CN113440441B - Oral bacteriostatic composition containing essential oil and preparation method thereof - Google Patents
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Abstract
The invention discloses an oral cavity bacteriostatic composition containing essential oil and a preparation method thereof, the composition takes essential oil compositions of disinfectants such as polyhexamethylene biguanide, chlorhexidine gluconate and the like and lavender essential oil, tea tree essential oil and garlic essential oil as main active ingredients, has good bacteriostatic action, can effectively inhibit periodontitis and relieve pain, can resist inflammation and refresh breath, and has good taste. The product has good stability, the mouthwash is convenient to use at any time, and the gel can quickly eliminate the inflammation of the oral mucosa at a fixed point and is convenient to use.
Description
Technical Field
The invention relates to an oral bacteriostatic composition containing essential oil and a preparation method thereof, belonging to the technical field of oral care and health care.
Background
Halitosis and oral ulcer are often related to the breeding of bacteria in the oral cavity, food residues can aggravate the growth of the bacteria in the oral cavity, and the oral bacteria can be aggravated because people often cannot brush teeth in time after lunch in office workers. At present, oral cleaning products are diversified, mainly take chemical disinfectants (such as polyhexamethylene biguanide, chlorhexidine gluconate and the like) as main components, and need higher concentration to achieve better antibacterial effect. Some disinfectants also have side effects, such as chlorhexidine gluconate products, which have a narrow antibacterial spectrum and can yellow and stain teeth after long-term use. In addition, the use of a large amount of disinfectant has a great influence on the environment, particularly on aquatic organisms.
In order to solve the above problems, some oral bacteriostatic agents of Chinese herbal medicines have been developed at present, for example, CN201911049382.6 discloses a Chinese medicinal bacteriostatic composition comprising, by weight, 0.1 to 2 parts of bacteriostatic raw materials, 7 to 50 parts of Chinese herbal medicinal raw materials and 0.02 to 0.2 part of surfactant, wherein the raw materials comprise scutellaria baicalensis, radix rehmanniae, prepared rehmannia root, ophiopogon root, white peony root, rhizoma anemarrhenae, cortex moutan, radix scrophulariae, dried orange peel and the like, and CN201910661682.3 discloses a bacteriostatic Chinese medicinal composition suitable for oral use and a preparation method thereof, and the Chinese medicinal raw materials comprise dragon's blood, calcined chinese urine, catechu, coptis chinensis, phellodendron, fried moonstone, bezoar, borneol, indigo naturalis and the like. The traditional Chinese medicine bacteriostatic preparation has slow response and poor mouthfeel caused by unique smell of Chinese herbal medicines. Consumers therefore have an urgent need for products that have less impact on teeth and faster onset of action.
Disclosure of Invention
The invention overcomes the defects of the prior art and provides an oral cavity antibacterial composition containing essential oil and a preparation method thereof, the composition takes essential oil compositions of disinfectants such as polyhexamethylene biguanide, chlorhexidine gluconate and the like, lavender essential oil, tea tree essential oil and garlic essential oil as main active ingredients, and has good antibacterial effect, effective periodontitis inhibition and pain relief, inflammation resistance, breath freshening and good taste.
The technical scheme of the invention is as follows: an oral bacteriostatic composition containing essential oil is characterized by comprising effective components, auxiliary agents and water, wherein the effective components are as follows:
a: one of a disinfectant polyhexamethylene biguanide, chlorhexidine gluconate or chlorhexidine acetate;
b: the essential oil composition comprises at least two of lavender essential oil, tea tree essential oil and garlic essential oil, and is preferably compounded by the lavender essential oil, the tea tree essential oil and the garlic essential oil, wherein the mass ratio of the lavender essential oil to the tea tree essential oil to the garlic essential oil is 2-3: 1;
the mass ratio of A to B is 1: 0.3-5.
Preferably, the mass ratio of the polyhexamethylene biguanide to the essential oil composition is 1: 3-5, and preferably, the mass ratio of the chlorhexidine gluconate to the essential oil composition is 1:0.3 to 1.0.
The auxiliary agent is one or more of solubilizer, thickener, humectant, algefacient, sour agent and sweetener.
The solubilizer is one or more of hydrogenated castor oil PEG-40/60/80, ethanol, tween, polyethylene oxide, polypropylene oxide and monobutyl ether. The thickener is one or more of poloxamer, hydroxyethyl cellulose, hydroxypropyl methylcellulose and xanthan gum. The humectant is one or more of silanized sodium hyaluronate, glycerin, pentanediol and nonanediol. The algefacient is one or more of menthol, oleum Menthae Dementholatum, and methyl salicylate. The sour agent is one or more of sodium citrate, citric acid, lactic acid, sodium lactate, sodium carbonate, sodium bicarbonate and vitamin C. The sweetener is one or more of sucrose, aspartame, xylitol and honey.
Further, the oral bacteriostatic composition comprises the following components in parts by weight: 2-50 parts of polyhexamethylene biguanide or chlorhexidine gluconate, 3-50 parts of an essential oil composition, 50-500 parts of a solubilizer, 20-2000 parts of a thickener, 0-1000 parts of a humectant, 0-200 parts of a sweetener, 0-30 parts of a freshener, 0-30 parts of a sour agent, and the balance of purified water to 10000 parts.
Preferably, the humectant comprises the following components in parts by weight: 200-500 parts of glycerol, 200-500 parts of pentanediol and 0-10 parts of silanized sodium hyaluronate.
Preferably, the thickener is hydroxyethyl cellulose or poloxamer. Preferably, the cooling agent is menthol. Preferably, the acidulant is sodium citrate.
The oral bacteriostatic composition of the invention comprises a liquid or gel (oral bacteriostatic gel), wherein the liquid comprises a spray or a mouthwash (oral bacteriostatic mouthwash).
Preferably, the oral bacteriostatic mouth wash comprises the following components in parts by weight: 2-5 parts of polyhexamethylene biguanide, 10-30 parts of an essential oil composition, 50-150 parts of ethanol, 50-150 parts of hydrogenated castor oil PEG-6050, 20-80 parts of a thickening agent, 400-600 parts of a humectant, 10-200 parts of a sweetening agent, 1-5 parts of a freshener, 5-20 parts of an acidulant and purified water in balance of 10000.
The preparation method of the oral bacteriostatic mouth wash comprises the following steps:
(1) mixing the essential oil composition, ethanol and hydrogenated castor oil PEG-60, and stirring to obtain phase A;
(2) mixing purified water, a thickening agent, a humectant and polyhexamethylene biguanide, and uniformly stirring to obtain a phase B;
(3) and adding the phase A into the phase B, stirring uniformly, adding the freshener, the sweetener and the sour agent, and stirring uniformly at room temperature to obtain the mouthwash.
Preferably, the gel comprises the following components in parts by weight: 20-50 parts of chlorhexidine gluconate, 10-30 parts of an essential oil composition, 50-150 parts of ethanol, 8050-150 parts of tween, 1000-2000 parts of a thickening agent, 400-600 parts of a humectant, 50-150 parts of a sweetening agent, 1-3 parts of a freshener, 5-20 parts of a sour agent and the balance of purified water to 10000.
The preparation method of the oral bacteriostatic gel comprises the following steps:
(1) mixing the essential oil composition, ethanol and tween 80 to obtain phase A;
(2) adding the thickening agent and the humectant into purified water, uniformly stirring, adding chlorhexidine gluconate, and uniformly stirring to obtain a phase B;
(3) dissolving freshener, sweetener and sour agent in water to obtain phase C;
(4) slowly adding phase A into phase B under stirring, mixing, adding phase C into A, B mixture, stirring, adding purified water to a specified weight, and stirring to obtain oral cavity antibacterial gel.
The oral bacteriostatic composition provided by the invention takes the disinfectants such as polyhexamethylene biguanide, chlorhexidine gluconate and the like and the essential oil composition of lavender essential oil, tea tree essential oil and garlic essential oil as main active ingredients. The garlic essential oil has good inhibiting and killing effects on various pathogenic bacteria such as staphylococcus, escherichia coli and other bacteria, the tea tree essential oil has the effects of diminishing inflammation and sterilizing, the lavender essential oil also has the effects of sterilizing and disinfecting, the sterilization spectrum and the sterilization effect of the lavender essential oil are expanded by compounding the garlic essential oil, the tea tree essential oil, the lavender essential oil and the lavender essential oil, and the garlic essential oil has good killing effects on staphylococcus aureus, escherichia coli, candida albicans, pseudomonas aeruginosa and the like. The four components are synergistic for antibiosis, so that the use amount of the disinfectant polyhexamethylene biguanide (chlorhexidine gluconate) is greatly reduced by more than 50%, and meanwhile, the lavender essential oil and the like are anti-inflammatory and can refresh breath, so that the oral liquid is very suitable for oral use.
The invention has the beneficial effects that: the composition takes the essential oil composition of disinfectants such as polyhexamethylene biguanide, chlorhexidine gluconate and the like and lavender essential oil, tea tree essential oil and garlic essential oil as main active ingredients, has good stability, not only has good bacteriostatic action, but also can effectively inhibit periodontitis and relieve pain, also can resist inflammation and refresh breath, has good mouthfeel, is convenient to use at any time, can be used for rapidly eliminating oral mucosa inflammation at a fixed point, and is convenient to use. The preparation of the invention selects the raw materials of pharmaceutical grade or food grade, and has good safety.
Detailed Description
The technical solution of the present invention will be further described with reference to the following specific examples. It is to be understood that the following examples are only illustrative of and illustrative of the present invention and are not to be construed as limiting the scope of the present invention. All the technologies implemented based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods. The compositions of the present invention are all food grade (or pharmaceutical grade).
Oral bacteriostatic mouth wash
1. Preparation of oral bacteriostatic mouth wash
The components and the mass of each component in examples 1 to 7 and comparative examples 1 to 2 are shown in Table 1.
TABLE 1 formulation (unit: g) of oral cavity antibacterial mouth rinse of examples 1 to 7 and comparative examples 1 to 2
Preparation of examples 1 to 7:
(1) adding ethanol into a container, sequentially stirring and adding the essential oil composition, uniformly stirring, and adding hydrogenated castor oil PEG-60 to obtain phase A;
(2) adding sufficient purified water into another container, adding poloxamer or hydroxyethyl cellulose as a thickening agent under stirring, stirring to obtain a uniform solution, adding glycerol, pentanediol and sodium silanized hyaluronate as humectants according to the formula amount, heating and stirring, adding polyhexamethylene biguanide after stirring uniformly, and stirring to obtain phase B;
(3) adding phase A into phase B under stirring, stirring for 30min, adding menthol as refreshing agent, xylitol as sweetener, sucrose, and sodium citrate as sour agent, stirring, and adding water to desired weight to obtain collutory.
Preparation of comparative example 1-2:
adding enough water into a container, adding poloxamer or hydroxyethyl cellulose, adding a humectant, uniformly stirring, adding polyhexamethylene biguanide, uniformly stirring, adding a freshener, a sweetener and an acidulant, uniformly stirring, and adding purified water to a specified weight to obtain comparative examples 1-2.
2. Mouth wash performance testing:
(1) and (4) testing standard:
the content is as follows: the content stability test was carried out according to 2.2.3.2.1 article of the Ministry of health, Disinfection technical Specification (2002 edition); detecting the content of polyhexamethylene biguanide in the bacteriostatic mouthwash according to the method in GB/T26367 and 2020;
appearance: carrying out appearance detection according to enterprise standards;
bacteriostasis: the bacteriostatic ability is detected according to annex C of GB 15979-2002 hygienic Standard for Disposable sanitary articles;
heavy metals: heavy metal limit detection is carried out according to Chinese pharmacopoeia (2020 edition);
(2) the test method comprises the following steps:
the samples were stored in an incubator at 37 ℃ for 90 days, and examined 1 time every 15 days.
The appearance, content, pH and heavy metal test were conducted for comparative examples 1-2 and examples 1-7.
Bacteriostatic experiments (Staphylococcus aureus ATCC6538, Escherichia coli ATCC8099, Candida albicans ATCC10231) were carried out for examples 1 to 7 and comparative examples 1 to 2.
Examples 1 to 7 and comparative examples 1 to 2 were subjected to 3-month stability examination and 14-day accelerated test.
(3) Test results
The results of the performance tests of examples 1 to 7 and comparative examples 1 to 2 are shown in Table 2.
TABLE 2 mouthwash test results
(4) And (3) analyzing an experimental result:
the high-temperature 54 ℃ accelerated test shows that: the products of 2 control examples and examples 1-7 were all stable.
Antibacterial experiments show that:
example 7 systems with only low concentrations of essential oil composition added, showed no significant bacteriostatic effect (less than 90%). Example 6 the result of adding only high concentration of essential oil shows that there is a certain bacteriostatic effect, but the effect is not ideal, and the tested bacteriostatic rate is less than 99%.
Comparative example 1, in which 0.2% polyhexamethylene biguanide was added, showed 99.99% inhibition rate; in comparative example 2, 0.03% of polyhexamethylene biguanide is added, the bacteriostasis rate of 99.99% is not reached after the action of the polyhexamethylene biguanide on escherichia coli and staphylococcus aureus is less than 20min, the bacteriostasis rate of 99.99% cannot be reached in candida albicans test (the bacteriostasis rate of only 58.6% in 2 min), and the low-concentration sample of the polyhexamethylene biguanide is basically under the lowest effective bacteriostasis concentration.
Example 1 adding low concentration polyhexamethylene biguanide 0.03% and low concentration essential oil 0.12%, the bacteriostatic effect on each strain can reach 99.99%; in example 2, the slightly high-concentration 0.1% polyhexamethylene biguanide and 0.25% essential oil are added, so that 99.99% of antibacterial effect can be achieved; the results show that the biguanide used concentration is reduced to 0.03% in the examples, so that the biguanide has a good bacteriostatic effect; examples 3 to 5, the addition of 0.1% polyhexamethylene biguanide and 0.2% total amount of two essential oils shows that 99.99% of bacteriostatic effect on escherichia coli and staphylococcus aureus can be achieved, but the bacteriostatic rate on candida albicans for 2min cannot reach 99.99%, and compared with example 1, the effect of the combination of the three essential oils is better than that of the combination of the two essential oils.
It can be seen that: through compounding, the antibacterial effect can be better achieved by 0.03% of polyhexamethylene biguanide and 0.12% of low-concentration essential oil, and compared with the method of adopting 0.2% of polyhexamethylene biguanide, the dosage of the polyhexamethylene biguanide is greatly saved. At the same time, it can be seen that: the polyhexamethylene biguanide and the essential oil composition have good compounding effect, and the dosage of effective components is greatly saved.
Examination at 37 ℃ for 90 days showed that the contents of examples 1 to 7 and comparative examples 1 to 2 were within acceptable ranges, although they were within small fluctuations.
Tests show that the essential oil composition selected in the composition combines with the polyhexamethylene biguanide, the essential oil compositions with different concentrations have obvious bacteriostasis and synergism, and the usage amount of the polyhexamethylene biguanide can be greatly reduced under the condition of ensuring effective bacteriostasis effect.
Second, oral cavity bacteriostatic gel
1. Preparation of oral cavity bacteriostatic gel
The composition and quality of the oral bacteriostatic gel are shown in table 3.
TABLE 3 formulation (unit: g) of oral cavity antibacterial gel of examples 8 to 14 and comparative example 3
The preparation processes of the embodiments 8 to 14 and the comparative example are as follows:
(1) adding solubilizer ethanol into a container, sequentially stirring and adding lavender essential oil, tea tree essential oil and garlic essential oil, uniformly stirring, and adding solubilizer Tween 80 to obtain phase A;
(2) adding sufficient purified water into a container, adding a mixture of a thickening agent poloxamer, humectant glycerol, pentanediol and silanized sodium hyaluronate under stirring, heating while stirring after uniform dispersion, adding a disinfectant chlorhexidine gluconate after the feed liquid is uniform and has no lumps, and uniformly stirring to obtain a phase B;
(3) dissolving a small amount of purified water with menthol as refreshing agent, xylitol as sweetener, aspartame, and sodium citrate as sour agent under stirring to obtain phase C;
(4) slowly adding phase A into phase B under stirring, mixing, adding phase C into A, B mixture, stirring, adding purified water to a specified weight, and stirring for more than 10min to obtain oral cavity antibacterial gel.
Comparative example C was added to B and stirred until homogeneous, purified water was added to the specified weight, and stirring was carried out for 10min or more to obtain comparative example gel.
2. Testing the performance of the oral bacteriostatic gel:
(1) and (4) testing standard:
the contents are as follows: according to 2.2.3.2.1 article of disinfection technical Specification (2002 edition), Ministry of health, performing content stability test, and detecting the content of chlorhexidine gluconate according to the method in GB/T26367-;
appearance: carrying out appearance detection according to enterprise standards;
bacteriostasis: carrying out bacteriostatic ability detection according to appendix C of GB 15979-2002 hygienic Standard for Disposable sanitary articles;
heavy metals: heavy metal limit detection is carried out according to Chinese pharmacopoeia (2020 edition);
(2) test method and results
Examples 8 to 14 and comparative example 3 were subjected to 3-month stability examination and 14-day accelerated test;
bacteriostatic experiments (staphylococcus aureus ATCC6538, candida albicans ATCC10231, escherichia coli ATCC8793) were performed for examples 8 to 14, and comparative example 3.
The test results of examples 8 to 14 and comparative example 3 are shown in Table 4;
TABLE 4 oral bacteriostatic gel test results
Description of the drawings: the killing logarithm value is less than 3.00, and no bacteriostatic effect exists.
(4) Analysis of results
Examination at 37 ℃ for 90 days shows that the contents of examples 8-13 and comparative example 3 have small fluctuation, and are within an acceptable range.
The comparative example 3 shows that the killing log values are all less than 3.00 by adding 50 parts of chlorhexidine gluconate gel, and the result shows that the chlorhexidine gluconate gel at the concentration does not achieve the ideal antibacterial effect;
examples 13 and 14, in which only high and low concentrations of essential oils were added, both showed a log kill value of less than 3.00, indicating that the essential oil composition gel formulation at this concentration did not achieve the desired bacteriostatic effect;
example 8 a killing effect with a log value of more than 5 can be achieved for each strain by adding 25 parts of chlorhexidine gluconate with low concentration and 12 parts of essential oil with low concentration; example 9 a slightly higher concentration of chlorhexidine gluconate 50 parts and essential oil 25 parts was added to achieve a kill effect with a log value greater than 5; the results show that chlorhexidine gluconate used in the examples at concentrations reduced to 25 parts combined with low concentrations of the essential oil composition has a better kill effect. Examples 10 to 12 show that addition of 25 parts of chlorhexidine gluconate and 20 parts of two total essential oils can achieve a killing effect on escherichia coli with a log value of greater than 5, but cannot achieve a killing effect on candida albicans and staphylococcus aureus with a log value of greater than 5 in a test of 1min, and compared with example 8, the effect of the combination of the three essential oils in the gel formulation is superior to that of the combination of the two essential oils.
Experiments show that the gel formulation is not beneficial to exerting the antibacterial effect, but the essential oil composition selected in the composition and the gel prepared by combining the chlorhexidine gluconate all show obvious antibacterial and synergistic effects.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, improvement and the like made within the spirit of the present invention shall be included in the protection of the present invention.
Claims (6)
1. An oral cavity antibacterial composition containing essential oil is characterized in that the oral cavity antibacterial composition is mouthwash, and comprises the following components in parts by weight: 2-5 parts of polyhexamethylene biguanide, 10-30 parts of an essential oil composition, 50-150 parts of ethanol, 50-150 parts of hydrogenated castor oil PEG-6050, 20-80 parts of a thickening agent, 400-600 parts of a humectant, 10-200 parts of a sweetening agent, 1-5 parts of a freshener, 5-20 parts of an acidulant and purified water, wherein the balance is 10000; the essential oil composition is prepared by compounding lavender essential oil, tea tree essential oil and garlic essential oil, wherein the mass ratio of the lavender essential oil to the tea tree essential oil to the garlic essential oil is 2-3: 1; the mass ratio of the polyhexamethylene biguanide to the essential oil composition is 1: 3-5.
2. An oral bacteriostatic composition containing essential oil is characterized by being a gel, and comprising the following components in parts by weight: 20-50 parts of chlorhexidine gluconate, 10-30 parts of an essential oil composition, 50-150 parts of ethanol, 8050-150 parts of tween, 1000-2000 parts of a thickening agent, 400-600 parts of a humectant, 50-150 parts of a sweetening agent, 1-3 parts of a freshener, 5-20 parts of a sour agent, and the balance of purified water to 10000; the essential oil composition is prepared by compounding lavender essential oil, tea tree essential oil and garlic essential oil, wherein the mass ratio of the lavender essential oil to the tea tree essential oil to the garlic essential oil is 2-3: 1; the mass ratio of the chlorhexidine gluconate to the essential oil composition is 1:0.3 to 1.0.
3. The oral bacteriostatic composition containing essential oil according to claim 1 or 2, which is characterized in that,
the thickening agent is one or more of poloxamer, hydroxyethyl cellulose, hydroxypropyl methyl cellulose and xanthan gum;
the humectant is one or more of silanized sodium hyaluronate, glycerin, pentanediol and nonanediol;
the algefacient is one or more of menthol, oleum Menthae Dementholatum, and methyl salicylate;
the sour agent is one or more of sodium citrate, citric acid, lactic acid, sodium lactate, sodium carbonate, sodium bicarbonate and vitamin C;
the sweetener is one or more of sucrose, aspartame, xylitol and honey.
4. The oral bacteriostatic composition containing essential oil according to claim 3,
the humectant comprises the following components in parts by weight: 200-500 parts of glycerol, 200-500 parts of pentanediol and 0-10 parts of silanized sodium hyaluronate;
the thickening agent is hydroxyethyl cellulose or poloxamer;
the freshener is menthol;
the sour agent is sodium citrate.
5. The method for preparing an essential oil-containing oral bacteriostatic composition according to claim 1, wherein the method for preparing the mouthwash comprises the following steps:
(1) mixing the essential oil composition, ethanol and hydrogenated castor oil PEG-60, and stirring to obtain phase A;
(2) mixing purified water, a thickening agent, a humectant and polyhexamethylene biguanide, and uniformly stirring to obtain a phase B;
(3) and adding the phase A into the phase B, stirring uniformly, adding the freshener, the sweetener and the sour agent, and stirring uniformly at room temperature to obtain the mouthwash.
6. The method for preparing an essential oil-containing oral bacteriostatic composition according to claim 2, wherein the method for preparing the gel comprises the following steps:
(1) mixing the essential oil composition, ethanol and tween 80 to obtain phase A;
(2) adding the thickening agent and the humectant into purified water, stirring uniformly, adding chlorhexidine gluconate, and stirring uniformly to obtain a phase B;
(3) dissolving freshener, sweetener and sour agent in water to obtain phase C;
(4) slowly adding phase A into phase B under stirring, mixing, adding phase C into A, B mixture, stirring, adding purified water to desired weight, and stirring to obtain gel.
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| CN114344184A (en) * | 2021-12-13 | 2022-04-15 | 中国科学技术大学 | Deodorizing oral spray |
| CN115350317B (en) * | 2022-08-30 | 2024-04-02 | 振德医疗用品股份有限公司 | Wound dressing composition and preparation method thereof |
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| CN104224923A (en) * | 2014-07-07 | 2014-12-24 | 海南华拓天涯制药有限公司 | Tea tree essential oil antimicrobial gel for treating vaginal disease in gynecology |
| CN104523513A (en) * | 2014-12-18 | 2015-04-22 | 东莞市阿比亚能源科技有限公司 | Tooth cleaning fluid |
| CN104997667A (en) * | 2015-07-01 | 2015-10-28 | 南阳市汇博生物技术有限公司 | Multifunctional antibacterial mouthwash and preparation method thereof |
| CN106619269A (en) * | 2016-10-14 | 2017-05-10 | 柳州环山科技有限公司 | Antiphlogosis antiallergic mouthwash and preparation method thereof |
| CN107198769A (en) * | 2017-05-04 | 2017-09-26 | 艾伯尔生物科技（重庆）有限公司 | Oral disinfecting spray and preparation method thereof |
| IE87094B1 (en) * | 2017-08-04 | 2020-05-13 | Laboratorios Kin S A | Gel comprising chlorhexidine |
| CN108403585A (en) * | 2018-04-18 | 2018-08-17 | 佛山科学技术学院 | A kind of mouthwash for treating canker sore |
| CN108938795A (en) * | 2018-09-10 | 2018-12-07 | 郁光雷 | The antibacterial spray of skin and its preparation process |
| CN111265556A (en) * | 2019-11-11 | 2020-06-12 | 五赫兹（厦门）医疗用品有限公司 | Medical oral bacteriostatic composition and preparation method and application thereof |
| CN110885717B (en) * | 2019-12-16 | 2022-04-08 | 株洲千金药业股份有限公司 | Natural antibacterial detergent for lady clothes |
| CN111920911B (en) * | 2020-07-08 | 2022-02-25 | 江苏正大清江制药有限公司 | Mosquito-proof disinfectant and preparation method thereof |
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