extraction at the temperature of 20-30 ℃, stirring uniformly, standing for 40-60 minutes, and filtering by using a 800-mesh filter screen to obtain second-stage extract and second-stage filter residue;
s104, mixing the second-stage extracting solution and the first-stage extracting solution to obtain a third extracting solution, and fully stirring at the temperature of 20-30 ℃; concentrating the third extract at 20-30deg.C and-0.09 to-0.1 Mpa under low temperature and vacuum to remove 50% of water to obtain catechin extract, and preserving at 2-5deg.C;
The catechin extraction solution comprises: catechin, epicatechin, gallocatechin, epigallocatechin, catechin gallate, epicatechin gallate and epicatechin gallate;
the ultrasonic power is 50-100W, and the extraction time is 1-2 h.
After catechin is dissolved in water to form catechin aqueous solution, the sterilizing and disinfecting effects of the catechin aqueous solution are gradually attenuated along with the change of temperature, and Guo Ziyu and the like are proposed in chemical stability of tea polyphenols and attenuation dynamics study of the catechin aqueous solution in the disinfecting process in China science and technology paper: the regression equation of the mass concentration of the tea polyphenol solution with the change of time accords with a first-order kinetic formula under the natural state, and the attenuation of the tea polyphenol is a first-order kinetic reaction. Temperature (temperature)The decay rate of tea polyphenol can be obviously influenced, and the decay is faster at high temperature; the self mass concentration of the tea polyphenol also affects the attenuation rate, and the attenuation rate is faster at low mass concentration. Thus if tea polyphenols are extracted with aqueous solution only at low temperature, the tea polyphenols are still continuously decaying at the rate of the primary kinetic reaction. To prevent this attenuation, we need to protect its active groups with a protective liquid. However, among catechins, epigallocatechin-gallate and epigallocatechin have the best antibacterial effect due to the galloyl group, whereas epicatechin and gallocatechin having no such group do not exhibit the good antibacterial effect. Therefore, it is known that the bactericidal and antibacterial effects of catechin in tea polyphenols are mainly due to the effect of phenolic hydroxyl groups on benzene rings. Therefore, it is desirable to protect the phenolic hydroxyl group from polycondensation or oxidation in aqueous solutions. The A phase of the anti-oxidation protective solution is an acidic solution, the catechin has better stability under an acidic environment, and the A phase of the anti-oxidation protective solution provides uniformly dispersed active positive charge clusters. Structurally, catechins have phenolic hydroxyl groups directly bonded to aromatic rings by sp 2 The hybridized carbon atoms are connected, the unshared P electron on the oxygen atom and pi electron cloud on the benzene ring form a P-pi conjugated system, so that the P electron is deviated to the direction of the benzene ring, the strength of the C-O bond is enhanced, the electron cloud density on the O-H bond is reduced, the strength is weakened, and the polarity is increased. In the case of polyphenols, since they contain a plurality of phenolic hydroxyl groups, the formation of the poly-p-x conjugated system increases the degree of electron delocalization even more, because of the polar effect of the phenolic hydroxyl groups, the phenolic hydroxyl groups on catechins free in aqueous solution are surrounded by active positively charged clusters and thus protected. At this time, each free catechin molecule is surrounded by active positive charge clusters due to the action of polar bonds, forming a center similar to an ionic atmosphere. In solution, the free ionic atmosphere undergoes thermal motion which in turn causes a chaotic distribution of the ionic atmosphere, but is insufficient to counteract the attractive effect of molecular bonds. At the same time, there are countless free catechin ion atmosphere centers in the solution, each catechin ionThe charge of the atmosphere is the surrounding ring loaded with the active positive charge particles, and according to the principle of homopolar repulsion, the collision probability of catechin and catechin is very small, so that the catechin generates the polycondensation reaction to generate theaflavine due to the existence of the active positive charge particles, the probability of consuming phenolic hydroxyl groups is greatly reduced, and the stability of catechin aqueous solution is obviously improved under the condition that the active positive charge particles exist.
Further, the sterilizing and deodorizing polyphenol liquid comprises the following substances in percentage by mass: 20.0 to 40.0 percent of catechin extract, 5.0 to 10.0 percent of oxidation-resistant protective liquid B phase, 2.0 to 4.0 percent of glycine, 2.0 to 5.0 percent of neroli hydrosol, 0.5 to 2.0 percent of panthenol, 2.0 to 5.0 percent of glycerol, 3.0 to 6.0 percent of bamboo charcoal liquid and the balance of deionized water;
further, the bamboo charcoal liquid is 20% bamboo charcoal powder, which is ground by a screen mesh of 800 meshes, soaked in 8-10% bamboo vinegar water solution for 24 hours, and then activated.
Further, the preparation method of the sterilizing and deodorizing polyphenol liquid comprises the following steps:
s201, placing catechin extracting solution and anti-oxidation protective solution B phase into a reaction kettle, and uniformly stirring at 100-200 r/min;
wherein the mass ratio of the active positive charge particles to the active negative charge particles is more than 1.2;
s202, adding panthenol, stirring at a speed of 400-600 r/min, dripping glycine, stirring uniformly, stirring at a speed of 100-200 r/min after dripping, reacting for 1-2 hours, adding bamboo charcoal liquid, stirring at a speed of 100-200 r/min, reacting for 1-2 hours, adjusting pH to 5.5-5.6, and standing for 1-2 hours;
Sampling and testing the mixture obtained in the step S202 to detect whether sediment exists or not; if the test result shows that there is a precipitate, repeating the stirring and standing processes in the step S202 until the detected test result shows that there is no precipitate, and then entering the step S203;
and S203, finally adding 2.0-5.0% of glycerin, 2.0-5.0% of neroli hydrolat and the balance of deionized water, and uniformly stirring to obtain polyphenol liquid.
Because the obtained catechin extract contains a large amount of active positive charge particles, phenolic hydroxyl groups are temporarily protected, and free catechin is prevented from being consumed in polycondensation reaction. However, under the action of positive charge in an acidic environment, the polarity of the free catechin increases, so that the dissociation tendency of hydrogen atoms in phenolic hydroxyl groups increases, and if the hydrogen atoms are dissociated, NH carried on active positive charge clusters is easy to follow 3 + Releasing protons H + The amino groups after the reaction of conjugated acid-base pair consume hydrogen ions, so that the pH value of catechin solution is increased, the acidic environment of catechin is changed, active positive charge clusters are changed, the active positive charge clusters are changed into an inner layer which can provide positive charges, and an outer layer which can release protons and is negatively charged, so that the denaturation of the positive charge clusters occurs. In order to maintain this balance, and also after the hydrogen ions have been consumed, a substance is available to supply and release protons H + To maintain this balance we have designed an opposite phase B of the antioxidant protection fluid containing active negatively charged clusters. The two active clusters are mutually restricted, are maintained in a dynamic balance, and when only one charge exists in the solution, the ion movement of the active clusters is messy, and the free catechin has a certain collision opportunity. When active positive charge clusters are excessive and active negative charge clusters exist in the solution, attractive movement of positive and negative charges can occur, repulsive movement of like charges can also occur, and finally dynamic balance is achieved between the two movements, so that free catechin can only move around the ion atmosphere. The dynamic balance further restricts the oxidation of catechin to form o-quinone, or the oxidation condensation reaction occurs in the presence of an acidic oxidant, so that the stability time of catechin aqueous solution is prolonged, and the sterilization and antibacterial effects are enhanced.
On the other hand, glycine is also added into the polyphenol liquid, the isoelectric point of the glycine is about 6.0, when the positive and negative charges in the solution are unbalanced and the pH begins to fluctuate, the glycine can immediately induce weak change, and the change of the charges is generated, so that the change of the electrons is converted into released substances Son H + Thereby the pH is kept around 5.5, and NH is also caused 3 + Releasing protons H + The amino group after the reaction is subjected to the reverse reaction of conjugate acid-base pair reaction, so that H + Further, glycine is converted into electron-accepting material to convert excessive H + Continue to store and wait for the next change.
Catechin is a broad-spectrum antibacterial drug, the antibacterial capacity and concentration of which are positively correlated, and the antibacterial characteristics of catechin mainly comprise: the antibacterial spectrum is wide, and the antibacterial composition has obvious inhibition effect on gram-positive bacteria and gram-negative bacteria; the antibacterial effect is strong, and the drug concentration is low; protecting and promoting beneficial bacteria growth, and regulating flora balance; and the bacteria are not easy to generate drug resistance. In addition, catechin has better selectivity on the action of microorganisms.
The bamboo charcoal contains mineral components such as potassium, calcium, sodium, etc., has effect of enhancing immunity, and can adsorb tiny particles. The bamboo charcoal has hexagonal molecular structure, hard texture, fine porosity, adsorption function and weak conductivity. Therefore, bamboo charcoal has been used in various fields in the form of bamboo charcoal powder as a substance for adsorbing, removing dust, filtering and purifying air. However, the bamboo charcoal activated by the bamboo vinegar adopted by the invention is matched with the polyphenol liquid in the sterilization and deodorization liquid applied by the bamboo charcoal, and the interaction can remove the irritation of the bamboo vinegar, so that the whole bamboo charcoal is mild and has no irritation, and the bamboo charcoal can be directly applied to skin. On the other hand, the bamboo charcoal liquid can also enhance the stability of catechin, and the effect is multiplied after the bamboo charcoal liquid is fused with catechin, so that the overall excellent disinfection and sterilization effects can be excited, the overall excellent disinfection and deodorization effects are realized, and the bamboo charcoal liquid plays an extremely strong adsorption function and rapidly adsorbs odor sources.
The catechin, the bamboo charcoal liquid and the active positive and negative granules are organically combined and mutually coordinated, so that the external-use catechin-based deodorant has excellent disinfecting and deodorizing effects, is non-irritating, does not need adding excessive components, increases the skin burden, is a novel disinfecting and deodorizing agent which can be applied to the parts of eyes, nose, ears and the like at present, creates the external-use catechin-based disinfecting range, and is used for disinfecting oral and nasal, eyes and oral mucosa.
Through the technical scheme, compared with the prior art, the invention has the following beneficial effects:
1. the invention utilizes the amphoteric characteristic of glutamic acid and lysine to respectively react with spherical sodium montmorillonite to prepare active positive charge particles and active negative charge particles, and the active positive and negative charge particles are used as antioxidant protection liquid. Meanwhile, the preparation method of the polyphenol liquid is also provided, catechin in the liquid is in dynamic balance, so that the stability of the catechin in an aqueous solution is improved, and the catechin has at least 90% of activity after being stored for one year at normal temperature.
2. The bamboo charcoal activated by the bamboo vinegar adopted by the invention is matched with the polyphenol liquid in the sterilization and deodorization liquid applied by the bamboo charcoal, and the interaction can remove the irritation of the bamboo vinegar, so that the bamboo charcoal is mild and has no irritation on the whole body, and can be directly applied to the skin. On the other hand, the bamboo charcoal liquid can also enhance the stability of catechin, and the effect is multiplied after the bamboo charcoal liquid is fused with catechin, so that the overall excellent disinfection and sterilization effects can be excited, the overall excellent disinfection and deodorization effects are realized, and the bamboo charcoal liquid plays an extremely strong adsorption function and rapidly adsorbs odor sources.
3. The polyphenol liquid prepared by the invention has broad-spectrum antibacterial effect under the synergistic effect of all the components, is used for medical sterilization and disinfection, and is used for preparing the external skin sterilization and disinfection agent for killing bacteria, fungi or viruses. And can rapidly respond to a variety of bacteria and fungi: the escherichia coli, staphylococcus aureus, bacillus subtilis, aspergillus and sweat form tinea alba are killed, the sterilization effect is strong, and the sterilization rate reaches about 90%; and can rapidly kill influenza virus, mumps virus, measles virus and eczema virus. The invention is prepared from pure natural raw materials, has no residue to human body, is safe and green, and has the advantages of wide raw material sources, simple preparation, low cost, economy and environmental protection.
4. Through the organic combination of catechin, bamboo charcoal liquid and active positive and negative charge particles, the three components are mutually coordinated, so that the deodorant has lasting disinfection and deodorization effects, is non-irritating, creates a novel disinfection and deodorization liquid form, and can be used for disinfecting oral mucosa, nose, eyes and oral mucosa.
5. The polyphenol liquid can be used in various fields, and is suitable for sterilizing and disinfecting the surfaces of objects in hospitals, riding vehicles and densely populated environments.
Drawings
FIG. 1 is a graph showing the content of catechin active ingredient in example 1 stored at 25℃for 1 year;
fig. 2 is a graph showing the effect of the polyphenol liquid of example 1 on the face before and after sterilization by the customer.
Detailed Description
The invention is further described below in conjunction with the detailed description. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Further, it is understood that various changes and modifications may be made by those skilled in the art after reading the teachings of the present invention, and such equivalents are intended to fall within the scope of the appended claims.
Example 1
The preparation of polyphenol liquid for sterilization, disinfection and deodorization firstly needs to prepare antioxidant protection liquid, and the preparation method comprises the following steps:
Selecting spherical sodium montmorillonite with average nanometer diameter of 10nm, adding 3% spherical sodium montmorillonite into deionized water, adding hydrochloric acid, stirring to disperse sodium montmorillonite in hydrochloric acid dilute solution thoroughly, heating to 60deg.C, adding 9% glutamic acid, stirring thoroughly, reacting for 2 hr to obtain montmorillonite suspension, taking out the suspension, centrifuging at 3500rpm, washing with deionized water for 3 times to remove hydrochloric acid, centrifuging, taking out bottom solid mixture, oven drying at 60deg.C, and grinding to obtain COO as inner layer - A group, the outer layer is NH 3 + Proton spherical montmorillonite, marked as active positive charge pellet;
then selecting spherical sodium montmorillonite with average nanometer diameter of 10nm, and placing in a reaction kettleAdding 3% nanometer spherical sodium montmorillonite into deionized water, adding sodium carbonate, stirring to obtain pH value of 9.0, dispersing spherical sodium montmorillonite in alkali solution, adding 9% lysine, stirring, reacting for 2 hr to obtain montmorillonite suspension, taking out suspension, centrifuging at 3500rpm, washing with deionized water for 3 times to remove sodium carbonate, centrifuging, taking out bottom solid mixture, oven drying at 60deg.C, and grinding to obtain inner layer of NH 3 + Proton, with COO as outer layer - The spherical montmorillonite of the group is marked as an active negative charge particle;
adding 3% of bamboo vinegar and deionized water into a reaction kettle, uniformly stirring, and adding 3% of active positive charge particles to fully disperse the active positive charge particles in the bamboo vinegar solution, wherein the pH value is 5.5. Stirring and reacting for 2 hours, and taking out the mixed solution at the moment to obtain phase A of the antioxidant protection solution;
adding 2% of active negative charge particles into a reaction kettle, adding deionized water, fully dispersing, and taking out the obtained mixed solution to obtain the phase B of the antioxidant protection solution.
Then extracting green tea at low temperature by using ultrasonic wave, which comprises the following steps:
cleaning 200g of green tea, freeze-drying, and pulverizing to obtain pulverized mixture; adding an antioxidant protection liquid A phase with the mass 3 times of that of the mixture into the crushed mixture, extracting in an ultrasonic extractor at the temperature of 5 ℃, stirring uniformly, standing for 60 minutes, and filtering with a 800-mesh filter screen to obtain a first-stage extraction liquid and a first-stage filter residue for later use;
adding 3 times of antioxidant protective solution A phase into the first-stage filter residue, placing into an ultrasonic extractor at 5 ℃ for secondary extraction, stirring uniformly, standing for 60 minutes, and filtering with a 800-mesh filter screen to obtain second-stage extract and second-stage filter residue;
Mixing the second-stage extract and the first-stage extract to obtain a third extract, and stirring at 5 deg.C; concentrating the third extractive solution at 5deg.C under vacuum degree-0.1 Mpa at low temperature to remove 50% water to obtain catechin extractive solution;
the ultrasonic power was 50W and the extraction time was 1 hour.
Finally, the preparation method of the polyphenol liquid comprises the following steps:
grinding 20% of bamboo charcoal powder, sieving with 800 mesh sieve, soaking in 8% of bamboo vinegar water solution for 10 hr, and activating to obtain bamboo charcoal liquid.
Placing 40% catechin extraction solution and 10% oxidation-resistant protection solution B phase into a reaction kettle, uniformly stirring at a speed of 100r/min, adding 1.5% panthenol, uniformly stirring at a speed of 400r/min, dropwise adding 4% glycine, uniformly stirring at a speed of 100r/min after the dropwise adding is finished, reacting for 1 hour, adding 3% bamboo charcoal solution, uniformly stirring at a speed of 100r/min, reacting for 1 hour, and standing for 1 hour at a pH of 5.6; and finally adding 2.0% of glycerin, 4.0% of neroli hydrosol and the balance of deionized water, and uniformly stirring to obtain polyphenol liquid.
The method for measuring the mass concentration of the tea polyphenol is improved according to Guo Ziyu and the like in the detection method of the content of the tea polyphenol and catechin in tea according to GB-T8313-2008 recorded in the chemical stability of the tea polyphenol and attenuation dynamics study of the tea polyphenol in the disinfection process. Preparing a solution of which the mass fraction is 10 percent of Fu Lin Fen and the mass fraction is 7.5 percent of Na 2 CO 3 And preparing catechin working solution by using the catechin mother solution. And (3) measuring the absorbance of catechin by using a DR6000 ultraviolet visible spectrophotometer and a 10mm quartz cuvette and setting a single wavelength of 765nm, and determining the mass concentration of the catechin solution by using a standard curve. The change in concentration of catechin in the polyphenol liquid over time in example 1 was measured by a standard curve. As can be seen from FIG. 1, the change of the concentration of the aqueous polyphenol solution at the room temperature of 25 ℃ has a good linear relationship with the change of time, and still accords with a first-order kinetic formula. However, under the protection of the antioxidant protective liquid, the stability is greatly improved, the lasting activity can be maintained, and 90.6% of active ingredients still exist after the storage for 1 year, so that the quality assurance is provided for the sterilization and disinfection effects of the polyphenol aqueous solution, and the quality of the polyphenol aqueous solution is improved.
Example 2
The preparation of polyphenol liquid for sterilization, disinfection and deodorization firstly needs to prepare antioxidant protection liquid, and the preparation method comprises the following steps:
selecting spherical sodium montmorillonite with average nanometer diameter of 30nm, adding 1% spherical sodium montmorillonite into deionized water, adding hydrochloric acid, stirring to make sodium montmorillonite fully dispersed in hydrochloric acid dilute solution, and making pH value be 3.5, heating to 60 deg.C, adding 8% glutamic acid, stirring fully, reacting for 1 hr to obtain montmorillonite suspension, taking out suspension, centrifugal separating at 3500rpm, washing with deionized water for 3 times to remove hydrochloric acid, centrifugal separating, taking out bottom solid mixture, oven drying at 60 deg.C, grinding to obtain inner layer COO - A group, the outer layer is NH 3 + Proton spherical montmorillonite, marked as active positive charge pellet;
then selecting spherical sodium montmorillonite with average nano diameter of 30nm, adding deionized water into 1% spherical nano sodium montmorillonite in a reaction kettle, adding sodium carbonate, stirring uniformly to make pH value be 9.5, making sodium montmorillonite fully disperse in alkali solution, continuously adding 8% lysine, fully stirring, reacting for 1 hr to obtain montmorillonite suspension, taking out the suspension, centrifugal separating at 3500rpm, washing 3 times with deionized water to remove sodium carbonate, centrifugal separating, taking out solid mixture at bottom, drying and grinding at 60 deg.C to obtain inner layer of NH 3 + Proton, with COO as outer layer - The spherical montmorillonite of the group is marked as an active negative charge aggregate;
then adding 4% of bamboo vinegar and deionized water into a reaction kettle, uniformly stirring, and then adding 5% of active positive charge particles to fully disperse the active positive charge particles in the bamboo vinegar solution, wherein the pH value is 5.6. Stirring and reacting for 1 hour, and taking out the obtained mixed solution to obtain phase A of the antioxidant protection solution;
adding 4% active negative charge particles into a reaction kettle, adding deionized water, fully dispersing, and taking out the obtained mixed solution to obtain the phase B of the antioxidant protection solution.
Then extracting green tea at low temperature by using ultrasonic wave, which comprises the following steps:
cleaning 200g of green tea, freeze-drying, and pulverizing to obtain pulverized mixture; adding an antioxidant protection liquid A phase with the mass 2 times of that of the mixture into the crushed mixture, extracting in an ultrasonic extractor at the temperature of 8 ℃, stirring uniformly, standing for 60 minutes for reaction, and filtering with a 800-mesh filter screen to obtain a first-stage extraction liquid and first-stage filter residues for later use;
adding 2 times of antioxidant protective solution A phase into the first-stage filter residue, placing into an ultrasonic extractor at 8 ℃ for secondary extraction, stirring uniformly, standing for 60 minutes, and filtering with a 800-mesh filter screen to obtain second-stage extract and second-stage filter residue;
mixing the second-stage extract and the first-stage extract to obtain a third extract, and stirring at 8deg.C; concentrating the third extractive solution at 5deg.C under vacuum degree-0.1 Mpa at low temperature to remove 50% water to obtain catechin extractive solution;
the ultrasonic power was 80W and the extraction time was 1 hour.
Finally, the preparation method of the polyphenol liquid comprises the following steps:
grinding 20% of bamboo charcoal powder, sieving with 800 mesh sieve, soaking in 10% of bamboo vinegar water solution for 10 hr, and activating to obtain bamboo charcoal liquid.
Placing 20% catechin extraction solution and 5% antioxidant protection solution B phase into a reaction kettle, and uniformly stirring at a speed of 100 r/min; adding 1.0% of panthenol, stirring at the speed of 500r/min, dripping 3% of glycine, fully stirring uniformly, stirring uniformly at the speed of 200r/min after dripping, reacting for 1 hour, adding 4% of bamboo charcoal liquid, stirring uniformly at the speed of 200r/min, reacting for 1 hour, and standing for 1 hour at the pH of 5.5; and finally adding 3.0% of glycerol, 5.0% of neroli hydrolat and the balance of deionized water, and uniformly stirring to obtain polyphenol liquid.
Example 3
The preparation of polyphenol liquid for sterilization, disinfection and deodorization firstly needs to prepare antioxidant protection liquid, and the preparation method comprises the following steps:
selecting spherical sodium montmorillonite with average nanometer diameter of 20nm, adding 2% spherical sodium montmorillonite into deionized water, adding hydrochloric acid, stirring to disperse sodium montmorillonite in hydrochloric acid dilute solution thoroughly, making pH value 3.5, adding 6% glutamic acid, stirring thoroughly, reacting for 1 hr to obtain montmorillonite suspension, taking out suspension, centrifuging at 3500rpm, washing with deionized water for 3 times to remove hydrochloric acid, centrifuging, taking out bottom solid mixture, oven drying at 60deg.C, grinding to obtain inner layer COO - A group, the outer layer is NH 3 + Proton spherical montmorillonite, marked as active positive charge pellet;
then selecting spherical sodium montmorillonite with average nano diameter of 20nm, adding deionized water into 2% spherical nano sodium montmorillonite in a reaction kettle, adding sodium carbonate, stirring uniformly to make pH value be 9.5, making sodium montmorillonite fully disperse in alkali solution, continuously adding 6% lysine, fully stirring, reacting for 1 hr to obtain montmorillonite suspension, taking out suspension, centrifugal separating at 3500rpm, washing 3 times with deionized water to remove sodium carbonate, centrifugal separating, taking out solid mixture at bottom, drying and grinding at 60 deg.C to obtain inner layer of NH 3 + Proton, with COO as outer layer - The spherical montmorillonite of the group is marked as an active negative charge particle;
then adding 5% of bamboo vinegar and deionized water into a reaction kettle, uniformly stirring, and adding 5% of active positive charge particles to fully disperse the active positive charge particles in the bamboo vinegar solution, wherein the pH value is 5.5. Stirring and reacting for 1 hour, and taking out the obtained mixed solution to obtain phase A of the antioxidant protection solution;
adding 3% active negative charge particles into a reaction kettle, adding deionized water, fully dispersing, and taking out the obtained mixed solution to obtain the phase B of the antioxidant protection solution.
Then extracting green tea at low temperature by using ultrasonic wave, which comprises the following steps:
cleaning 200g of green tea, freeze-drying, and pulverizing to obtain pulverized mixture; adding an antioxidant protection liquid A phase with the mass 2 times of that of the mixture into the crushed mixture, extracting in an ultrasonic extractor at the temperature of 8 ℃, stirring uniformly, standing for 60 minutes for reaction, and filtering with a 800-mesh filter screen to obtain a first-stage extraction liquid and first-stage filter residues for later use;
adding 2 times of antioxidant protective solution A phase into the first-stage filter residue, placing into an ultrasonic extractor at 8 ℃ for secondary extraction, stirring uniformly, standing for 60 minutes, and filtering with a 800-mesh filter screen to obtain second-stage extract and second-stage filter residue;
mixing the second-stage extract and the first-stage extract to obtain a third extract, and stirring at 8deg.C; concentrating the third extractive solution at 5deg.C under vacuum degree-0.1 Mpa at low temperature to remove 50% water to obtain catechin extractive solution;
the ultrasonic power was 80W and the extraction time was 1 hour.
Finally, the preparation method of the polyphenol liquid comprises the following steps:
grinding 20% of bamboo charcoal powder, sieving with 800 mesh sieve, soaking in 10% of bamboo vinegar water solution for 10 hr, and activating to obtain bamboo charcoal liquid.
Placing 30% catechin extract and 8% antioxidant protective solution B phase into a reaction kettle, and uniformly stirring at a speed of 100 r/min; adding 2.0% of panthenol, adopting a speed of 500r/min to stir at a high speed, dripping 3% of glycine, uniformly stirring, adopting a speed of 200r/min to stir uniformly after dripping, reacting for 1 hour, adding 4% of bamboo charcoal liquid, adopting a speed of 200r/min to stir uniformly, and reacting for 1 hour with a pH value of 5.6;
standing for 1 hour; finally adding 5.0% of glycerin, 4.0% of neroli hydrosol and the balance of deionized water, and uniformly stirring to obtain polyphenol liquid.
Comparative example 1: equivalent amount of antioxidant protection liquid A was replaced with deionized water, equivalent amount of antioxidant protection liquid B was replaced with deionized water, otherwise the same as in example 1;
comparative example 2: the same procedure as in example 1 was followed except that the antioxidant protective solution A phase was not added and was replaced with equal amount of deionized water;
comparative example 3: the same procedure as in example 1 was followed except that the anti-oxidant protective solution B phase was not added and was replaced with equal amount of deionized water;
comparative example 4: the product of example 7 in a tea polyphenol hand sanitizer disclosed in chinese patent publication No. CN114209635 a;
comparative example 5: the model of the polyphenol sterilizing disinfectant on the latest date sold in the market is the compound tea polyphenol lotion of xiaoling.
The bactericidal effect of the polyphenol liquid on 9 strains of escherichia coli, staphylococcus aureus, candida albicans, bacillus subtilis, trichophyton, aspergillus, gram-negative bacteria, gram-positive bacteria and tinea alba sweaty was verified by an oxford cup method according to examples 1-3 and comparative examples 1-3 which are just prepared. Inoculating test strains on a test tube slant culture medium under aseptic conditions, placing the test strains in a constant temperature incubator at 37 ℃ for culturing for 20 hours, adding sterile distilled water, dissolving, oscillating to form a suspension, heating and melting the sterile solid culture medium, pouring the suspension into a sterile culture dish, respectively adding 15ml of the prepared suspension, slightly shaking uniformly, placing sterile oxford cups on plates containing each strain rapidly, respectively injecting 20ml of polyphenol liquid of examples 1-3 and comparative examples 1-3 into each plate, culturing for 20 hours at 37 ℃, observing sterilization conditions, measuring the diameter of a bacteriostasis ring generated by each strain, measuring 3 times for each bacteriostasis ring, repeating 3 times for each concentration, and taking an average value. The results are shown in Table 1,
the polyphenol liquids prepared in examples 1 to 3 and comparative examples 1 to 3 were left at 50℃for 30 days, and then the sterilizing effect of these 9 strains was again tested by the oxford cup method, as shown in Table 2;
TABLE 1 Sterilization effect of polyphenol liquid on different strains 1 (diameter of inhibition zone mm)
TABLE 2 Sterilization effect of polyphenol liquid on different strains 2 (diameter of inhibition zone mm)
| Bacterial strain | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Coli bacterium | 22.1 | 18.5 | 22.1 | 9.1 | 10.2 | 9.3 |
| Staphylococcus aureus | 21.5 | 17.7 | 20.7 | 9.0 | 11.3 | 9.1 |
| Candida albicans | 19.0 | 15.7 | 18.8 | 8.5 | 10.9 | 8.8 |
| Bacillus subtilis | 21.8 | 18.9 | 22.0 | 8.7 | 9.6 | 8.9 |
| Trichophyton mentagrophytes | 19.5 | 17.0 | 19.2 | 6.9 | 10.1 | 7.5 |
| Aspergillus | 19.2 | 17.5 | 18.9 | 8.2 | 9.5 | 8.9 |
| Gram-negative bacteria | 19.5 | 15.9 | 18.7 | 7.5 | 10.1 | 8.1 |
| Gram-positive bacteria | 18.2 | 14.1 | 17.5 | 6.8 | 10.6 | 9.2 |
| Sweat-like tinea alba | 19.4 | 15.8 | 19.1 | 7.1 | 11.0 | 8.9 |
As can be seen from Table 1, the polyphenol solution has different degrees of inhibition on the 9 strains, and the inhibition on the escherichia coli by the polyphenol solution under the same concentration is the best, and presumably the reasons for the inhibition are related to the types of the strains, the growing pH, the selectivity of the polyphenol solution on the bacteria inhibition of microorganisms and the like; in addition, as the concentration ratio of the polyphenol solution increases, the antibacterial effect is enhanced. Especially, when the phase A of the antioxidant protective liquid is added in the extraction process, the antibacterial effect is obviously better than that of the comparative example 1 without the phase A of the antioxidant protective liquid. In conclusion, the polyphenol solution has a certain inhibition effect on common bacteria and fungi of foods, the stronger the inhibition effect is along with the increase of the concentration, and the antioxidation protection liquid can effectively protect the activity of catechin, so that the catechin is not oxidized in the extraction process. As can be seen from the antibacterial effects of tables 1 and 2, after the anti-oxidation protective liquid B phase is added, the A phase and the B phase interact in the storage process of the polyphenol liquid, so that the activity of phenolic hydroxyl groups in the polyphenol liquid is stable, the activity of the polyphenol liquid can be continuously maintained in the storage process, and the sterilizing and antibacterial effects are maintained.
The sterilization rate test is carried out on the polyphenol liquid by referring to an annex C of the sanitary Standard of the disposable sanitary products of GB15979-2002 and a test method of the sterilization performance, the bacteriostasis performance and the stability of the product, the action time is 5 minutes, the sterilization rate is tested according to a data table, the polyphenol liquid is placed at the constant temperature of 50 ℃ for 1 month, the sterilization rate test is carried out, the result is shown in a table 3, and the sterilization rate is shown in a table 4 after being placed at the temperature of 50 ℃ for 6 months.
TABLE 3 results 1 of sterilization rate test (sterilization rate%)
| Bacterial strain | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 |
| Coli bacterium | 99.1 | 96.3 | 98.5 | 30.8 | 50.1 | 30.5 | 45.2 | 53.8 |
| Staphylococcus aureus | 98.8 | 97.5 | 98.6 | 29.5 | 49.9 | 29.9 | 42.5 | 49.7 |
| Candida albicans | 90.5 | 89.3 | 90.4 | 8.5 | 48.7 | 8.6 | 41.3 | 51.3 |
| Bacillus subtilis | 98.3 | 95.1 | 98.3 | 27.9 | 47.4 | 30.5 | 45.9 | 57.1 |
| Trichophyton mentagrophytes | 89.7 | 87.2 | 89.5 | 18.9 | 48.3 | 21.9 | 28.8 | 47.1 |
| Aspergillus | 92.1 | 90.9 | 91.8 | 14.8 | 44.2 | 19.1 | 30.5 | 48.9 |
| Gram-negative bacteria | 85.4 | 82.8 | 85.4 | 14.8 | 34.0 | 18.5 | 28.7 | 44.7 |
| Gram-positive bacteria | 88.1 | 86.7 | 87.8 | 11.3 | 31.5 | 11.5 | 32.9 | 41.5 |
| Sweat-like tinea alba | 90.4 | 88.1 | 90.1 | 15.9 | 45.4 | 16.3 | 39.1 | 48.0 |
TABLE 4 results of sterilization test 2 (percent sterilization)
| Bacterial strain | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 |
| Coli bacterium | 90.1 | 86.0 | 87.4 | 11.9 | 38.1 | 18.7 | 13.3 | 25.1 |
| Staphylococcus aureus | 88.2 | 81.9 | 88.6 | 14.8 | 30.9 | 21.6 | 18.5 | 22.7 |
| Candida albicans | 79.9 | 89.3 | 78.1 | - | 28.5 | - | - | - |
| Bacillus subtilis | 78.1 | 75.4 | 77.3 | 8.7 | 37.6 | 33.8 | 15.3 | 21.8 |
| Trichophyton mentagrophytes | 74.4 | 67.2 | 72.5 | - | 21.3 | - | - | - |
| Aspergillus | 78.7 | 73.9 | 76.4 | - | 25.4 | - | - | - |
| Gram-negative bacteria | 72.5 | 70.8 | 71.9 | - | 19.7 | - | - | - |
| Gram-positive bacteria | 78.3 | 76.1 | 77.8 | - | 18.9 | - | - | - |
| Sweat-like tinea alba | 75.6 | 68.5 | 74.9 | - | 21.3 | - | - | - |
As shown in the results of tables 3-4, the polyphenol liquid for sterilization, disinfection and deodorization has high-efficiency sterilization performance and extremely high sterilization effects on bacteria and fungi; as is clear from comparative examples 1 and 2, the absence of the antioxidant protective liquid A causes a loss of a certain activity of phenolic hydroxyl groups during the extraction process, so that the sterilization effect is reduced. As is clear from comparative examples 1 and 3, the anti-oxidation protective liquid B phase is not added, the sterilizing effect of the polyphenol liquid is gradually lost in the storage process, especially after the high-temperature storage time exceeds 6 months, the sterilizing effect of the polyphenol liquid on bacteria is rapidly reduced, and the effect on fungi is basically lost, so that the anti-oxidation protective liquid is the combined action of the A phase and the B phase, can protect the polyphenol liquid in the extraction and storage processes, maintain good stability, permanently maintain the sterilizing capability of phenolic hydroxyl groups, has spectral effect on various strains, and has good sterilizing effect. For human body disinfection, the commercial similar products are basically weak acid, and the sterilizing effect of the weak acid products on fungus is basically zero after catechin loses activity.
Finally, it should be noted that the above-mentioned embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (8)
1. A preparation method of polyphenol liquid for sterilization, disinfection and deodorization is characterized by comprising the following steps: the sterilizing, disinfecting and deodorizing polyphenol liquid comprises the following substances in percentage by mass: 20 to 40 percent of catechin extracting solution, 5 to 10 percent of anti-oxidation protective solution B phase, 2.0 to 4.0 percent of glycine, 2.0 to 5.0 percent of neroli hydrosol, 0.5 to 2.0 percent of panthenol, 2.0 to 5.0 percent of glycerol, 3.0 to 6.0 percent of bamboo charcoal solution and the balance of deionized water;
the catechin extracting solution is obtained by adopting an oxidation-resistant protective solution A phase to perform ultrasonic low-temperature extraction;
the catechin extract comprises epigallocatechin gallate and epigallocatechin, and has antibacterial and disinfectant effects.
2. The method for preparing the polyphenol liquid for sterilization, disinfection and deodorization according to claim 1, which is characterized in that: the catechin extracting solution is extracted from green tea, and the extracting method is an ultrasonic low-temperature extracting method and comprises the following steps:
S101, cleaning tea leaves, freeze-drying and then crushing to obtain a crushed mixture;
s102, adding an antioxidant protection liquid A phase with the mass 1-3 times of that of the mixture into the crushed mixture, extracting in an ultrasonic extractor at the temperature of 5-10 ℃, uniformly stirring, standing for reaction for 40-60 minutes, and filtering by a filter screen with 800 meshes to obtain a first-stage extraction liquid and first-stage filter residues for later use;
s103, adding 1-3 times of antioxidant protection liquid A phase into the first-stage filter residue in the step S102, placing the filter residue in an ultrasonic extractor for secondary extraction at the temperature of 5-10 ℃, stirring uniformly, standing for reaction for 40-60 minutes, and filtering by a 800-mesh filter screen to obtain second-stage extract and second-stage filter residue;
s104, mixing the second-stage extracting solution and the first-stage extracting solution to obtain a third extracting solution, and fully stirring at the temperature of 5-10 ℃; concentrating the third extract at a temperature of 5-10 ℃ and a vacuum degree of-0.09 to-0.1 Mpa under low temperature and vacuum to remove 50% of water to obtain catechin extract;
the ultrasonic power is 50-100W, and the extraction time is 1-2 h.
3. The method for preparing the polyphenol liquid for sterilization, disinfection and deodorization according to claim 1, which is characterized in that: the preparation method of the antioxidant protection liquid specifically comprises the following steps:
S001, selecting spherical sodium montmorillonite with nanometer diameter of 10-30 nm, adding deionized water into the spherical sodium montmorillonite, adding hydrochloric acid, stirring uniformly to ensure that the pH value is 3.2-3.8, fully dispersing the sodium montmorillonite in hydrochloric acid dilute solution, heating to 60 ℃, adding glutamic acid, fully stirring, reacting for 1-2 hours to obtain a montmorillonite suspension, taking out the suspension, centrifugally separating at 3500rpm, washing with deionized water for 2-3 times to remove hydrochloric acid, centrifugally separating, taking out a solid mixture at the bottom, drying and grinding at 60 ℃ to obtain COO as an inner layer - A group, the outer layer is NH 3 + Proton spherical montmorillonite, marked as active positive charge pellet;
the mass percentage of the spherical sodium-based montmorillonite is 1-3%, and the mass ratio of the spherical sodium-based montmorillonite to the glutamic acid is 1:3-8;
s002, selecting spherical sodium montmorillonite with nanometer diameter of 10-30 nm, adding deionized water into the spherical sodium montmorillonite, adding sodium carbonate, stirring uniformly to make pH value be 9.0-9.5, making sodium montmorillonite fully disperse in alkali solution, continuously adding lysine, fully stirring, reacting for 1-2 hr to obtain montmorillonite suspension, taking out suspension, centrifugal separating at 3500rpm, washing 2-3 times with deionized water to remove sodium carbonate, centrifugal separating, taking out bottom solid mixture, drying and grinding at 60 deg.C to obtain inner layer of NH 3 + Proton, with COO as outer layer - Radicals (C)Is marked as active negative charge pellet;
the mass percentage of the spherical sodium-based montmorillonite is 1-3%, and the mass ratio of the spherical sodium-based montmorillonite to lysine is 1:3-8;
s003, adding bamboo vinegar and deionized water into a reaction kettle, uniformly stirring, and then adding active positive charge particles to enable the active positive charge particles to be fully dispersed in a bamboo vinegar solution, wherein the pH value is 5.5-6.0; stirring and reacting for 1-2 hours, and taking out the mixed solution to obtain a phase A of the antioxidant protection solution; the mass percentage of the bamboo vinegar is 3-5%, and the active positive charge grain mass is 3-5%;
s004, adding deionized water into a reaction kettle, adding active negative charge particles, and fully dispersing to obtain a mixed solution which is the B phase of the antioxidant protection solution, wherein the active negative charge particles are 2-4%.
4. The method for preparing the polyphenol liquid for sterilization, disinfection and deodorization according to claim 1, which is characterized in that: the bamboo charcoal liquid is obtained by grinding 20% of bamboo charcoal powder, sieving with 800 mesh sieve, soaking in 8-10% of bamboo vinegar water solution for 10-12 hours, and activating.
5. The method for preparing the polyphenol liquid for sterilization, disinfection and deodorization according to claim 1, which is characterized in that: the preparation method of the polyphenol liquid comprises the following steps:
S201, placing catechin extracting solution and anti-oxidation protective solution B phase into a reaction kettle, and uniformly stirring at 100-200 r/min;
s202, adding panthenol, stirring at 400-600 r/min, dripping glycine, stirring uniformly, stirring at 100-200 r/min after dripping, reacting for 1-2 hours, adding bamboo charcoal liquid, stirring at 100-200 r/min, reacting for 1-2 hours, adjusting pH to 5.5-5.6, and standing for 1-2 hours;
and S203, finally adding glycerol, the neroli hydrosol and the balance of deionized water, and uniformly stirring to obtain polyphenol liquid.
6. The method for producing a polyphenol liquid for sterilization, disinfection and deodorization according to any one of claims 1 to 5, characterized in that: the polyphenol liquid is used for medical sterilization and disinfection and is used for preparing an external skin sterilization and disinfection agent for killing bacteria, fungi or viruses.
7. The method for preparing the polyphenol liquid for sterilization, disinfection and deodorization according to claim 6, wherein: the polyphenol liquid is sprayed on the surface of the skin to form a protective film.
8. The method for preparing the polyphenol liquid for sterilization, disinfection and deodorization according to claim 6, wherein: the bacteria or fungi are Escherichia coli, staphylococcus aureus, bacillus subtilis, aspergillus and tinea alba.
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| CN102813955A (en) * | 2012-08-17 | 2012-12-12 | 天津市中科健新材料技术有限公司 | Absorbent product containing tea polyphenol deodorization composition |
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| CN102813955A (en) * | 2012-08-17 | 2012-12-12 | 天津市中科健新材料技术有限公司 | Absorbent product containing tea polyphenol deodorization composition |
| CN104726994A (en) * | 2014-12-26 | 2015-06-24 | 安徽省中日农业环保科技有限公司 | Catechinic acid fiber blended deodorization flame-retardant woven fabric and manufacturing method thereof |
| CN110623937A (en) * | 2018-06-21 | 2019-12-31 | 四川大学 | Tea polyphenol-based multifunctional nano-composite as well as preparation method and application thereof |
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