CN112843091B - Rhinitis antibacterial spray containing lignite extract and preparation method and application thereof - Google Patents

Rhinitis antibacterial spray containing lignite extract and preparation method and application thereof Download PDF

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CN112843091B
CN112843091B CN202110032625.6A CN202110032625A CN112843091B CN 112843091 B CN112843091 B CN 112843091B CN 202110032625 A CN202110032625 A CN 202110032625A CN 112843091 B CN112843091 B CN 112843091B
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王鹏云
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Yunnan Zhongyi Dingdong Energy Technology Development Co ltd
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Abstract

The invention relates to a rhinitis antibacterial spray containing a lignite extract and a preparation method and application thereof. The invention relates to a rhinitis bacteriostatic spray containing a lignite extract, which comprises the following compound raw materials: the feed additive comprises a lignite extract, a centipeda minima extract or a centipeda minima fresh grass juice, wherein the content of the centipeda minima extract or the centipeda minima fresh grass juice is 1-6% by weight. The beneficial effects are as follows: the rhinitis antibacterial spray is subjected to complete skin irritation test, and the irritation strength is nonirritant. The rhinitis bacteriostatic agent containing the lignite extract has the inhibition rate of 100 percent on staphylococcus aureus, escherichia coli, candida albicans and other bacteria within 2 minutes.

Description

Rhinitis antibacterial spray containing lignite extract and preparation method and application thereof
Technical Field
The invention relates to the technical field of bacteriostat, in particular to a rhinitis bacteriostat spray containing lignite extract and a preparation method and application thereof.
Background
Rhinitis, an inflammatory disease of the nasal cavity, is inflammation of the mucous membrane of the nasal cavity caused by viruses, bacteria, allergens, various physicochemical factors and certain systemic diseases. The main pathological changes of rhinitis are congestion, swelling, exudation, hyperplasia, atrophy or necrosis of the nasal mucosa. The health of the nasal cavity is related to the resistance of various respiratory diseases of the human body.
Centipeda minima, a traditional Chinese medicine, is a whole herb of Centipeda minima (L.) A.Braun e tAschers. Has effects of dispelling pathogenic wind and cold, relieving nasal obstruction, relieving cough, and removing toxic substance. It can be used for treating wind-cold type common cold, nasal obstruction, cough with asthma due to cold-phlegm, sore, carbuncle, and toxic swelling. Compendium of materia Medica: the goose eats grass and reaches the head and brain to treat the symptoms of head ache and eye disease, and the goose is flat and has no nose; treating phlegm malaria, sore and swelling by entering lung meridian; it is especially wonderful in removing nebula. The book Ben Cao Hui Yan (treatise on materia Medica): shihutuo, jiu Qiao, also can be used for relieving stuffy nose. Its flavor is pungent and drastic, its qi is pungent and smoked, its property is ascending and dispersing, it can dredge lung channel, it reaches head, so phlegm dyspnea, qi block obstruction, nasal obstruction and nasal hemorrhoid, swelling and stuffiness, remove nebula in eyes, and cold pathogen in head, headache and brain pain, all choose the pungent and temperature-rising to disperse the effect too. However, the single centipeda minima has the disadvantage of bacteriostasis, and a compound synergistic product is a trend to be developed.
Lignite is mineral coal with a relatively low coalification degree, is an initial product which is transformed into organic biogenic rock through dehydration and compaction after peat deposition, and is named because the external surface is brown or dark brown. The lignite storage capacity is large, but the defects of high moisture and high ash content are undoubtedly revealed and are difficult to utilize all the time, the key point is that the heat generation efficiency is influenced by the overhigh water content, so the lignite can be utilized only after being upgraded, the existing lignite drying and upgrading system directly uses the lignite as electric coal after drying the lignite, the water smoke after drying and upgrading the lignite is discharged after reaching the discharge standard, and the liquid is used as a byproduct of drying and upgrading the lignite. The applicant researches lignite drying and upgrading for a long time, accumulates core technologies, and finds that water smoke obtained after condensation, drying and upgrading contains rich short-chain fatty acids, ancient plant polyphenols, ancient plant aromatic substances, ancient alkaloids and other substances as lignite extracting solution, so that the water smoke has great utilization value in the antibacterial field.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a preparation process for overcoming the complexity of the existing rhinitis preparation, a plurality of additives are required to be added, a lignite extracting solution is obtained based on a lignite extracting solution or distilled lignite in a lignite drying and upgrading process, and a bacteriostatic agent containing the lignite extracting solution, a centipeda minima extract or a centipeda minima fresh grass juice and aiming at rhinitis, and a preparation method and application thereof. The extractive solution of lignite, the extract of herba Centipedae or the fresh juice of herba Centipedae has the functions of improving quality and enhancing efficacy for rhinitis bacteriostasis after being compounded. Develops a brand new rhinitis bacteriostatic spray.
The invention provides a rhinitis bacteriostatic spray containing a lignite extract, which has the technical scheme that:
a rhinitis bacteriostatic spray containing lignite extract comprises the following compound raw materials: the feed additive comprises a lignite extract, a centipeda minima extract or a centipeda minima fresh grass juice, wherein the content of the centipeda minima extract or the centipeda minima fresh grass juice is 1-6% by weight.
Preferably, the lignite extract comprises short-chain fatty acids, acetic acid and plant polyphenols.
Preferably, the lignite extract contains 0.05-0.2% of acetic acid, 0.05-0.2mg/L of archaea polyphenol and 0.02-0.1% of short chain fatty acid in terms of acetic acid.
Preferably, the lignite extracting solution is obtained by collecting water smoke generated in the upgrading and drying process of condensed lignite, and is extracted by a distillation process or a semi-distillation process;
the lignite extracting solution is a liquid obtained by extracting the middle part after being statically stored for a period of time.
Preferably, the content of the centipeda minima extract or the fresh centipeda minima juice is 2 to 4 percent by weight.
A preparation method of a rhinitis antibacterial spray containing a lignite extracting solution comprises the following steps:
(1) Firstly, standing and storing a lignite extracting solution for a period of time;
(2) Extracting the middle part as mother liquor;
(3) Adding 1-6% of centipeda minima extract or fresh centipeda minima juice into the mother solution by weight;
(4) Chelating at 70-90 deg.c for 2-4 hr;
(5) Filtering to remove residues to obtain the rhinitis antibacterial spray.
Preferably, in the step (1), the standing storage time is 2-3 months;
in the step (3), the content of the centipeda minima extract or the fresh centipeda minima juice is 2 to 4 percent;
in the step (4), chelating for 2.6-3.5 hours at the temperature of 75-85 ℃;
in the step (5), filter residues are removed by a filter with 500 meshes.
Preferably, the preparation method of the lignite extracting solution comprises the following steps: powdery lignite and high-temperature hot air with low oxygen content are introduced into a cavity of a drying device in a concurrent flow mode, the powdery lignite is depolymerized and dispersed at high speed in the drying device and directly contacts with the hot air to perform high-efficiency heat exchange, an induced draft fan is arranged at the tail end of an air outlet of the drying device, so that negative pressure is generated in the cavity of the drying device, water smoke in the drying device is led out under the action of the negative pressure, and after the water smoke is subjected to dust removal treatment, the water smoke is condensed to obtain lignite extract;
the temperature of the hot air flow is 600-1300 ℃, the oxygen content is less than 12%, the negative pressure in the cavity of the drying device is 900-6000 Pa, the flow rate of the hot air flow in the cavity is 8-18m/s, and the drying time of the lignite in the whole cavity is 1-5s.
A rhinitis antibacterial spray containing lignite extract is used for treating stuffy nose or nasal cavity inflammation.
Preferably, the bacteriostatic spray is used for inhibiting staphylococcus aureus, escherichia coli or candida albicans.
The implementation of the invention comprises the following technical effects:
1. the rhinitis bacteriostatic agent containing the lignite extract is a bacteriostatic agent which has broad spectrum, long effect, safety and no toxicity and is derived from ancient plants, has good inhibition effect on bacteria and fungi, and has inhibition and treatment effects on stuffy nose, rhinitis, nasal inflammation and the like.
2. The compound raw materials are safe and nontoxic: the lignite extract is nontoxic through acute oral toxicity experiments and chronic toxicological experiments.
3. Strong force and high efficiency: within 2 minutes, the rhinitis bacteriostatic agent containing the lignite extracting solution has the inhibition rate of 100 percent on staphylococcus aureus, escherichia coli, candida albicans and other bacteria.
4. Has no stimulation: the stimulation intensity is nonirritant through a complete skin stimulation experiment.
Detailed Description
The present invention will be described in detail with reference to the following examples, which are intended to facilitate the understanding of the present invention and should not be construed as limiting the scope of the present invention.
Example 1
The rhinitis bacteriostatic spray containing the lignite extract provided by the embodiment comprises the following compound raw materials: the feed additive comprises a lignite extract, a centipeda minima extract or a centipeda minima fresh grass juice, wherein the content of the centipeda minima extract or the centipeda minima fresh grass juice is 1-6% by weight. Experiments show that the lignite extract, the small centipeda herb extract or the small centipeda herb fresh juice is compounded to have the functions of improving the quality and enhancing the effect of bacteriostasis.
In this embodiment, the lignite extract solution includes short-chain fatty acids, acetic acid, and plant polyphenols. The brown coal extracting solution comprises the following components: contains 0.06% short chain fatty acid (calculated as acetic acid), 0.01% acetic acid, and 0.1mg/L of ancient plant polyphenol. Specifically, the lignite extracting solution is obtained by collecting water smoke in a condensed lignite extracting and drying process, and is extracted by a distillation process or a semi-distillation process; the lignite extracting solution is a liquid obtained by extracting the middle part after being statically stored for a period of time.
The preparation method of the rhinitis antibacterial spray containing the lignite extract provided by the embodiment comprises the following steps:
(1) Firstly, standing and storing the lignite extracting solution for 2-3 months;
(2) Extracting the middle part as mother liquor; the lignite extracting solution is stored in the liquid storage device for a period of time in a static mode, layering phenomena occur, small particles are deposited at the bottom of the lignite extracting solution, supernate is arranged at the top of the lignite extracting solution, the middle portion of the lignite extracting solution is relatively thick, and multiple times of experimental researches prove that the bacteriostatic agent prepared by the middle portion has a better effect.
(3) Adding 1-6% of small centipeda herb extract or small centipeda herb fresh juice into the mother solution;
(4) Chelating at 70-90 deg.c for 2-4 hr;
(5) Filtering to remove residues to obtain rhinitis antibacterial spray;
as a specific example:
(1) Firstly, standing and storing the lignite extracting solution for 3 months;
(2) Extracting the middle part as mother liquor;
(3) Adding 3% of centipeda minima extract or fresh centipeda minima juice into the mother solution;
(4) Chelating at 80 deg.c for 3 hr;
(5) And removing filter residues by using a 500-mesh filter to obtain the rhinitis antibacterial spray.
The bacteriostatic agent has a strong bacteriostatic function, contacts and adsorbs microorganisms, thereby inhibiting the splitting function of bacteria and viruses, leading the bacteria and the viruses to lose the reproductive capacity, blocking the breathing channel of the microorganisms and leading the microorganisms to die by suffocation. The lignite extract is rich in short-chain fatty acids, ancient plant polyphenols, ancient plant aromatic substances, ancient alkaloids and the like, and is a novel green antibacterial product.
As an example, the preparation method of the lignite extracting solution comprises the following steps: the method comprises the following steps of leading powdery lignite and high-temperature hot air flow with low oxygen content into a cavity of a drying device in a parallel flow mode, depolymerizing and dispersing the powdery lignite at a high speed in the drying device, directly contacting the powdery lignite with the hot air flow to carry out high-efficiency heat exchange, arranging a draught fan at the tail end of an air outlet of the drying device to enable the cavity of the drying device to generate negative pressure, leading out water and smoke in the drying device under the action of the negative pressure, and condensing the water and smoke to obtain a lignite extracting solution after dedusting the water and smoke; the temperature of the hot air flow is 600-1300 ℃, the oxygen content is less than 12%, the negative pressure in the cavity of the drying device is 900-6000 Pa, the flow rate of the hot air flow in the cavity is 8-18m/s, and the drying time of the lignite in the whole cavity is 1-5s. Preferably, the temperature of the hot gas stream is 901-1100 ℃. Furthermore, the water smoke can be condensed through the shift sprinkling technology, and the water smoke flows through the shift sprinkling plate and then is condensed into liquid, so that the equipment transformation cost is low, and the liquefaction effect is good. And discharging the dried lignite from the drying device to obtain the lignite high-efficiency coal powder which can be used as electric coal. In the embodiment, parameters such as negative pressure value, temperature, oxygen content and the like are limited, so that the dehydration rate of the drying method limited by the invention is greatly improved; the explosion critical value can not be reached, explosion can not occur, and the workshop operation is safe; the drying rate is high. The water content of the dried coal is well controlled, the granularity of the material is uniform, and the quality of the dried product is effectively guaranteed. The limitation of the invention ensures that the drying time of the material in the whole cavity is short, which can ensure high dehydration rate and can not cause the material to generate pyrolysis (combustion reaction), and the material is dried quickly and can not be stuck on the cavity shell. The beneficial substances carried in the water smoke under the condition can not be decomposed.
As an example, the centipeda minima extract is prepared by a method comprising the following steps:
s1, crushing dry whole centipeda minima, and extracting by a supercritical carbon dioxide extraction method to obtain a supercritical carbon dioxide extract of the centipeda minima;
s2, applying the centipeda minima supercritical carbon dioxide extract to a silica gel column, then eluting by using a mixed solvent, and collecting an elution part of the mixed solvent;
s3, placing the elution part of the mixed solvent on a gel column, eluting the gel column by using an organic solvent, analyzing, tracking and detecting by using GC-MS, collecting fractions with retention time of 80-120 min, concentrating under reduced pressure, and drying to obtain a centipeda minima extract;
wherein, the specific conditions of the supercritical carbon dioxide extraction method in the S1 are as follows: the extraction pressure is 20-30 MPa, the extraction temperature is 30-40 ℃, the flow rate is 15-25 liters/hour, and the extraction time is 1-3 hours;
wherein, the mixed solvent in S2 is a mixed solvent composed of petroleum ether and ethyl acetate, and the volume ratio of the mixed solvent is (9);
wherein, the type of the gel column in the S3 is SephadexLH-20, and the organic solvent is methanol.
The above methods are merely exemplary, and one skilled in the art may select other methods of preparation of the centipeda minima extract.
The fresh centipeda minima juice is prepared by cutting, smashing and twisting and pressing the fresh centipeda minima juice.
The implementation of the technical scheme of the invention has the following technical effects:
1. the invention has strong bacteriostatic function, and the lignite extract is used as mother liquor to be compounded with the centipeda minima extract or the fresh grass juice of the centipeda minima, so that the effect of the centipeda minima is exerted efficiently. The bacteriostasis rate of the antibacterial agent on staphylococcus aureus, escherichia coli and candida albicans reaches 99 percent through detection.
2. Contains no harmful substances such as iodine, aldehyde, chlorine, heavy metals, etc.
3. The invention is safe and nontoxic.
The rhinitis antibacterial spray containing the lignite extract has the following purposes: can be used for treating nasal obstruction, rhinitis, and nasal inflammation.
The rhinitis bacteriostatic agent containing the lignite extract is a bacteriostatic agent which has broad spectrum, long effect, safety and no toxicity and is derived from ancient plants, and compared with the existing commonly used rhinitis bacteriostatic agent, the rhinitis bacteriostatic agent has the following innovation points:
1. broad-spectrum long-acting antibiosis: the rhinitis bacteriostatic agent containing the lignite extract has good inhibition effect on bacteria and fungi.
2. The compound raw materials are safe and nontoxic: the lignite extract is non-toxic through acute oral toxicity experiments and chronic toxicological experiments.
3. Strong force and high efficiency: the rhinitis bacteriostatic agent containing the lignite extract has the inhibition rate of 100 percent on staphylococcus aureus, escherichia coli, candida albicans and other bacteria within 2 minutes.
4. No stimulation: the stimulation intensity is nonirritant through complete skin stimulation experiments.
Example 2
The preparation method of the rhinitis antibacterial spray containing the lignite extract provided by the embodiment comprises the following steps:
(1) Firstly, standing the lignite extracting solution for 2 months;
(2) Extracting the middle part as mother liquid;
(3) Adding 1% of Centipeda minima extract or Centipeda minima fresh grass juice into the mother liquor;
(4) Chelating at 70 ℃ for 2 hours;
(5) And removing filter residues by using a 500-mesh filter to obtain the rhinitis antibacterial spray.
Example 3
The preparation method of the rhinitis antibacterial spray containing the lignite extract provided by the embodiment comprises the following steps:
(1) Firstly, standing and storing the lignite extracting solution for 3 months;
(2) Extracting the middle part as mother liquor;
(3) Adding 6% of centipeda minima extract or fresh centipeda minima juice into the mother solution;
(4) Chelating at 90 deg.c for 4 hr;
(5) And removing filter residues by using a 500-mesh filter to obtain the rhinitis antibacterial spray.
Example 4
The preparation method of the rhinitis antibacterial spray containing the lignite extract provided by the embodiment comprises the following steps:
(1) Firstly, standing the lignite extracting solution for 2.5 months;
(2) Extracting the middle part as mother liquor;
(3) Adding 4% of herba Centipedae extract or fresh herba Centipedae juice into the mother liquor;
(4) Chelating for 2.6 hours at 75 ℃;
(5) And removing filter residues by using a 500-mesh filter to obtain the rhinitis antibacterial spray.
Example 5
The preparation method of the rhinitis antibacterial spray containing the lignite extract provided by the embodiment comprises the following steps:
(1) Firstly, standing the lignite extracting solution for 3.5 months;
(2) Extracting the middle part as mother liquor;
(3) Adding 2% of herba Centipedae extract or fresh herba Centipedae juice into the mother liquor;
(4) Chelating at 85 deg.C for 3.5 hr;
(5) And removing filter residues by using a 500-mesh filter to obtain the rhinitis antibacterial spray.
Example 6
The preparation method of the rhinitis antibacterial spray containing the lignite extract provided by the embodiment comprises the following steps:
(1) Firstly, standing and storing the lignite extracting solution for 3 months;
(2) Extracting the middle part as mother liquor;
(3) Adding 4% of herba Centipedae extract or fresh herba Centipedae juice into the mother liquor;
(4) Chelating at 80 ℃ for 3 hours;
(5) And removing filter residues by using a 500-mesh filter to obtain the rhinitis antibacterial spray.
The rhinitis bacteriostatic spray containing the lignite extracting solution is subjected to a bacteriostatic experiment and is detected, and the result is recorded as follows:
a first part: microbial detection
1. Equipment
1. Nutrient agar culture medium; 2. a Sabouraud agar medium; 3. lactose bile salt fermentation medium; SCDLP liquid culture medium; 5. glucose nutrient broth; 6. cetyl trimethyl ammonium bromide agar; 7. blood agar plates; 8. an electrothermal constant-temperature incubator; 9. a mould incubator; 10. an autoclave; 11. an electronic scale; 12. a biological safety cabinet; 13. clean bench.
2. Method of producing a composite material
The test was carried out according to GB15979 2002 "hygienic Standard for Disposable sanitary articles" appendix B "method for detecting product microorganisms".
3. As a result, the
TABLE 1 results of microbial detection
Figure BDA0002892049290000101
4. Conclusion
The microbial detection results of the rhinitis bacteriostatic agent containing the lignite extracting solution all conform to the regulation of GB15979-2002 hygienic Standard for Disposable sanitary articles.
A second part: staphylococcus aureus bacteriostatic performance test
1. Equipment
1. Experimental strains: staphylococcus aureus (ATCC 6538) was cultured for the third generation and provided by the research and development center of food microbial safety engineering in Guangdong province.
2. Culture medium: nutrient agar medium.
3. An instrument device: an electric heating constant temperature incubator and a biological safety cabinet.
2. Method for producing a composite material
1. The test is carried out according to the method for testing the sterilization performance, the bacteriostatic performance and the stability of the product in appendix C of GB15979-2002 sanitary Standard for Disposable sanitary articles.
2. The rhinitis bacteriostatic agent containing brown coal extract is used for respectively treating Staphylococcus aureus for 2min,5min,10min, and 20min, and the test is repeated for 3 times at 20 deg.C and 1 deg.C.
3. Results
The results of three repeated tests at 20 ℃ and 1 ℃ show that: the average bacteriostasis rate of the rhinitis bacteriostat containing the lignite extracting solution to staphylococcus aureus is 100 percent, and the results are shown in the following table:
TABLE 2 rhinitis bacteriostatic action of bacteriostatic agent containing brown coal extract on staphylococcus aureus
Figure BDA0002892049290000111
4. Conclusion
After the three times of repeated treatment, the rhinitis bacteriostatic agent containing the lignite extracting solution acts for 2min,5min,10min and 20min respectively, the bacteriostatic rate of staphylococcus aureus is 100 percent, and the product has strong bacteriostatic action.
And a third part: escherichia coli bacteriostatic performance test
1. Equipment
1. Strain: escherichia coli 8099, 3 rd generation, was provided by the research and development center of food microbial safety engineering, guangdong province.
2. Culture medium: nutrient agar medium.
3. An instrument device: an electric heating constant temperature incubator and a biological safety cabinet.
Test method
1. The test is carried out according to the method for testing the sterilization performance, the bacteriostasis performance and the stability of the product in appendix C of GB15979-2002 hygienic Standard for Disposable sanitary articles.
2. The rhinitis bacteriostatic agent containing brown coal extract is applied to Escherichia coli for 2min,5min,10min, and 20min, and the test is repeated 3 times at 20 deg.C and 1 deg.C.
3. Results
The results of three repeated tests at 20 ℃ and 1 ℃ show that: the average bacteriostasis rate of the rhinitis bacteriostat containing the lignite extracting solution to escherichia coli is 100 percent, and the result is shown in the following table:
TABLE 3 bacteriostatic action of rhinitis bacteriostatic agent containing lignite extract on escherichia coli
Figure BDA0002892049290000121
4. Conclusion
After the three times of repeated treatment, the rhinitis bacteriostatic agent containing the lignite extracting solution acts for 2min,5min,10min and 20min respectively, the bacteriostatic rate of escherichia coli is 100%, and the product has strong bacteriostatic action.
The fourth part: candida albicans bacteriostasis test
1. Equipment
1. The strain is as follows: candida albicans (ATCC 10231), third generation cultured, supplied by North Na Biotech Limited.
2. The formula of the neutralizer is as follows: an aqueous solution containing 2.1% lecithin +2.0% glucose +2.4% sodium thiosulfate +1.5% tween 80+0.5% peptone +1.2% sodium sulfite.
2. Culture medium: nutrient agar medium.
3. An instrument device: a constant temperature and humidity incubator, an electric heating constant temperature incubator and a biological safety cabinet.
2. Method of producing a composite material
1. The test is carried out according to the method for testing the sterilization performance, the bacteriostatic performance and the stability of the product in appendix C of GB15979-2002 hygienic Standard for Disposable sanitary articles.
2. The rhinitis bacteriostatic agent containing brown coal extract is used for respectively treating Candida albicans for 2min,5min,10min and 20min, and the test is repeated for 3 times at 20 deg.C and 1 deg.C.
3. As a result, the
The results of three repeated experiments under the conditions of 20 ℃ and 1 ℃ show that: the average bacteriostasis rate of the primary liquid of the bacteriostatic agent for a while to candida albicans is 100%, and the result is shown in the following table:
TABLE 4 rhinitis bacteriostatic action of bacteriostatic agent containing lignite extract on Candida albicans
Figure BDA0002892049290000131
4. Conclusion
After the three times of repeated treatment, the rhinitis bacteriostatic agent containing the lignite extracting solution acts for 2min,5min,10min and 20min respectively, the bacteriostatic rate of the product on the candida albicans is 100 percent, and the product has strong bacteriostatic action.
The fifth part is that: stability test (37 ℃,90 days, candida albicans)
1. Apparatus
1. Strain: candida albicans (ATCC 10231), third generation cultured and supplied by North Na institute of Biotechnology Limited.
2. The formula of the neutralizer is as follows: an aqueous solution containing 2.1% lecithin +2.0% glucose +2.4% sodium thiosulfate +1.5% tween 80+0.5% peptone +1.2% sodium sulfite.
2. Culture medium: nutrient agar culture medium
3. The instrument equipment comprises: a constant temperature and humidity incubator, an electric heating constant temperature incubator and a biological safety cabinet.
2. Method for producing a composite material
1. The test is carried out according to the method for testing the sterilization performance, the bacteriostatic performance and the stability of the product in appendix C of GB15979-2002 sanitary Standard for Disposable sanitary articles.
2. The stability test comprises storing rhinitis bacteriostatic agent containing brown coal extract at 37 deg.C for 90 days, respectively treating Candida albicans with the stock solution for 2min,5min,10min, and 20min, and repeating the test at 20 deg.C and 1 deg.C for 3 times.
3. As a result, the
The results of 3 times of repeated tests at 20 ℃ and 1 ℃ of soil show that: after the bacteriostatic agent is stored for 90 days at 37 ℃, the stock solution of the bacteriostatic agent acts on candida albicans for 2min, the average bacteriostatic rate is 100%, and the results are shown in the following table:
TABLE 5 rhinitis bacteriostatic action of bacteriostatic agent containing lignite extract on Candida albicans
Figure BDA0002892049290000141
4. Conclusion
The rhinitis bacteriostatic agent containing lignite extract has average bacteriostatic rate of 100% for 2min,5min,10min and 20min after being preserved at 37 deg.C for 90 days, and the product has bacteriostatic effect at room temperature for at least two years.
A sixth part: multiple complete skin irritation test
1. Test materials and methods
1. The test substance: rhinitis bacteriostatic agent containing lignite extract.
2. Animals: common-grade guinea pigs, provided by suzhou lake bridge biotechnology limited, animal certification No.: 20200702152.
3. Environmental conditions: room temperature: 20 ℃ to 25 ℃, relative humidity: 40 to 70 percent.
4. The test method comprises the following steps: according to the multiple complete skin irritation tests of the ' Disinfection technical Specification ' (2002 edition) ' of Ministry of health, 24 hours before test, the hairs on two sides of the spinal column of an experimental animal are cut off, the skin is not damaged, the hair removal range is 3cmx3cm respectively, 0.5mL of a tested object is taken on the next day, the tested object is directly coated on the complete skin with the hair removed on one side with the area of 2.5cmX2.5cm, the whole skin is covered by a layer of oil paper and is fixed by using a non-irritant adhesive plaster, the covering is removed after 4 hours, the tested object is removed by using warm water, the tested object is coated once a day and is continuously coated for 14 days, the result is observed and scored 24 hours after each coating, and the method of the control area is the same as that of the test area.
2. Test results
TABLE 6 rhinitis bacteriostat multiple skin irritation response scores containing lignite extract
Figure BDA0002892049290000151
Figure BDA0002892049290000161
3. Conclusion
The rhinitis bacteriostatic agent containing the lignite extract has an integral average value of 0.0 for skin irritation reaction of experimental animals, and has no irritation.
A seventh part: detection of lead, arsenic and mercury content
1. Equipment
Test samples: rhinitis bacteriostatic agent containing lignite extract.
Reagent name and concentration: superior pure nitric acid.
2. Method for producing a composite material
The detection basis is as follows: safety technical Specification for cosmetics (2015 year edition)
Detection conditions are as follows: ambient temperature 20.6 ℃ and humidity 46% RH. Number of sample repetitions: 2 times.
3. As a result, the
Table 7 test results of the content of Pb, as and Hg in the sample
Figure BDA0002892049290000162
Figure BDA0002892049290000171
4. Conclusion
The lead content in the rhinitis bacteriostatic agent containing the lignite extracting solution in the sample is less than 0.090mg/kg; the arsenic content is 0.0061mg/kg; the mercury content is less than 0.0033mg/kg, and meets the standard requirements of technical safety standards of cosmetics (2015 edition).
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (6)

1. A preparation method of rhinitis antibacterial spray containing lignite extract is characterized by comprising the following steps:
(1) Firstly, standing and storing a lignite extracting solution for a period of time;
(2) Extracting the middle part as mother liquor;
(3) Adding 1-6% of small centipeda herb extract or fresh small centipeda herb juice by weight into the mother solution;
(4) Chelating at 70-90 deg.c for 2-4 hr;
(5) Filtering to remove residues to obtain the rhinitis antibacterial spray.
2. The preparation method of the rhinitis antibacterial spray containing the lignite extracting solution as claimed in claim 1, wherein the preparation method comprises the following steps:
in the step (1), the standing storage time is 2-3 months;
in the step (3), the content of the centipeda minima extract or the fresh grass juice of the centipeda minima is 2 to 4 percent;
in the step (4), chelating for 2.6-3.5 hours at the temperature of 75-85 ℃;
in the step (5), filter residues are removed by using a 500-mesh filter.
3. The preparation method of the rhinitis antibacterial spray containing the lignite extracting solution according to claim 1, which is characterized by comprising the following steps: the preparation method of the lignite extract comprises the following steps: the method comprises the following steps that powdery lignite and high-temperature hot air with low oxygen content are led into a cavity of a drying device in a cocurrent flow mode, the powdery lignite is depolymerized and dispersed at a high speed in the drying device and directly contacted with the hot air to perform high-efficiency heat exchange, an induced draft fan is arranged at the tail end of an air outlet of the drying device, so that negative pressure is generated in the cavity of the drying device, water smoke in the drying device is led out under the action of the negative pressure, and after the water smoke is subjected to dust removal treatment, the water smoke is condensed to obtain a lignite extracting solution;
the temperature of the hot air flow is 600-1300 ℃, the oxygen content is less than 12%, the negative pressure in the cavity of the drying device is 900-6000 Pa, the flow rate of the hot air flow in the cavity is 8-18m/s, and the drying time of the lignite in the whole cavity is 1-5s.
4. The preparation method of the rhinitis antibacterial spray containing the lignite extracting solution according to claim 1, which is characterized by comprising the following steps: the lignite extract comprises short-chain fatty acid, acetic acid and plant polyphenol.
5. The preparation method of the rhinitis antibacterial spray containing the lignite extracting solution according to claim 1, which is characterized by comprising the following steps: the lignite extract contains 0.05-0.2% of acetic acid, 0.05-0.2mg/L of ancient plant polyphenol and 0.02-0.1% of short chain fatty acid in terms of acetic acid.
6. The preparation method of the rhinitis antibacterial spray containing the lignite extracting solution as claimed in claim 1, wherein the preparation method comprises the following steps: the prepared bacteriostatic spray is used for inhibiting staphylococcus aureus, escherichia coli or candida albicans.
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CN102048784A (en) * 2009-11-10 2011-05-11 董根荣 Spray for treating rhinitis and preparation method thereof
CN105770211A (en) * 2016-03-15 2016-07-20 东莞市达庆医疗器械有限公司 Medical rhinitis antibacterial agent and preparation method thereof
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