CN108552216B - Sporicide and preparation method and application thereof - Google Patents
Sporicide and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a sporicide and a preparation method and application thereof, and the sporicide comprises the following components in percentage by weight: (1) 0.05-5% chlorite; (2) 0.1-10% of hydrogen peroxide antioxidant; (3) a pH adjusting agent; (4) the balance being solvent; wherein the pH regulator is used in an amount such that the pH value of the sporicide is 3 to 6. The invention also relates to a preparation method and application of the sporicide. The sporicide is slightly acidic and does not contain a large amount of strong electrolyte, satisfactorily solves the problems of instability of chlorite under acidic conditions and low disinfection and sterilization activity, simultaneously generates excellent disinfection and sterilization effects, and can be widely applied to disinfection or sterilization of surfaces of various objects and closable spaces (such as operating rooms of hospitals, workshops of production enterprises, isolators, laboratories, biosafety cabinets and the like).
Description
Technical Field
The invention relates to the technical field of disinfection, in particular to a sporicide consisting of chlorite and a hydrogen peroxide antioxidant, and a preparation method and application thereof.
Background
Disinfectant (disinfectant) refers to a chemical agent used for killing pathogenic microorganisms on a transmission medium to make the transmission medium achieve the harmless requirement. Sporicide (sporicide) is a disinfectant that kills spores. The sporicides commonly used at present are classified mainly into peroxide sporicides (such as hydrogen peroxide, peroxyacetic acid and the like), active chlorine sporicides (such as hypochlorous acid/sodium, chlorine dioxide and the like), and aldehyde substances sporicides (such as formaldehyde, glutaraldehyde, o-phthalaldehyde and the like), and the method of atomizing or vaporizing is frequently used for space sterilization.
When the atomization or vaporization method is adopted to use the peroxide sporicide with single component for space disinfection and sterilization, the use range is limited because higher concentration (for example, the use concentration of hydrogen peroxide needs to be more than 30 percent) is needed and the corrosivity is relatively serious, the disinfection and sterilization effect is not ideal under the conditions of low temperature and high humidity, and particularly the killing capability to certain viruses is not ideal.
When the space sterilization is carried out by using the composite peroxide sporicide (such as a composite of hydrogen peroxide and peroxyacetic acid) by adopting an atomization or vaporization method, although the use concentration of the peroxide can be reduced and the corrosivity can be reduced, the problem that the sterilization effect is not ideal under the conditions of low temperature and high humidity is still not solved.
When the aldehyde sporicide is used for space sterilization, although the sterilization effect is not greatly influenced by temperature and humidity, the aldehyde sporicide is forbidden to be used in many fields, particularly in the field of medicine and food manufacturing in many countries because of high toxicity.
When the commonly used active chlorine sporicide (such as hypochlorous acid/salt, chlorine dioxide and the like) is used for space disinfection and sterilization, the active chlorine sporicide has better disinfection and sterilization effects under the conditions of low temperature and high humidity, has higher virus killing activity than common peroxides, but is very unstable and very inconvenient to use.
Chlorine dioxide (ClO)2) Is a good disinfectant which is recognized at present and can kill all microorganisms including bacterial propagules, bacterial spores, fungi, mycobacteria, viruses and the like. ClO2It is easily soluble in water, and almost 100% of it exists in molecular state, so it easily penetrates cell membrane, infiltrates into bacterial cell, oxidizes its nucleic acid (DNA or RNA), thereby prevents bacterial anabolism and makes bacteria die. Thus ClO2Has the advantages of wide application range, low dosage, quick response, good effect, long duration, no toxicity, no harmful effect on the environment and the like. However, chlorine dioxide is extremely unstable in both gas and solution, and particularly, when exposed to light and heat or to organic substances, it promotes its decomposition (gaseous ClO)2Half-life in sunlight of only about 1 hour), at 50 ℃ will cause explosive decomposition to produce oxygen (O)2) And toxic chlorine gas (Cl)2) Therefore, the safety of the gaseous chlorine dioxide in practical application is not completely guaranteed, the use is very inconvenient, and the gaseous chlorine dioxide needs to be prepared on site. Although the aqueous solution using chlorine dioxide is relatively safe, it has the same problem of instability, and the half-life of the chlorine dioxide solution after activation is only 1 day, so it must be prepared as it is, and before activation, it is often stored in the form of "stable" chlorine dioxide (which is essentially an alkaline solution containing chlorite) without antibacterial activity, and when used, it is activated by adding acid or an oxidizing agent to generate chlorine dioxide. The activation reaction is as follows:
ClO- 2+H+→HClO2(pH adjustment with addition of a small amount of acid)
5HClO2→4ClO2↑+HCl+2H2O (Placement)
4ClO- 2+2H+→2ClO2↑+HClO3+HCl+H2O (activated by addition of large amounts of acid, pH<1, no addition of Cl-)
5ClO- 2+4H+→4ClO2↑+Cl-+2H2O (activated by addition of large amounts of acid, pH<1, with addition of Cl-)
2ClO- 2+S2O2- 8→2C1O2↑+2SO2- 4(activated by addition of a large amount of strong oxidant, pH 5-9)
From the above reaction, it can be seen that: when the chlorine dioxide disinfectant is prepared by activating sodium chlorite by adding strong acid or enhancing oxidant, a large amount of strong electrolyte can be generated, even strong acid such as hydrochloric acid, chloric acid and the like can be generated, and the chlorine dioxide disinfectant prepared by the methods is only suitable for surface disinfection and water disinfection under low concentration, is not suitable for space disinfection by adopting a spraying mode under high concentration, and otherwise can generate corrosion action on the surface of a disinfected object, particularly on the surface of a metal object.
When chlorous acid is converted to chlorite salts such as sodium and potassium chlorite salts, etc., it is relatively stable in both solid and solution states.
Recent studies have shown that chlorite also has disinfecting activity at lower pH and is more stable than chlorine dioxide.
PCT international patent (WO2014/188310EN 2014.11.27) discloses a disinfectant comprising a chlorous acid aqueous solution, which is mainly used as an object surface disinfectant, a food additive, an antiseptic, a pharmaceutical preparation, and the like, and which generates only a small amount of chlorine dioxide at a ph of about 6.5 and is thus relatively stable. The technique does not note the specific stabilizable time. In fact, the disinfectant generates a large amount of chlorine dioxide at pH 3.5, so that chlorous acid disinfectant proposed by the art is unstable at pH below 6.5, and is not suitable for space disinfection by spraying due to a large amount of strong electrolyte.
PCT international patent (WO2014/188312EN 2014.11.27) discloses long-term storage and new use of a chlorous acid aqueous solution formulation characterized by comprising a chlorous acid aqueous solution, a metal hydroxide and a metal phosphate for disinfection of the surface of an object and removal of an odor in the air. The disinfectant has the greatest characteristic that the antibacterial activity is strongest when the pH value is 5-7, and the antibacterial activity (expressed by a phenol coefficient) of the disinfectant is reduced by about 10 percent only after the disinfectant is placed for 1 month; however, when the pH is less than 4, the antibacterial activity (expressed by the phenol coefficient) is reduced by about 70% after the storage for 1 month. When left at a pH below 3 for 1 month, the antibacterial activity (expressed by the phenol coefficient) was completely lost (chlorine dioxide (no maximum absorption in the UV spectrum at a wavelength of 355-358 nm) and chlorous acid (no maximum absorption in the UV spectrum at a wavelength of 260 nm) were not detected).
PCT international patent (WO2008/099911JA 2008.08.21) discloses a broad-spectrum antiviral pharmaceutical composition having excellent storage stability, which is characterized by being composed of a pure chlorine dioxide liquid preparation containing, as constituent components, a dissolved chlorine dioxide gas, chlorite, and a pH adjuster (phosphoric acid or a salt thereof), and which has broad-spectrum antiviral activity after one year of storage due to the addition of phosphoric acid or a salt thereof as a pH adjuster and a stabilizer (pH5.5 to 6).
It can be seen that the disinfection solution containing sodium chlorite prepared by the prior art has a pH value of more than 5.5 and contains a large amount of strong electrolyte. If the pH is below 5.5, the stability is not more than 1 month.
Disclosure of Invention
The invention provides a stable sporicide which only contains a small amount of electrolytes and has good killing effect on bacterial spores and viruses, and aims to solve the problems of safety, effectiveness, corrosiveness and stability of the existing chlorine-containing sporicide when used for space disinfection and sterilization, in particular to solve the problems that the existing active chlorine disinfectant is unstable (especially unstable under acidic conditions), contains a large amount of strong electrolytes and is easy to corrode metal materials, is not suitable for space disinfection and sterilization and the like.
The sporicide of the invention comprises the following components by weight percent:
(1) 0.05-5% chlorite;
(2) 0.1-10% of hydrogen peroxide antioxidant;
(3) a pH adjusting agent;
wherein the dosage of the pH regulator is that the pH value of the sporicide is 3-6 (preferably 3.5-5.5).
The sporicide of the invention is slightly acidic (pH3-6) and does not contain a large amount of strong electrolyte. The sporicide satisfactorily solves the problems of instability of chlorite under an acidic condition and low sterilization activity, simultaneously generates excellent sterilization effect, and can be widely applied to the sterilization or the sterilization of surfaces of various objects and closable spaces (such as operating rooms of hospitals, workshops of manufacturing enterprises, isolators, laboratories, biosafety cabinets and the like).
Preferably, the chlorite is 0.1-2.5% by mass.
Preferably, the chlorite is one or a mixture of more of potassium salt, sodium salt, calcium salt or magnesium salt of chlorous acid, and is more preferably sodium chlorite.
In order to provide the sporicide with more excellent effect, the present invention preferably uses hydrogen peroxide as an antioxidant. In addition, the antioxidant of the present invention can also be used as a stabilizer and a synergist of the sporicide of the present invention.
The antioxidant of the invention can be 0.1-10% by mass, preferably 0.5-8% by mass. Within the above concentration range, the antioxidant of the present invention can make HClO2/ClO- 2The following cyclic reaction occurs in the solution to prevent ClO2Decomposition to Cl2And O2Thereby achieving stabilization of HClO2/ClO- 2The purpose of (1).
Theoretically, any acidic substance can be used as the pH adjuster, and various inorganic acids such as hydrochloric acid, sulfuric acid, phosphoric acid, carbonic acid and the like, various organic acids such as oxalic acid, citric acid, acetic acid, lactic acid and the like, and various acidic salts such as sodium hydrogen sulfate, sodium dihydrogen phosphate and the like can be included. However, it has been found through studies that the stability of sodium chlorite varies when a different pH adjusting agent (acidic substance) is added to the chlorite solution to adjust the pH of sodium chlorite.
In order to improve the comprehensive performance such as stability and the like of the sporicide, the pH regulator is preferably an acidic substance or a cation exchange resin which can release hydrogen ions.
Preferably, the cation exchange resin is a styrene-type strong-acid cation exchange resin, more preferably a 001 × 7 styrene-type strong-acid cation exchange resin.
Preferably, the acidic substance is phosphoric acid or sulfamic acid.
The pH regulator can obviously improve the stability of the sporicide, wherein the strong-acid cation exchange resin has better stabilizing effect, and phosphoric acid and sulfamic acid are used secondarily. The possible reason is that the strong acid cation exchange resin can adsorb various metal ions therein, and the presence of the metal ions can catalyze the decomposition of chlorite and chlorine dioxide.
The invention selects strong acid cation exchange resin or phosphoric acid or sulfamic acid as pH regulator, which not only can adjust pH, but also can play a role of stabilizer, in addition, the strong acid cation exchange resin can play a role of reducing strong electrolyte in solution.
Preferably, the strong-acid cation exchange resin is a styrene-type strong-acid cation exchange resin. Since the strong acid cation exchange resin is insoluble in water and only exchanges with metal ions in the solution, the metal ions in the solution are slowly substituted with H+The substitution is performed to adjust pH, and when the desired pH is reached, the ion exchange resin is removed by filtrationFat, too, does not produce local peracid.
In the present invention, it is preferable to adjust the pH of the solution to a range of 3 to 6, more preferably 3.5 to 5.5, from the viewpoint of long-term storage stability and from the viewpoint of sterilization effect.
Further studies have shown that the pH regulator and antioxidant of the present invention also synergistically stabilize HClO2/ClO- 2The antioxidant also has the function of reacting with HClO2/ClO- 2Synergistic antibacterial effect.
In order to make the solvent used by the sporicide of the invention quickly volatilize to generate faster disinfection and sterilization effects, the invention can select water and other volatile low-carbon chain alcohol (C) besides purified water as the first solvent2-C3) The mixed solution is used as a solvent; the volatile low carbon chain alcohol is selected from one or more of ethanol, n-propanol and isopropanol, and the concentration of the volatile low carbon chain alcohol is only required to be capable of dissolving the components, and preferably accounts for 0.5-50% (w/w), more preferably 1-10% (w/w) of the solvent.
The sporicide of the present invention may contain optional other soluble substances such as hydrogen peroxide stabilizers, surfactants, corrosion inhibitors, wetting agents, fragrances, colorants and the like, in addition to the above-described main components. These added soluble substances are known in the art and do not chemically react or otherwise interfere with other ingredients already present. The amount of the additive is not particularly limited as long as the required or prescribed residual level after sterilization is not increased, and the amount of the additive is different depending on the kind of the additive.
As a preferred technical scheme, the sporicide consists of the following components in percentage by weight:
(1) 0.1-2.5% sodium chlorite salt;
(2) 0.5-8% of hydrogen peroxide antioxidant;
(3) a pH adjusting agent;
(4) the balance of water;
wherein the pH regulator is one of phosphoric acid, sulfamic acid or styrene type strong-acid cation exchange resin; the dosage of the pH regulator is such that the pH value of the sporicide is 3.5-5.5.
As a preferred technical scheme, the sporicide formula of the invention is as follows:
(1) 1% sodium chlorite salt;
(2) 5% hydrogen peroxide;
(3) a pH adjusting agent;
(4) the balance of water;
wherein the pH regulator is styrene type strong-acid cation exchange resin; the amount of the pH regulator is such that the pH of the sporicide is 4.
The sporicide can be prepared by the conventional preparation method in the field, and in order to realize the best effect of the sporicide, the invention also provides a preparation method of the sporicide, which comprises the following steps:
(1) adding chlorite into solvent to dissolve to obtain solution;
(2) adding a pH regulator into the solution obtained in the step (1) to adjust the pH value of the solution (if the pH value is adjusted by using ion exchange resin, filtering to remove the ion exchange resin after the pH value meets the requirement);
(3) and (3) adding an antioxidant into the solution obtained in the step (2), supplementing a solvent to a required concentration, and uniformly stirring to obtain the antioxidant.
The sporicide prepared by the invention is a transparent solution. Preferably, the prepared solution (sporicide) is stored separately in a light-tight container.
The invention also provides the application of the sporicide in disinfection of object surfaces and disinfection or sterilization of spaces.
The invention selects hydrogen peroxide as an antioxidant, selects phosphoric acid, sulfamic acid or strong acid cation exchange resin as a pH regulator, and selects purified water or purified water and alcohol (C) with a low carbon chain2-C3) The composite mixed solution is used as solvent to prepare sporicide, and H in the solution is well inhibited under slightly acidic condition (pH3-6)ClO2/ClO- 2To ClO2Conversion, or the already generated ClO in solution2Reconversion to HClO2/ClO- 2Thereby ensuring HClO2/ClO- 2Is further improved or prolonged and also due to the synergistic effect of the antioxidants, HClO is obtained2/ClO- 2The sterilizing activity of the composition is enhanced. Since the sporicide prepared by the invention does not contain a large amount of strong electrolyte, the sporicide is preferably particularly suitable for disinfection or sterilization of surfaces of various objects and closable spaces (such as operating rooms in hospitals, workshops and isolators of production enterprises, laboratories, biosafety cabinets and the like) by adopting a spraying method.
Compared with the active chlorine sporicide product on the current market, the invention has the following characteristics:
(1) the disinfectant does not contain a large amount of strong electrolyte, particularly does not contain a large amount of strong acid electrolyte such as sulfuric acid, hydrochloric acid or chloric acid, so that the corrosivity is low, and the disinfectant is particularly suitable for disinfection or sterilization of surfaces of various objects and closable spaces (such as operating rooms of hospitals, workshops of manufacturing enterprises, isolators, laboratories, biosafety cabinets and the like) by adopting a spraying method;
(2) under slightly acidic environment, no obvious ClO2Release, thereby increasing HClO2/ClO- 2Stability of (2);
(3) has synergistic antibacterial effect with antioxidant, and also has improved disinfecting and sterilizing activity.
Detailed Description
The following test examples and examples are intended to illustrate the present invention, but are not intended to limit the scope of the present invention. The concentrations of the respective components described below are all referred to as mass percentage concentrations.
Test example 1: effect of pH adjusting Agents on the stability of chlorite solutions
1.25g of sodium chlorite with the content of 80 percent (equivalent to 1g of pure sodium chlorite) is taken, 90ml of water is firstly added for dissolving, then the pH value of the solution is adjusted to 3.5 by using the pH regulator listed in the table 1, finally, water is further added to 100ml, so as to obtain a sodium chlorite/chlorous acid solution with the concentration of 1 percent, the solution is respectively placed for 1 hour and 24 hours at the temperature of 54 ℃, and the maximum absorbance change (the concentration change of the sodium chlorite is checked) at the wavelength of 260nm is measured after the solution is diluted by 20 times, and the result is shown in the table 1. The results show that: the strong acid cation exchange resin or phosphoric acid or sulfamic acid is selected as the pH regulator of the chlorite, which not only can play a role in regulating the pH, but also can play a role in stabilizing.
TABLE 1 influence of pH regulators on the stability of chlorite/salt solutions
Test example 2: effect of Hydrogen peroxide antioxidant on the stability of chlorite solution
1.25g of 80% sodium chlorite (equivalent to 1g of pure sodium chlorite) is taken, 90ml of water is firstly added for dissolving, an appropriate amount of pH regulator listed in the table 2 is added for regulating the pH value of the solution to 4, then water is added to 100ml, 1% sodium chlorite/chlorous acid solution is obtained, 1.25g of 80% sodium chlorite (equivalent to 1g of pure sodium chlorite) is also taken, 90ml of water is firstly added for dissolving, 2g of 50% hydrogen peroxide solution is added for stirring uniformly, the pH value of the solution is regulated to 4 by the same method, then water is added to 100ml, 1% sodium chlorite/chlorous acid solution (containing 1% hydrogen peroxide) is obtained, the prepared solution is respectively placed for 1 hour and 24 hours at 54 ℃, and the maximum absorbance change (the concentration change of the sodium chlorite is detected) at the wavelength of 260nm is measured after 20 times of dilution, and the result is shown in the table 2. The results show that: the stability of the chlorous acid/sodium solution is significantly improved after the addition of hydrogen peroxide.
TABLE 2 Effect of antioxidants (Hydrogen peroxide) on the stability of the chlorite/salt solutions
Example 1
This example provides a sporicide (total 100g) formulated as follows:
(1) 1.25g of 80% sodium chlorite;
(2) 5g of 50% hydrogen peroxide;
(3)001 x 7 type cation exchange resin, adjusting the pH value of the sporicide to 3.5;
(4) the balance being water.
Examples 2 to 3
The formulation is shown in Table 3.
Examples 4 to 6
This example provides the preparation of the sporicide of the previous examples 1-3, the sporicide of examples 1-3 is formulated according to the composition of table 3, the specific formulation steps are as follows:
(1) taking sodium chlorite, adding a proper amount of the solvent listed in the table 3, stirring to dissolve the sodium chlorite, and preparing a solution;
(2) adding a pH regulator listed in Table 3 to adjust the pH of the solution (if an ion exchange resin is used to adjust the pH, the ion exchange resin should be removed by filtration after the pH is as desired);
(3) adding hydrogen peroxide as an antioxidant;
(4) stirring uniformly to obtain a transparent solution;
(5) subpackaging in a lightproof container.
TABLE 3 formulation compositions of examples 1-3
Performance testing
1. Corrosion test on metals
The sporicide of the invention (examples 1 and 2) was tested for its corrosiveness to metals (diluted with purified water to a concentration of 500mg/L sodium chlorite before the test) in comparison with a commercially available "stable chlorine dioxide disinfectant solution" (activated before use according to the instructions and diluted with purified water to a concentration of 500mg/L chlorine dioxide) with reference to the disinfection specifications (2008) using carbon steel, stainless steel, copper and aluminum as test objects, as follows:
respectively taking carbon steel, stainless steel, copper and aluminum, respectively, making into a product with a diameter of 24 + -0.2 mm and a thickness of about 1.0mm,
and a wafer with a small hole with the diameter of about 2.0mm is ground during the test, the surface oxide layer is measured, the diameter, the thickness and the aperture are measured, the surface area is calculated, and then the wafer is cleaned and dried for 1 hour at the temperature of 50 ℃. Weighing the mass, soaking in experimental solution (at a ratio of 20 ml/cm)2Liquid volume), 1 container was used for 1 metal, and the experimental solution was changed 1 time for 24 hours. Soaking for 72h, taking out the metal sheet, washing with distilled water, and drying at 50 deg.C for 1 h. And weighing the mass of the soaked metal sheet, and calculating the corrosion rate R (mm/a) according to the mass loss.
[ R is corrosion rate, mm/a (mm/year); m is the weight of the metal sheet before the test, g; m istWeight of the sheet metal after the test, g; m iskFor chemical treatment to remove the weight loss value g of the corrosion product sample wafer, and for those without chemical removal treatment in the test, the formula is calculated by deleting mkA value; s is the total surface area of the metal sheet in cm2(ii) a t is test time, h; d is the density of the metal material in kg/m3。]
The test results are shown in Table 4. As can be seen from Table 4, the sporicide of the present invention is significantly less corrosive than commercially available stable chlorine dioxide solutions.
TABLE 4 results of corrosion test on metals
2. Space sterilization test and surface sterilization test
(1) Space sterilization test method and results
The sporicide prepared according to example 3 of table 3 was subjected to a space sterilization test and simultaneously compared with a single sodium chlorite solution and a single hydrogen peroxide solution (comparative example 1 and comparative example 2), as follows.
(I) Main Experimental materials
Biological indicator (Bacillus stearothermophilus spores with spore amount of 10 respectively3And 106CFU/sheet, containing the same batch number biological indicator special culture solution) and TSA,
type-1 low-temperature vaporization nano-mist generator (provided by nano-mist technology ltd., wuhan city, atomization speed is 15ml/min, and can atomize the disinfection solution to small particles below 1 micron).
② test workshop
The height of a production workshop of a certain pharmaceutical enterprise is 2.8m, the width is 4.4m, the length is 6.5m, and the total volume of the space is about 80m3. Before the test, the workshop is dehumidified and the relative humidity is kept below 70%.
③ test method
Placing the nanometer fog generator in the middle of a workshop, wherein the spore amount arranged around the workshop is 10 respectively3And 1064 biological indicators of CFU/tablet (total 8 tablets), the height of the arranged biological indicators from the ground is 1m, then the tested sporicide or solution is added, all doors and windows are sealed, the machine is stopped after starting atomization for 10min, and the machine is kept stand for 2 hours (about equivalent to atomization of 5 ml/m)3) Taking out the biological indicator (spore strip) according to an aseptic method, putting the biological indicator into the thermophilic fat spore culture solution with the corresponding number (simultaneously observing whether the hydrogen peroxide color-changing chemical indicator changes color or not), putting the biological indicator into a constant-temperature incubator according to the instruction of the purchased biological indicator, and observing the biological indicator after culturing the biological indicator for 24 hours at the temperature of 55-60 ℃. Meanwhile, 1 tablet of the same batch of biological indicators is taken as a positive control. After 24 hours of culture, if the culture solution turns turbid and the color changes from purple to yellow, the culture solution is judged to be positive; if the culture solution is clear and the color does not change, the culture solution is negative; continuing culturing until 7 days, and if the culture solution turns yellow, judging that the sterilization is unqualified; if the culture medium is purple, the culture medium is judged to be qualified for sterilization.
Experimental results
The results of the experiment are shown in Table 5. As can be seen from Table 5, when the atomization volume was 5mL/m3With a 2 hour seal, the sporicide formulated according to table 3, example 3, killed six log spores, while the single sodium chlorite solution and hydrogen peroxide solution (comparative examples 1 and 2) killed only three log spores. Thus, the sporicide of the invention is obviously superior to a single sodium chlorite solution and a single hydrogen peroxide solution, and the sodium chlorite solution and the hydrogen peroxide solution have synergistic disinfection and sterilization effects.
TABLE 5 results of space sterilization tests with different sporicides or solutions
Note: the 4 indicators are all purple after being cultured, which indicates that the aseptic growth mark is- -;
the 4 pieces indicated yellow after incubation, indicating that all the bacteria were grown and marked +++;
4 pieces indicate that 2 pieces are purple and 2 pieces are yellow, which indicates that part of the bacteria grows and is marked as ++ -.
(2) Surface disinfection test method and results
Surface disinfection test method
The sporicide formulated according to example 3 of table 3 was subjected to a surface disinfection test: using atomization, 80m of the sporicide pair prepared in example 5 was used3The space is sterilized by nano mist, and the volume of the mist is 5ml/m3And the sealing time is 90 min. After the disinfection is finished, each surface (2 points on each wall surface and 8 points on the ground surface are randomly selected) in the sterilized clean area is wiped by using a sterile cotton swab, and the wiping area of each point is 5 x 5cm2After the rubbing, the head (cotton part) of the cotton swab was cut with sterile surgical scissors, and the cut cotton swab was put into a conical flask containing 50ml of 0.9% sterile sodium chloride solution, and sealed. The flask containing the sample was shaken repeatedly to release the microorganisms on the cotton swab into the solution. Filtering 50ml of sample solution with membrane, taking out the filter membrane, sticking the filter membrane with the bacteria face upward on TSA culture medium, culturing at 30-35 deg.C for 5 days, counting, and testing before sterilizationAnd (5) comparing the measurement results.
② surface sterilization test results
The results are shown in Table 6, and it can be seen from Table 6 that: when the atomization volume is 5ml/m3When the sealing time is 90 minutes, the sporicide can be used for space sterilization and can also be used for disinfecting the surface of an object, and after disinfection, the surface microorganisms of walls, floors and equipment all meet the requirements of GMP environment.
TABLE 6 comparison of microbial contamination levels before and after sterilization
In conclusion, the sporicide produced according to the invention not only has stronger disinfection and sterilization capability than chlorite or hydrogen peroxide with a single component, but also obviously improves the stability of chlorite under an acidic condition, reduces the corrosivity to metal objects due to not containing a large amount of strong electrolyte, better solves the problems of instability and low disinfection and sterilization activity of chlorite under an acidic condition, simultaneously generates the disinfection and sterilization effect of 1+1 & gt 2, and can be widely applied to disinfection or sterilization of surfaces of various objects and closable spaces (such as operating rooms of hospitals, workshops of production enterprises, isolators, laboratories, biosafety cabinets and the like).
In addition, the above experiment was repeated with the sporicide of examples 1-3 of the present invention after 12 months of storage, and the experimental results showed that the sterilizing effect was not significantly reduced. Therefore, the sporicide has good stability and has a shelf life of more than 1 year.
As described above, the present invention is explained by the specific examples and embodiments based on the claims, but the present invention is not limited thereto. While the embodiments described in the claims can be implemented, various modifications that can be made by those skilled in the art are intended to fall within the scope of the present application.
Claims (4)
1. A sporicide, comprising, in weight percent:
(1) 1% sodium chlorite salt;
(2) 5% of hydrogen peroxide antioxidant;
(3) a pH adjusting agent;
wherein the pH regulator is used in an amount such that the pH value of the sporicide is 4; the pH regulator is styrene type strong-acid cation exchange resin.
2. The sporicide of claim 1, wherein the balance of the sporicide is a solvent; the solvent is water or a mixed solution of water and volatile low-carbon chain alcohol; the alcohol with low carbon chain is selected from one or more of ethanol, n-propanol and isopropanol.
3. A process for the preparation of a sporicide according to claim 1 or 2, characterized in that it comprises the following steps:
(1) adding sodium chlorite into a solvent to dissolve to prepare a solution;
(2) adding a pH regulator into the solution obtained in the step (1) to regulate the pH value of the solution;
(3) and (3) adding a hydrogen peroxide antioxidant into the solution obtained in the step (2), and uniformly stirring to obtain the catalyst.
4. Use of the sporicide of claim 1 or 2 for disinfecting, spatially disinfecting or sterilizing surfaces of objects.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2628156A1 (en) * | 1975-07-16 | 1977-02-03 | Conforto Gaetano M | Chlorine dioxide soln. prepn. from sodium chlorite solns. - passed through acid cation exchanger resin pref. sulphonated crosslinked polystyrene |
| JP2008044862A (en) * | 2006-08-11 | 2008-02-28 | Sukegawa Chemical Co Ltd | Method for treating and preventing scuticociliatosis in fishes |
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| US20070104798A1 (en) * | 1999-10-04 | 2007-05-10 | S.K. Pharmaceuticals, Inc. | Synergistic antimicrobial preparations containing chlorite and hydrogen peroxide |
| US20040037891A1 (en) * | 1999-10-04 | 2004-02-26 | Karagoezian Hampar L. | Synergistic antimicrobial ophthalmic and dermatologic preparations containing chlorite and hydrogen peroxide |
| ITMI20080027A1 (en) * | 2008-01-09 | 2009-07-10 | Industrie De Nora Spa | BIOCIDAL COMBINATION FOR USE IN AGRICULTURAL FIELD |
| CN103070192A (en) * | 2012-12-28 | 2013-05-01 | 青岛大学 | Oxygen-increasing type solid stabilized chlorine dioxide, and preparation method and application thereof |
| JP6310745B2 (en) * | 2014-03-26 | 2018-04-11 | 保土谷化学工業株式会社 | Bactericidal composition |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2628156A1 (en) * | 1975-07-16 | 1977-02-03 | Conforto Gaetano M | Chlorine dioxide soln. prepn. from sodium chlorite solns. - passed through acid cation exchanger resin pref. sulphonated crosslinked polystyrene |
| JP2008044862A (en) * | 2006-08-11 | 2008-02-28 | Sukegawa Chemical Co Ltd | Method for treating and preventing scuticociliatosis in fishes |
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