Disinfectant containing supermolecule silver and preparation method thereof
阅读说明：本技术 一种含超分子银的消毒剂及其制备方法 (Disinfectant containing supermolecule silver and preparation method thereof ) 是由 韩兴帅 袁伏中 于 2021-01-13 设计创作，主要内容包括：本发明公开了一种含超分子银的消毒剂及其制备方法,涉及化学消毒剂技术领域。本发明提供的含超分子银的消毒剂,其结构式为Ag-xR-yS-Z；式中,x＝1或2或3；y＝1或2；z＝3；其中,Ag为一价银离子Ag～+或二价银离子Ag～(++)；R选自甘氨酸,谷氨酸,天门冬氨酸,乳酸,柠檬酸,苹果酸,醋酸,乙醇酸中的任意一种；S选自水分子或双氧水分子。本发明利用有机酸将银离子与水分子或过氧化氢分子相结合,银离子能够催化水或过氧化氢产生活性羟基自由基,提高其杀菌效率；该含超分子银的消毒剂能够在接触病原微生物时相互促进,杀菌谱更广,杀菌速度更快。(The invention discloses a disinfectant containing supramolecular silver and a preparation method thereof, and relates to the technical field of chemical disinfectants. The disinfectant containing supermolecule silver provided by the invention has a structural formula of Ag x R y S Z (ii) a Wherein x is 1 or 2 or 3; y is 1 or 2; z is 3; wherein Ag is monovalent silver ion Ag + Or divalent silver ion Ag ++ (ii) a R is selected from any one of glycine, glutamic acid, aspartic acid, lactic acid, citric acid, malic acid, acetic acid and glycolic acid; s is selected from water molecules or hydrogen peroxide molecules. The invention combines silver ions with water molecules or hydrogen peroxide molecules by using organic acid, and the silver ions can catalyze water or hydrogen peroxide to generate active hydroxyl radicals, thereby improving the yield of the productThe sterilization efficiency is improved; the disinfectant containing the supermolecule silver can promote each other when contacting pathogenic microorganisms, and has the advantages of wider sterilization spectrum and higher sterilization speed.)
1. The disinfectant containing supermolecule silver is characterized in that the structural formula of the disinfectant is AgxRySZ；
Wherein x is 1 or 2 or 3; y is 1 or 2; z is 3;
wherein Ag is monovalent silver ion Ag+Or divalent silver ion Ag++；
R is selected from any one of glycine, glutamic acid, aspartic acid, lactic acid, citric acid, malic acid, acetic acid and glycolic acid;
s is selected from water molecules or hydrogen peroxide molecules.
2. The supramolecular silver-containing disinfectant as claimed in claim 1, selected from any one of the compounds represented by the following structural formula:
formula I: ag+ xRy(H2O2)Z(ii) a Wherein x is 1 or 2 or 3; y is 1; z is 3;
formula II: ag++ xRy(H2O2)Z(ii) a Wherein x is 1 or 3; y is 1 or 2; z is 3;
formula IIII: ag++ xRy(H2O)Z(ii) a Wherein x is 1 or 3; y is 1 or 2; and z is 3.
3. The supramolecular silver-containing disinfectant as claimed in claim 1, wherein R is selected from any one of glutamic acid, aspartic acid, glycolic acid, citric acid.
4. A process for the preparation of a disinfectant containing supramolecular silver, as claimed in any of claims 2-3, obtained by reacting substantially: silver oxide or silver peroxide, organic acid, distilled water or hydrogen peroxide;
wherein the molar ratio of the organic acid to the silver oxide or the silver peroxide is 1: 1-1: 3;
the molar ratio of the organic acid to the hydrogen peroxide is 1: 1-1: 10;
the mass of the organic acid is 0.1-10% of the mass of the distilled water;
the organic acid is any one of glycine, glutamic acid, aspartic acid, lactic acid, citric acid, malic acid, acetic acid and glycolic acid.
5. The method of preparing a disinfectant containing supramolecular silver as claimed in claim 4, comprising the steps of:
proportionally adding organic acid and hydrogen peroxide into a reaction vessel filled with distilled water, stirring at 50-80 ℃, adding silver oxide, and fully reacting to obtain the product, namely the disinfectant containing the supermolecule silver shown in the formula I.
6. The method of preparing a disinfectant containing supramolecular silver as claimed in claim 4, comprising the steps of:
proportionally adding organic acid and hydrogen peroxide into a reaction vessel filled with distilled water, stirring at 50-80 ℃, adding silver peroxide, and fully reacting to obtain a product, namely the disinfectant containing supramolecular silver shown in a formula II.
7. The method of preparing a disinfectant containing supramolecular silver as claimed in claim 4, comprising the steps of:
proportionally adding organic acid into a reaction vessel filled with distilled water, stirring at 50-80 ℃, adding silver peroxide, and fully reacting to obtain a product, namely the disinfectant containing supramolecular silver shown in formula IIII.
8. The method of preparing a disinfectant containing supramolecular silver as claimed in claim 4, wherein said organic acid is selected from any one of glutamic acid, aspartic acid, glycolic acid, citric acid.
9. The supramolecular silver-containing disinfectant as claimed in any of claims 1-3, for use in vitro disinfection of humans and animals, air disinfection in public places, disinfection of daily samples.
Technical Field
The invention relates to the technical field of chemical disinfectants, in particular to a disinfectant containing supermolecule silver and a preparation method thereof.
Background
The disinfectant is used for killing pathogenic microorganisms on a transmission medium, so that the requirement of harmlessness is met, the pathogenic microorganisms are killed out of a human body, the transmission path of infectious diseases is cut off, and the purpose of controlling the infectious diseases is achieved.
The disinfectant can be divided into a sterilizing agent, a high-efficiency disinfectant, a middle-efficiency disinfectant and a low-efficiency disinfectant according to the action level. The sterilizing agent can kill all microorganisms to meet the sterilizing requirement, and comprises formaldehyde, glutaraldehyde, ethylene oxide, peracetic acid, hydrogen peroxide, chlorine dioxide, chlorine, copper sulfate, quicklime, ethanol and the like. Therefore, disinfectants are also commonly referred to as "chemical disinfectants".
The hydrogen peroxide belongs to a high-efficiency sterilizing agent, has good killing effect on most of bacteria, fungi, viruses, spores, pathogenic ova, algae and other harmful organisms, has the excellent characteristics of low toxicity, easy decomposition, no residue and high environmental safety, and has become the main component of the current environment-friendly sterilizing agent. But the hydrogen peroxide disinfectant has poor stability at low concentration, is easy to decompose, has slow sterilization speed and short duration, so that a plurality of hydrogen peroxide disinfectant products are compounded with synergistic components to improve the sterilization speed and prolong the duration.
Silver ions are positively charged cations of silver atoms with loss of one or more electrons, e.g. Ag+、Ag2+、Ag3+And the like. Usually in the form of an aqueous solution, silver ions have an oxidizing action and are commonly used in daily life for sterilization, disinfection and the like.
The existing disinfectant containing silver ions mainly uses silver nitrate to provide silver ions, and nitrate radicals can remain after the disinfectant is used, so that potential safety hazards exist; in addition, the current silver ion disinfectant has the sterilization rate of about 85 percent when used for air disinfection, and low cost performance, thereby limiting the application of the silver ion disinfectant.
Disclosure of Invention
The technical problem to be solved by the invention is some defects mentioned in the background technology, and the invention provides a disinfectant containing supermolecule silver and a preparation method thereof.
In order to solve the above problems, the present invention proposes the following technical solutions:
disinfectant containing supermolecule silver, its structural formula is AgxRySZ；
Wherein x is 1 or 2 or 3; y is 1 or 2; z is 3;
wherein Ag is monovalent silver ion Ag+Or divalent silver ion Ag++；
R is selected from any one of glycine, glutamic acid, aspartic acid, lactic acid, citric acid, malic acid, acetic acid and glycolic acid;
s is selected from water molecules or hydrogen peroxide molecules.
The disinfectant containing the supermolecule silver is selected from any one of the compounds shown in the following structural formula:
formula I: ag+ xRy(H2O2)Z(ii) a Wherein x is 1 or 2 or 3; y is 1; z is 3;
formula II: ag++ xRy(H2O2)Z(ii) a Wherein x is 1 or 3; y is 1 or 2; z is 3;
formula IIII: ag++ xRy(H2O)Z(ii) a Wherein x is 1 or 3; y is 1 or 2; and z is 3.
The further technical proposal is that R is selected from any one of glutamic acid, aspartic acid, glycolic acid and citric acid.
The invention also provides a preparation method of the disinfectant containing the supermolecule silver, which is obtained by fully reacting the following components: silver oxide or silver peroxide, organic acid, distilled water or hydrogen peroxide;
wherein the molar ratio of the organic acid to the silver oxide or the silver peroxide is 1: 1-1: 3;
the molar ratio of the organic acid to the hydrogen peroxide is 1: 1-1: 10;
the mass of the organic acid is 0.1-10% of the mass of the distilled water;
the organic acid is any one of glycine, glutamic acid, aspartic acid, lactic acid, citric acid, malic acid, acetic acid and glycolic acid.
The further technical scheme is that the preparation method comprises the following steps:
proportionally adding organic acid and hydrogen peroxide into a reaction vessel filled with distilled water, stirring at 50-80 ℃, adding silver oxide, and fully reacting to obtain the product, namely the disinfectant containing the supermolecule silver shown in the formula I.
The further technical scheme is that the preparation method also comprises the following steps:
proportionally adding organic acid and hydrogen peroxide into a reaction vessel filled with distilled water, stirring at 50-80 ℃, adding silver peroxide, and fully reacting to obtain a product, namely the disinfectant containing supramolecular silver shown in a formula II.
The further technical scheme is that the preparation method also comprises the following steps:
proportionally adding organic acid into a reaction vessel filled with distilled water, stirring at 50-80 ℃, adding silver peroxide, and fully reacting to obtain a product, namely the disinfectant containing supramolecular silver shown in formula IIII.
The further technical proposal is that the organic acid is any one of glutamic acid, aspartic acid, glycolic acid and citric acid.
The disinfectant containing the supramolecular silver provided by the invention can be used for in-vitro disinfection of human and animals, air disinfection of public places and disinfection of daily samples.
Compared with the prior art, the invention can achieve the following technical effects: the disinfectant containing supramolecular silver provided by the invention has the functions which are not possessed by the traditional inorganic silver ion disinfectant (silver nitrate) or the traditional organic acid silver hydrate: the disinfectant does not contain harmful ions such as nitrate radical and the like, and is safer and more environment-friendly; the test proves that: the disinfectant has the activity 300-10000 times that of the traditional inorganic silver ion disinfectant (silver nitrate) or the traditional organic acid silver hydrate, and has high activity and small using amount.
According to the disinfectant containing supramolecular silver, silver ions are combined with water molecules or hydrogen peroxide molecules by using organic acid, and the silver ions can catalyze water or hydrogen peroxide to generate active hydroxyl radicals, so that the sterilization efficiency of the disinfectant is improved; the disinfectant containing the supermolecule silver can promote each other when contacting pathogenic microorganisms, and has the advantages of wider sterilization spectrum and higher sterilization speed.
Experiments prove that the disinfectant containing the supermolecule silver can be used for in-vitro disinfection of people and animals, air disinfection of public places and disinfection of daily supplies, and the disinfection and sterilization effect reaches 99.999%.
The preparation method of the disinfectant containing supramolecular silver provided by the invention is simple in steps and can realize quantitative production.
Detailed Description
The technical solutions in the examples will be clearly and completely described below. It is apparent that the embodiments to be described below are only a part of the embodiments of the present invention, and not all of them. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It will be understood that the terms "comprises" and/or "comprising," when used in this specification and the appended claims, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
It is also to be understood that the terminology used in the description of the embodiments of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the embodiments of the invention. As used in the description of embodiments of the present invention and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
Example 1
This example provides a disinfectant containing supramolecular silver selected from the group consisting of compounds represented by the following structural formula:
formula I: ag+ xRy(H2O2)Z(ii) a Wherein x is 2; y is 1; z is 3; through detection, the concentration of the hydrogen peroxide contained in the embodiment is 33.0g/L, and the proportion is 3% (w/w); the silver ion concentration is 14.4mg/L, and the occupation ratio is 0.0015% (w/w).
The disinfectant containing supramolecular silver of the present example was tested as follows:
1 materials and methods
1.1 materials
And (3) testing a sample: example 1, a colorless transparent liquid containing 3% (w/w) of hydrogen peroxide and 0.0015% (w/w) of silver ions, and having a pH of 2.86.
Test strains: coli (8099) cultured to the 8 th generation; staphylococcus aureus (ATCC6538), cultured to passage 7; candida albicans (ATCC10231) cultured up to passage 5, and the original strain was purchased from Kyork, Guangdong, Microscience, Inc.
Metal corrosion test piece: 4 metal sample sheets (round, diameter 24.0mm, thickness 1.0mm, small hole with diameter 2.0mm, total surface area 9.8017 cm)2And 4-6) of finish.
Neutralizing agent: D/E neutralization Broth +5g/LNa2S2O3。
Culture medium: and sterilizing the nutrient agar culture medium, the Sabouraud agar culture medium and the TSA (tryptone soy agar culture medium) by pressure steam for later use.
Organic interferents: 3% bovine serum albumin.
Diluting liquid: PBS buffer.
A subject: hand of worker of Zhongying science and technology Co., Ltd, plain white cotton cloth (5.0 cm. times.5.0 cm), table top, door, stainless steel plate surface, and cucumber surface (25 cm. times.5.0 cm) with uniform thickness2)
Sterile cotton swab: the disposable medical cotton swab is sterilized for later use.
Test animals: kunming mice, SPF grade, weight 25-30g, 50, half each of male and female, provided by the center of experimental animals in Henan province, and qualification number DW 2020040023; new Zealand white rabbits, normal grade, female 3, weigh about 2.5kg, supplied by Sian Dilep biomedical Co., Ltd, and have a certification number NO 2020022823.
1.2 methods
1.2.1 stability test
And placing the packed eight-cereal silver hydrogen peroxide silver ion disinfectant stock solution in a thermostat at 54 ℃ for 14 days. And respectively measuring the contents of hydrogen peroxide and silver ions of the samples before and after placement by adopting a chemical titration method, and calculating the reduction rate of the contents of the hydrogen peroxide and the silver ions.
1.2.2 acute oral toxicity test
According to the first-time limit method of acute oral toxicity test in disinfection technical specification (2002 edition), the environmental temperature is 20-24 ℃, the environmental humidity is: 40 to 70 percent. 5.0ml of the solution obtained in example 1 is taken and added with distilled water to a constant volume of 20ml and mixed evenly to be used as gastric perfusion fluid. 20 mice (male and female halves) were fasted overnight, and the test substance was administered once every morning, with a gavage amount of 20ml/kg, and the gavage amount of 5000mg/kg in practical example 1, and observed for 14 days, and death and poisoning were recorded.
1.2.3 multiple integrity skin irritation tests
The method is carried out according to the disinfection technical specification (2002 edition) 2.3.3 skin irritation test, hairs on two sides of the spine of the back of the white rabbit are subtracted by a pet repairing scissors 24 hours before the test, the hair removal range is 3cm multiplied by 3cm, and the epidermis cannot be damaged. 0.5ml of the product of example 1 was applied directly to the unhaired animal skin at 2.5cm x 2.5cm area and 4h after application, washed with water or a suitable non-irritating washing solvent to remove the residue. The application was carried out once a day for 14 days and the other side was used as a blank control. The skin irritation response was observed 24h after each application.
1.2.4 mouse bone marrow pleochromatic cell micronucleus test
The test was carried out according to "Disinfection protocol" (2002 edition) 2.3.3.8.4 "mouse bone marrow pleochromocyte micronucleus test". Animal grouping and dosage preparation: the low, medium and high dose groups were 1.25g/kg, 2.50g/kg and 5.00g/kg, 10 mice were used for each dose group, and the male and female half of each dose group. Weighing 1.25g, 2.50g and 5.00g of samples respectively, adding distilled water to 20ml, and mixing uniformly; the solvent control group is distilled water, the positive control group is cyclophosphamide 40mg/kg BW, 40mg cyclophosphamide is weighed, and physiological saline is added to the solution until the volume is 20 ml. The method is used for 30h of oral gavage, and the gavage amount is 20 ml/kg. The interval between two infections is 24h, and the animals are sacrificed 6h after the second infection. Taking the sternum, extruding marrow liquid by using a hemostatic forceps, uniformly mixing with calf serum at one end of a slide, and performing conventional smear. And naturally drying the smear, fixing the smear in methanol for 10 minutes, drying the smear, putting the dried smear in Giemsa application solution, dyeing the smear for 15 minutes, immediately washing the smear by using phosphate buffer solution with pH6.8, and drying the smear. And observing and counting 1000 PCEs under a microscope, and calculating the micronucleus rate ([ permillas ]) and the PCE/NCE value.
1.2.5 Sterilization Effect test
1.2.5.1 preparation of bacterial suspension 1X 10 was prepared according to the 2002 edition "Disinfection technical Specification8～5×108cfu/mL (Candida albicans 1X 10)7～5×107cfu/mL) of the bacterial suspension for use.
1.2.5.2 neutralizer identification test
Coli and candida albicans were used as representative strains of bacterial propagules and fungi, respectively, for testing. The test is carried out by adopting a neutralizer identification test of a suspension quantitative sterilization test, the test is divided into 6 groups, the disinfection action time of the 1 st group and the 2 nd group is 1.0min, and each group is repeated for 3 times.
1.2.5.3 quantitative Sterilization test
The test was carried out using a suspension quantitative sterilization test. Test and positive control groups: placing the prepared suspension of Escherichia coli, Staphylococcus aureus, Candida albicans and disinfectant in a constant temperature water bath at 20 deg.C, adding 1mL of test bacterial suspension and 4mL of disinfectant (diluent for positive control instead of disinfectant), respectively, mixing, allowing test groups to act for 2.5min, 5min and 7.5min, allowing positive control group to act for 5min, adding 0.5mL of the above mixed solution of bacteria and drugs into 4.5mL of neutralizer, neutralizing for 10min, and adding 0.5mL of diluent for negative control group into 4.5mL of neutralizer, and neutralizing for 10 min. Inoculating 1mL of the suspension into a sterile plate, culturing in a constant temperature box at 37 ℃ for 48h, counting viable bacteria, and calculating the killing logarithm value. Each set of experiments was repeated 3 times.
1.2.5.4 object surface Sterilization on-site test
A sterile specification plate is used for marking a stain area (5.0cm multiplied by 5.0cm) in the middle of the surface of a tested table top, a table top and a door, each object is tested for 30 samples, each sample is tested for 2 areas, wherein 1 area is a test group, and the other area is a positive control group. Sucking the bacterial suspension with sterile pipette, dripping into the bacterial staining area with 0.1ml per area, spreading with sterile cotton stick, and drying in 37 deg.C oven.
Positive control group: the sterile cotton swab was wetted in a test tube containing 5ml of diluent, and 30 control blocks were sampled, each block being traversed 8 times. After sampling, the sampling end of the cotton swab is cut into the original diluent test tube in an aseptic operation mode, and the cotton swab is rapped for 200 times and acts for 10 min. Diluting with diluent.
Test groups: example 1 the test area on the surface of each object was wiped and sterilized, after 15 minutes, a sterile cotton swab was wetted in a test tube containing 5ml of neutralizer, and 30 sterilized blocks were smeared and sampled, each block being traversed 8 times in the horizontal and vertical directions. After sampling, the sampling end of the cotton swab is cut into the original neutralizer test tube in an aseptic operation mode, and the vibration is carried out for 200 times for 10 min. If necessary, the mixture is diluted with a neutralizing agent.
Negative control group: after the completion of the test, 1.0ml of each of the used neutralizer and diluent of the same lot was mixed, and then the medium was inoculated to serve as a negative control sample.
The positive control group, the negative control group and the group sample of the example 1 are sucked by 1.0ml each, inoculated to an agar culture dish, inoculated to 3 plates each sample, placed in a 37 ℃ incubator for 48h, and observed to obtain the final result. And calculating the killing logarithm value.
1.2.5.5 Fabric surface, stainless Steel dinner plate surface, cucumber surface Disinfection on-site test
Example 1 the fabric surface, stainless steel dish surface, cucumber surface were sterilized by soaking for 15 minutes, the rest being the same as the sterilization of the object surface.
1.2.5.6 hand in-situ Disinfection test
Test samples: at the site of use, subjects were randomly selected. The test is not less than 30 people.
Positive control group: before disinfection, the left fingers of the testee are closed after the two hands of the testee are rubbed fully, the testee is soaked in a test tube containing 10ml of diluent by using a sterile cotton swab, after the tube wall is squeezed to be dry, the two fingers are rubbed repeatedly for 2 times from the bent surfaces of the five fingers to the finger roots, and the cotton swab is rotated once every time the rubbing is performed. After sampling, the sampling end of the swab was aseptically cut into a neutralizer tube, which served as a positive control sample.
Test groups: the right hand was sprayed with the stock solution of example 13 times for 1min for disinfection. After sterilization, the neutralizing agent was used instead of the diluent, and the natural bacteria remaining on the right hand of the subject were sampled once in the same manner as in the positive control group, and used as a test group sample.
Negative control group: the unused neutralizer of the same batch, 1.0ml of each diluent and 1-2 parts of cotton swab are mixed respectively to be used as a negative control group sample.
Respectively taking 1ml of samples of the test group, the positive control group and the negative control group, inoculating the samples into the plates by an agar pouring method, inoculating 2 plates into each sample, placing the samples into a 37 ℃ incubator for culturing for 48 hours, and observing the final result. Calculating kill logarithm value
1.2.5.7 poliovirus inactivation assay
1.2.5.7.1 test for identifying physical removal method of residual disinfectant
According to the disinfection technical specification (2002 edition), an identification test of a physical removal method of residual disinfectants is carried out, a sample stock solution of a sample is subjected to an action time of 5min, and the test is divided into 5 groups according to standard requirements;
1.2.5.7.2 poliovirus inactivation assay
The test sample stock solution for the poliovirus inactivation test was subjected to the disinfection specification (2002 edition) for a prescribed period of time, and the test was repeated 3 times.
1.2.6 Metal Corrosion test
Stainless steel, carbon steel, copper and aluminum are taken as metal test sample pieces respectively, and the metal test sample pieces are weighed after being cleaned, frosted and dried. The metal sample was immersed in the disinfectant of example 1, and the disinfectant was changed and the metal sample was washed daily for 3 consecutive days for 72 hours. And taking out the metal sample, washing the metal sample by distilled water, drying the metal sample, weighing the metal sample again, and calculating the corrosion rate (R). The judgment standard of the corrosivity is that R is less than 0.0100, no corrosion exists basically, R is more than 0.0100 and less than 0.1000, mild corrosion, R is more than 0.1000 and less than 1.00 moderate corrosion, and R is more than or equal to 1.00 severe corrosion.
2 results
2.1 stability test results
After the disinfectant in the embodiment 1 is stored in a constant temperature and humidity box at 54 ℃ for 14 days, the silver ion content is 13.9mg/L and the reduction rate is 3.4 percent by graphite furnace atomic absorption spectrophotometry; the content of the hydrogen peroxide is 32.6g/L, the reduction rate is 1.2 percent and is less than 10 percent through volumetric method detection, the requirements of 'sterilization technical specification' (2002 edition) are met, and the validity period of the product meets the requirement of storage for 1 year. See table 1 and table 2 for details.
TABLE 1 silver ion stability test results for the disinfectant of example 1
TABLE 2 disinfectant Hydrogen peroxide stability test results of example 1
2.2 acute oral toxicity test results
20 mice (female and male halves) have no obvious symptoms and death within 14 days of observation period, and no obvious abnormality is found at necropsy after the experiment is finished. Acute oral median lethal dose LD of mice50>5000mg/kg, according to the Disinfection Specification (2002 edition), the disinfectant of example 1 of the present invention is of a practical non-toxic grade. The detailed results are shown in table 3.
TABLE 3 acute oral toxicity test results for the disinfectant of example 1
Sex
Dosage (mg/kg)
Animal number (only)
Number of dead animals
Mortality (%)
Female part
5000
10
0
0
Male part
5000
10
0
0
2.3 multiple complete skin irritation test results
TABLE 4 disinfectant of example 1 multiple intact skin irritation test results
The disinfectant of example 1 was non-irritating to rabbits in multiple complete skin irritation tests according to the disinfection specifications (2002 edition) rating criteria for skin irritation intensity. See table 4 for details.
2.4 mouse bone marrow pleochromocyte micronucleus test results
TABLE 5 results of the mouse myelophilia polycystic erythrocyte micronucleus test with the disinfectant of example 1
Dosage (g/kg)
Animals (only)
PCE number under test
PCE number containing microkernel
Micronuclear cell rate (‰)
PCE/NCE
1.25
10
10000
18
1.8±0.3
1.04±0.02
2.50
10
10000
17
1.7±0.4
1.04±0.02
5.00
10
10000
18
1.8±0.4
1.04±0.02
Solvent control
10
10000
17
1.7±0.5
1.05±0.03
Positive control
10
10000
340
3.4±1.6
0.95±0.07
The disinfectant of example 1 of the present invention was negative to mouse bone marrow pleochromocyte micronucleus test according to the Disinfection Specification (2002 edition).
2.5 results of Metal Corrosion test
After the disinfectant of example 1 of the present invention soaks the metal sheet for 72 hours, the corrosion rates (R) of the disinfectant on stainless steel, carbon steel, aluminum and copper were 0.0000mm/a, 0.0261mm/a, 0.0628mm/a and 3.3649mm/a, respectively, as shown in Table 6 below. The disinfectant of example 1 of the present invention was judged to have substantially no corrosion on stainless steel, mild corrosion on carbon steel and aluminum, and severe corrosion on copper according to the corrosion classification criteria.
Table 6 disinfectant metal corrosion test results of inventive example 1
2.6 results of the quantitative killing of Escherichia coli and Staphylococcus aureus with the disinfectant of example 1 of the present invention
2.6.1 results of the experiment for quantitatively killing Escherichia coli with disinfectant in example 1 of the present invention
The disinfectant of the embodiment 1 of the invention is used for disinfecting escherichia coli, the action is 1min, and the neutralization identification test result is as follows: the average number of growing colonies in the first group was 0cfu/ml, and the average number of growing colonies in the 2 nd group was 1.25X 102cfu/ml, the average number of growing colonies of groups 3, 4 and 5 were 2.02X 107cfu/ml、2.13×107cfu/ml、2.40×107cfu/ml, inter-group error rate 6.54%, group 6 aseptically grown. See table 7 for details. Description of broth taken in D/E +5g/LNa2S2O3The neutralizing agent effectively neutralizes the disinfection of example 1 of the present inventionInhibition of bacterial propagules (E.coli) by the agent; and the neutralizing agent and the neutralizing product formed by the neutralizing agent and the disinfectant of the embodiment 1 have no influence on the growth and culture of the tested bacteria.
TABLE 7 results of the identification test of Escherichia coli neutralizer of example 1 of the present invention
TABLE 8 results of E.coli killing by the disinfectant of example 1 of the present invention
TABLE 9 results of killing Staphylococcus aureus by the disinfectant of example 1 of the present invention
Under the test condition, the disinfectant of the embodiment 1 of the invention is repeated for 3 times, acts for 5 minutes, has an average killing logarithm value of more than or equal to 5.00 (the sterilization rate is more than or equal to 99.999%) on staphylococcus aureus and escherichia coli, is shown in tables 8 and 9 in detail, meets the requirements of disinfection technical specification (2002 edition), and is qualified in disinfection.
2.6.2 results of the test for quantitative killing of Candida albicans by the disinfectant of the invention example 1
The invention embodiment 1 disinfects Candida albicans for 1min, and the neutralization identification test result is as follows: the average number of growing colonies in the first group was 0cfu/ml, and the average number of growing colonies in the 2 nd group was 1.25X 102cfu/ml, the average number of growing colonies of groups 3, 4 and 5 were 2.02X 107cfu/ml、2.13×107cfu/ml、2.40×107cfu/ml, 6.54% inter-group error rate, sterile group 6And (5) growing. See table 10 for details. Description of broth taken in D/E +5g/LNa2S2O3The neutralizing agent can effectively neutralize the (candida albicans) inhibition effect of the disinfectant of the embodiment 1 on the fungus propagules; and the neutralizing agent and the neutralizing product formed by the neutralizing agent and the disinfectant of the embodiment 1 have no influence on the growth and culture of the tested bacteria.
TABLE 10 identification test results for disinfectant Candida albicans neutralizer of inventive example 1
TABLE 11 results of Candida albicans killing by the disinfectant of example 1 of the present invention
Under the test condition, the disinfectant of the embodiment 1 of the invention is repeated for 3 times, acts for 5 minutes, has an average killing logarithm value of Candida albicans of more than or equal to 4.00 (the sterilization rate is more than or equal to 99.99 percent), is detailed in tables 10 and 11, meets the requirements of the technical specification for disinfection (2002 edition), and is disinfected qualified.
2.6.3 simulation test results of the disinfectant of example 1 of the present invention on the disinfection of the surface of an object
Table 12 simulation test results of the disinfectant of example 1 of the present invention for disinfecting the surface of an object
The disinfectant of the embodiment 1 of the invention is used for wiping and disinfecting the surface of a general object, acts for 15min, has an average killing logarithm value of more than or equal to 3.0 for escherichia coli polluted on the surface of the object, is detailed in table 12, and meets the requirements of disinfection technical specification (2002 edition).
TABLE 13 simulated on-site sterilization test results of the disinfectant of example 1 of the present invention on tableware
The disinfectant of the embodiment 1 of the invention has a disinfecting effect of 15min, has an average killing logarithm value of more than or equal to 3.0 for escherichia coli polluted on the surface of a stainless steel dinner plate, is detailed in table 13, and meets the requirements of disinfection technical specification (2002 edition).
2.6.4 simulation test results of the disinfectant of embodiment 1 of the invention on the surface disinfection of fruits and vegetables
TABLE 14 simulation test results of surface sterilization of fruits and vegetables by the disinfectant of example 1 of the present invention
The disinfectant of the embodiment 1 of the invention has a disinfection effect of 15min, has an average killing logarithm value of more than or equal to 3.0 for escherichia coli polluted on the surface of cucumber, is detailed in table 14, and meets the requirements of disinfection technical specification (2002 edition).
2.6.5 simulation test results of the disinfectant of example 1 of the present invention on the surface of the fabric
TABLE 15 simulation test results of disinfectant of inventive example 1 on fabric surface disinfection
The disinfectant of the embodiment 1 of the invention has the soaking disinfection effect for 15min, has the average killing logarithm value of more than or equal to 3.0 for escherichia coli polluted on the surface of the fabric, is detailed in table 15, and meets the requirements of disinfection technical specification (2002 edition).
2.6.6 results of the in situ hand sanitization test with the sanitizer of example 1 of this invention
TABLE 16 results of the disinfectant of example 1 of the present invention on-site hand disinfection test
The disinfectant of the embodiment 1 of the invention has a wiping disinfection effect of 1.0min, has an average killing logarithm value of natural bacteria on hand surfaces of more than or equal to 1.0, is shown in table 16 in detail, meets the requirements of disinfection technical specification (2002 edition), and is qualified in disinfection.
2.6.7 simulation test results of disinfectant inactivated poliovirus of example 1 of the invention
2.6.7.1 method for physically removing residual disinfectant
TABLE 17 identification test results of physical removal method of residual disinfectant
2.6.7.2 simulation test results of disinfectant inactivated poliovirus of example 1 of the invention
Table 18 simulation test results of disinfectant-inactivated poliovirus of example 1 of the present invention
The physical removal method used in this test was effective in terminating the bactericidal activity of example 1, as detailed in table 17. The disinfectant stock solution of the example 1 is acted for 10min, the test is repeated for 3 times, the average inactivation log value of the poliovirus is 4.53, the details are shown in a table 18 and are more than 4.00, and the disinfectant stock solution meets the requirements of the disinfection technical specification 2002 edition-2.1.1.10.7 standard.
Experiments prove that the disinfectant containing the supramolecular silver provided by the embodiment of the invention can be used for in-vitro disinfection of people and animals, air disinfection of public places, disinfection of daily supplies and disinfection and sterilization effect of 99.999%. The activity of the disinfectant is 300-10000 times of that of the traditional inorganic silver ion disinfectant (silver nitrate) or the traditional organic acid silver hydrate, and the disinfectant has the characteristics of high activity and small using amount.
In the above embodiments, the descriptions of the respective embodiments have respective emphasis, and for parts that are not described in detail in a certain embodiment, reference may be made to related descriptions of other embodiments.
While the invention has been described with reference to specific embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.