CN116459190A - Nasal cavity nursing liquid and preparation method thereof - Google Patents
Nasal cavity nursing liquid and preparation method thereof Download PDFInfo
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- CN116459190A CN116459190A CN202310401409.3A CN202310401409A CN116459190A CN 116459190 A CN116459190 A CN 116459190A CN 202310401409 A CN202310401409 A CN 202310401409A CN 116459190 A CN116459190 A CN 116459190A
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- 239000007788 liquid Substances 0.000 title claims abstract description 82
- 210000003928 nasal cavity Anatomy 0.000 title claims abstract description 80
- 230000000474 nursing effect Effects 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000004480 active ingredient Substances 0.000 claims abstract description 55
- 239000011248 coating agent Substances 0.000 claims abstract description 28
- 238000000576 coating method Methods 0.000 claims abstract description 28
- -1 pre-treating Substances 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 86
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 52
- 239000007787 solid Substances 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- 239000008367 deionised water Substances 0.000 claims description 32
- 229910021641 deionized water Inorganic materials 0.000 claims description 32
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 25
- AEMOLEFTQBMNLQ-AQKNRBDQSA-N D-glucopyranuronic acid Chemical compound OC1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O AEMOLEFTQBMNLQ-AQKNRBDQSA-N 0.000 claims description 21
- IAJILQKETJEXLJ-UHFFFAOYSA-N Galacturonsaeure Natural products O=CC(O)C(O)C(O)C(O)C(O)=O IAJILQKETJEXLJ-UHFFFAOYSA-N 0.000 claims description 21
- 229940097043 glucuronic acid Drugs 0.000 claims description 21
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 20
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 claims description 20
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 19
- 238000000605 extraction Methods 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 15
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 14
- 235000019441 ethanol Nutrition 0.000 claims description 14
- FALRKNHUBBKYCC-UHFFFAOYSA-N 2-(chloromethyl)pyridine-3-carbonitrile Chemical compound ClCC1=NC=CC=C1C#N FALRKNHUBBKYCC-UHFFFAOYSA-N 0.000 claims description 13
- 229940014800 succinic anhydride Drugs 0.000 claims description 13
- KIUKXJAPPMFGSW-DNGZLQJQSA-N (2S,3S,4S,5R,6R)-6-[(2S,3R,4R,5S,6R)-3-Acetamido-2-[(2S,3S,4R,5R,6R)-6-[(2R,3R,4R,5S,6R)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylic acid Chemical compound CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 KIUKXJAPPMFGSW-DNGZLQJQSA-N 0.000 claims description 12
- 235000011187 glycerol Nutrition 0.000 claims description 12
- 229920002674 hyaluronan Polymers 0.000 claims description 12
- 229960003160 hyaluronic acid Drugs 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 12
- 229920000053 polysorbate 80 Polymers 0.000 claims description 12
- 229920001661 Chitosan Polymers 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- 230000002195 synergetic effect Effects 0.000 claims description 9
- 241000245665 Taraxacum Species 0.000 claims description 7
- 235000005187 Taraxacum officinale ssp. officinale Nutrition 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 230000003204 osmotic effect Effects 0.000 claims description 6
- 239000008055 phosphate buffer solution Substances 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- LEAHFJQFYSDGGP-UHFFFAOYSA-K trisodium;dihydrogen phosphate;hydrogen phosphate Chemical compound [Na+].[Na+].[Na+].OP(O)([O-])=O.OP([O-])([O-])=O LEAHFJQFYSDGGP-UHFFFAOYSA-K 0.000 claims description 6
- 230000006196 deacetylation Effects 0.000 claims description 5
- 238000003381 deacetylation reaction Methods 0.000 claims description 5
- 238000001694 spray drying Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 4
- 210000004081 cilia Anatomy 0.000 abstract description 25
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- 241000894006 Bacteria Species 0.000 abstract description 11
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- 230000000052 comparative effect Effects 0.000 description 8
- 238000004140 cleaning Methods 0.000 description 7
- 206010039083 rhinitis Diseases 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
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- 206010028748 Nasal obstruction Diseases 0.000 description 4
- 230000007794 irritation Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 208000024891 symptom Diseases 0.000 description 4
- 241000269420 Bufonidae Species 0.000 description 3
- 206010019233 Headaches Diseases 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
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- 230000029058 respiratory gaseous exchange Effects 0.000 description 3
- 241000588724 Escherichia coli Species 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
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- 108010062010 N-Acetylmuramoyl-L-alanine Amidase Proteins 0.000 description 1
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Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
- A61K8/345—Alcohols containing more than one hydroxy group
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
- A61K8/4993—Derivatives containing from 2 to 10 oxyalkylene groups
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/735—Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/736—Chitin; Chitosan; Derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P11/00—Drugs for disorders of the respiratory system
- A61P11/02—Nasal agents, e.g. decongestants
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
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- A—HUMAN NECESSITIES
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- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/60—Particulates further characterized by their structure or composition
- A61K2800/61—Surface treated
- A61K2800/62—Coated
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- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/82—Preparation or application process involves sonication or ultrasonication
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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Abstract
The invention provides a nasal cavity nursing liquid and a preparation method thereof, and belongs to the field of nasal cavity nursing liquids. The preparation method of the nasal cavity nursing liquid comprises the following steps: extracting active ingredient, pre-treating, coating and preparing. The nasal cavity nursing liquid can effectively clean and care nasal cavities under the condition of low dosage; the nasal mucosa is not stimulated, so that the nasal mucosa can be nursed and repaired, and the possible problems of damage of nasal cilia and the like are effectively avoided; has good inhibition performance on bacteria and viruses.
Description
Technical Field
The invention relates to the field of nasal cavity nursing solutions, in particular to a nasal cavity nursing solution and a preparation method thereof.
Background
The human body is breathed to sustain life, and in the breathing process, the nasal cavity is contacted with the outside air first, and is the first guard of human respiratory system. The nasal cavity has narrow top and wide bottom long and narrow cavity structure, and is connected with the nasopharynx part from front nostril and back nostril. Most of the nasal cavity is covered by mucous membrane, cilia grow on the surface of the mucous membrane, and mucous secreted by goblet cells and other secretion cells is covered on the cilia, so that a mucous blanket which moves along with the cilia is formed on the surface of the mucous membrane, and a nasal mucous cilia system is formed.
The nasal cavity has effects of cleaning and filtering inhaled air, and regulating temperature. After entering the nasal cavity, the air is divided into laminar flow and turbulent flow, after being moderately heated and humidified, the dust is filtered through nasal hair of the nasal cavity, and foreign matters are discharged through reflecting sneeze or smaller dust particles entering the nasal cavity are subjected to turbulent flow, and the dust particles are settled on a mucus blanket on the surface of the nasal mucosa, are sent into the pharynx through continuous movement of the nasal cilia and are discharged from the oral cavity. Meanwhile, the mucus blanket also contains antibodies such as mucopolysaccharide, mucin, lysozyme, interferon, secretory IgA and the like, and can inhibit and eliminate adhered bacteria and viruses. It can be seen that the nasal cavity has a great significance for the health of the human body.
Through measurement and calculation, the adult can suck and exhale about 1.5 kiloliter of air every day, and the nasal cavity can deal with various external environments by means of the cleaning effect of the nasal mucus cilia system, and smooth breathing can be kept. However, with the continuous promotion of industrialization progress and the popularization of fuel vehicles, the problem of air pollution frequently occurs in recent years, the addition of haze is gradually increased in the whole year, and the content of pollutants such as dust, smog and the like in the air is also greatly increased, so that pollutants are remained in the vestibule of a nasal cavity in the breathing process of a human body, the pollutants gradually exceed the due cleaning capability of the nasal cavity, further dust dirt in the nasal cavity cannot be timely removed, the nasal hair is scabbed, and harmful substances such as dust, bacteria and viruses are accumulated, so that the normal nasal cilia cleaning function and the self sterilization function of the nasal cavity can be damaged, and various discomforts such as runny nose, sneeze, nasal obstruction and the like can be stimulated to be caused by nasal mucosa, so that the nasal cavity becomes a serious hidden danger for pathopoiesia. In the prior art, the nasal cavity is cleaned by adopting the nasal cavity care solution, so that the nasal cavity is kept clean, dirt such as dust, bacteria, viruses and allergic sources accumulated in the nasal cavity is removed, the state of nasal cavity congestion and edema is relieved, and the normal physiological function of the nasal cavity is maintained, so that the nasal cavity care solution is an important means for nasal cavity health care and rhinitis prevention.
However, the inventors have found that, in order to achieve an ideal nasal cavity care effect, it is generally necessary to clean and care both sides of the nasal cavity by 150 to 250mL of a nasal cavity care solution to thoroughly remove accumulated dust, bacteria, viruses, allergens and other contaminants in the nasal cavity. The existing nasal cavity nursing liquid can not realize effective cleaning and nursing of nasal cavities under the condition of low dosage, and can not effectively remove dust, bacteria, viruses, allergic sources and other dirt accumulated in the nasal cavities; meanwhile, the volatile components added in the existing nasal cavity care solution can stimulate nasal mucosa, so that nasal cilia can be damaged after long-term use, and the nasal mucosa can not be nursed and repaired while the nasal cavity is cleaned and nursed. Furthermore, the inhibition performance of the existing nasal cavity care solution on bacteria and viruses needs to be further improved.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a nasal cavity nursing liquid and a preparation method thereof, wherein the nasal cavity nursing liquid can effectively clean and care nasal cavities under the condition of low dosage; meanwhile, the nasal mucosa is not stimulated, so that the nasal mucosa can be nursed and repaired, and the possible problems of damage of nasal cilia and the like are effectively avoided; and has good inhibition performance on bacteria and viruses.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of a nasal cavity nursing liquid comprises the following steps: extracting active ingredient, pre-treating, coating and preparing.
The method comprises the steps of extracting active ingredients, placing dandelion whole herb in a constant temperature oven, drying at 40-50 ℃ until the moisture content is 3-7wt%, crushing to 80-100 meshes, then putting into an ethanol solution with 10-12 times of the weight of the dandelion whole herb, performing microwave-ultrasonic synergistic extraction for 20-30min, filtering out solid matters, and collecting a first filtrate; adding the solid into ethanol solution with the weight of 5-7 times of that of the solid, performing microwave-ultrasonic synergistic extraction again for 20-30min, filtering the solid, and collecting second filtrate; combining the first filtrate and the second filtrate, and spray drying to obtain active ingredient.
The concentration of the ethanol solution in the extracted active ingredients is 65-75% (volume percent);
in the microwave-ultrasonic collaborative extraction process, the extraction temperature is controlled to be 40-50 ℃, the microwave frequency is 2.1-2.3GHz, and the microwave power is 400-500W; the ultrasonic frequency is 30-35kHz, and the ultrasonic power is 500-600W.
The pretreatment, namely putting chitosan with the deacetylation degree of 80-90% into absolute ethyl alcohol with the weight of 8-10 times of that of the chitosan, and uniformly dispersing to prepare a first liquid; adding succinic anhydride into 20-22 times of absolute ethyl alcohol by weight, and stirring until the succinic anhydride is completely dissolved to prepare a second liquid; heating the first liquid to 50-60 ℃, and preserving heat; dropwise adding the second liquid at a dropwise adding rate of 5-8mL/min under the stirring condition; after the second liquid is added dropwise, preserving heat and stirring for 7-9 hours, and centrifugally separating to obtain a solid; washing the solid with 8-10 times of deionized water for 2-3 times, standing at 40-50deg.C, and drying to obtain pretreated product.
In the pretreatment, the weight ratio of the first liquid to the second liquid is 1:2.5-3.
The coating is carried out, the pretreated matter is put into deionized water, and the mixture is uniformly dispersed to prepare third liquid; uniformly mixing the third liquid with silver ammonia solution, heating to 50-60 ℃, and preserving heat; under the stirring condition, dripping the active ingredient solution at the dripping rate of 3-5mL/min, and finishing dripping the active ingredient solution; dripping glucuronic acid solution at the dripping rate of 1-3mL/min, and continuing to keep the temperature and stir for 20-50min after the dripping of the glucuronic acid solution is completed; centrifugal separation is carried out for 10-15min at 12000-15000rpm, thus obtaining solid matters; washing the solid with 8-10 times of deionized water for 2-3 times, standing at 40-50deg.C, and drying to obtain the final product.
In the coating, the content of the active ingredient in the active ingredient solution is 4-6wt%;
the concentration of glucuronic acid solution is 1-1.2mg/mL.
In the coating, the ratio of the pretreated matter to deionized water in the third liquid by weight is 1-1.5:100;
the concentration of the silver ammonia solution is 7-9mmol/L;
the volume ratio of the third liquid to the silver ammonia solution is 2.2-2.5:1;
the volume ratio of the silver ammonia solution to the active ingredient solution to the glucuronic acid solution is 1:0.4-0.5:0.7-0.8.
The preparation is prepared by uniformly mixing deionized water, tween 80, hyaluronic acid, a coating and glycerol, adopting disodium hydrogen phosphate-sodium dihydrogen phosphate buffer solution to adjust the pH value to 5.8-7.0, and then adopting sodium chloride to adjust the osmotic pressure to 290-300 mOsm/L.
In the preparation, the weight ratio of deionized water to tween 80 to hyaluronic acid to coating to glycerin is 100-110:0.5-0.8:1-2:4-5:2-3.
A nasal cavity care solution is prepared by the preparation method.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the preparation method of the nasal cavity care solution, the active ingredients are extracted through the steps of extracting the active ingredients, so that the active ingredients are prepared; simultaneously, a pretreatment step is set, and succinic anhydride is adopted to pretreat chitosan; preparing a pretreatment substance; and after the pretreatment substance is used for coating the active ingredients, the active ingredients are used in the preparation and matched with specific raw materials, so that the nasal cavity can be effectively cleaned and nursed under the condition of low dosage (85-90 mL); the nasal mucosa is not stimulated, so that the nasal mucosa can be nursed and repaired, and the possible problems of damage of nasal cilia and the like are effectively avoided; has good inhibition performance on bacteria and viruses.
(2) Through experiments, in the nasal cavity care solution disclosed by the invention, the continuous swing time of cilia on the surface of a mucous membrane is 649-659min in a cilia irritation experiment, so that the nasal cavity care solution has low irritation to the mucous membrane cilia, has no toxic or side effect, and can be used for caring and repairing the mucous membrane cilia.
(3) Through experiments, in the in-vitro bacteriostasis experiment, the nasal cavity nursing liquid provided by the invention can be diluted to 25%, and can still effectively inhibit staphylococcus aureus, escherichia coli and streptococcus pneumoniae, and the nasal cavity nursing liquid has good inhibition performance on bacteria and viruses.
(4) Through experiments, the nasal cavity nursing liquid can obviously improve nasal obstruction and headache symptoms caused by moderate rhinitis; the nasal cavity nursing liquid is continuously applied for 7 days, and the nose is obviously smooth; meanwhile, the single effective application amount is about 85-90mL, and the nasal cavity can be effectively cleaned and nursed under the condition of low use amount.
Detailed Description
Specific embodiments of the present invention will now be described in order to provide a clearer understanding of the technical features, objects and effects of the present invention.
Example 1
A preparation method of a nasal cavity nursing liquid specifically comprises the following steps:
1) Extracting active ingredient
Placing dandelion whole herb in a constant temperature oven, drying at 40 ℃ until the moisture content is 3wt%, crushing to 80 meshes, then putting into 10 times of ethanol solution, carrying out microwave-ultrasonic synergistic extraction for 20min, filtering out solid matters, and collecting first filtrate; adding the solid into ethanol solution with the weight of 5 times of that of the solid, performing microwave-ultrasonic synergistic extraction again for 20min, filtering the solid, and collecting second filtrate; combining the first filtrate and the second filtrate, and spray drying to obtain active ingredient.
Wherein the concentration of the ethanol solution is 65% (volume percent).
In the microwave-ultrasonic collaborative extraction process, the extraction temperature is controlled to be 40 ℃, the microwave frequency is 2.1GHz, and the microwave power is 400W; the ultrasonic frequency was 30kHz and the ultrasonic power was 500W.
2) Pretreatment of
Adding chitosan with the deacetylation degree of 80% into absolute ethyl alcohol with the weight being 8 times that of the chitosan, and uniformly dispersing to prepare a first liquid; adding succinic anhydride into 20 times of absolute ethyl alcohol by weight, and stirring until the succinic anhydride is completely dissolved to prepare a second liquid; heating the first liquid to 50 ℃, and preserving heat; dropwise adding the second liquid at a dropwise adding rate of 5mL/min under stirring; after the second liquid is added dropwise, preserving heat and stirring for 7 hours, and centrifugally separating to obtain a solid; washing the solid with 8 times of deionized water for 2 times, standing at 40deg.C, and drying to obtain pretreated product.
Wherein the weight ratio of the first liquid to the second liquid is 1:2.5.
3) Coating
Adding the pretreated matter into deionized water, and uniformly dispersing to prepare a third liquid; uniformly mixing the third liquid with silver ammonia solution, heating to 50 ℃, and preserving heat; under the stirring condition, dripping the active ingredient solution at the dripping rate of 3mL/min, and finishing dripping the active ingredient solution; dripping glucuronic acid solution at the dripping rate of 1mL/min, and continuing to keep the temperature and stir for 20min after the dripping of the glucuronic acid solution is completed; centrifugal separation is carried out at 12000rpm for 10min, thus obtaining solid matters; washing the solid with 8 times of deionized water for 2 times, standing at 40deg.C, and drying to obtain the final product.
In the third liquid, the weight ratio of the pretreatment to the deionized water is 1:100.
The concentration of the silver ammonia solution was 7mmol/L.
The volume ratio of the third liquid to the silver ammonia solution is 2.2:1.
The active ingredient content in the active ingredient solution was 4wt%.
The concentration of glucuronic acid solution was 1mg/mL.
The volume ratio of the silver ammonia solution, the active ingredient solution and the glucuronic acid solution is 1:0.4:0.7.
4) Formulations
Deionized water, tween 80, hyaluronic acid, a coating and glycerin are uniformly mixed, the pH value is regulated to 5.8 by adopting disodium hydrogen phosphate-sodium dihydrogen phosphate buffer solution, and then the osmotic pressure is regulated to 290mOsm/L by adopting sodium chloride, so that the nasal cavity nursing liquid is prepared.
Wherein, the weight ratio of deionized water, tween 80, hyaluronic acid, coating and glycerin is 100:0.5:1:4:2.
Example 2
A preparation method of a nasal cavity nursing liquid specifically comprises the following steps:
1) Extracting active ingredient
Placing dandelion whole herb in a constant temperature oven, drying at 45 ℃ until the moisture content is 4wt%, crushing to 90 meshes, then putting into 11 times of ethanol solution, performing microwave-ultrasonic synergistic extraction for 25min, filtering out solid matters, and collecting first filtrate; adding the solid into an ethanol solution with the weight being 6 times that of the solid, performing microwave-ultrasonic synergistic extraction again for 25min, filtering the solid, and collecting a second filtrate; combining the first filtrate and the second filtrate, and spray drying to obtain active ingredient.
Wherein the concentration of the ethanol solution is 70% (volume percent).
In the microwave-ultrasonic collaborative extraction process, the extraction temperature is controlled to be 45 ℃, the microwave frequency is 2.2GHz, and the microwave power is 450W; the ultrasonic frequency was 32kHz and the ultrasonic power was 550W.
2) Pretreatment of
Adding chitosan with the deacetylation degree of 85% into 9 times of absolute ethyl alcohol, and uniformly dispersing to prepare a first liquid; adding succinic anhydride into absolute ethyl alcohol with the weight being 21 times that of the succinic anhydride, and stirring until the succinic anhydride is completely dissolved to prepare a second liquid; heating the first liquid to 55 ℃, and preserving heat; dropwise adding the second liquid at a dropwise adding rate of 6mL/min under stirring; after the second liquid is added dropwise, preserving heat and stirring for 8 hours, and centrifugally separating to obtain a solid; washing the solid with 9 times of deionized water for 3 times, standing at 45deg.C, and drying to obtain pretreated product.
Wherein the weight ratio of the first liquid to the second liquid is 1:2.8.
3) Coating
Adding the pretreated matter into deionized water, and uniformly dispersing to prepare a third liquid; uniformly mixing the third liquid with silver ammonia solution, heating to 55 ℃, and preserving heat; under the stirring condition, dripping the active ingredient solution at the dripping rate of 4mL/min, and finishing dripping the active ingredient solution; dripping glucuronic acid solution at the dripping rate of 2mL/min, and continuing to keep the temperature and stir for 35min after the dripping of the glucuronic acid solution is completed; centrifugally separating at 13500rpm for 12min to obtain a solid; washing the solid with 9 times of deionized water for 3 times, standing at 45deg.C, and drying to obtain the coated product.
In the third liquid, the weight ratio of the pretreatment to the deionized water is 1.2:100.
The concentration of the silver ammonia solution is 8mmol/L.
The volume ratio of the third liquid to the silver ammonia solution is 2.3:1.
The active ingredient content in the active ingredient solution was 5wt%.
The concentration of glucuronic acid solution was 1.1mg/mL.
The volume ratio of the silver ammonia solution, the active ingredient solution and the glucuronic acid solution is 1:0.45:0.75.
4) Formulations
Deionized water, tween 80, hyaluronic acid, a coating and glycerin are uniformly mixed, the pH value is regulated to 6.0 by adopting disodium hydrogen phosphate-sodium dihydrogen phosphate buffer solution, and then the osmotic pressure is regulated to 295mOsm/L by adopting sodium chloride, so that the nasal cavity nursing liquid is prepared.
Wherein the weight ratio of deionized water, tween 80, hyaluronic acid, coating and glycerin is 105:0.6:1.5:4.5:2.5.
Example 3
A preparation method of a nasal cavity nursing liquid specifically comprises the following steps:
1) Extracting active ingredient
Placing dandelion whole herb in a constant temperature oven, drying at 50 ℃ until the moisture content is 7wt%, crushing to 100 meshes, then putting into 12 times of ethanol solution, performing microwave-ultrasonic synergistic extraction for 30min, filtering out solid matters, and collecting first filtrate; adding the solid into 7 times of ethanol solution, performing microwave-ultrasonic synergistic extraction again for 30min, filtering the solid, and collecting second filtrate; combining the first filtrate and the second filtrate, and spray drying to obtain active ingredient.
Wherein the concentration of the ethanol solution is 75% (volume percent).
In the microwave-ultrasonic collaborative extraction process, the extraction temperature is controlled to be 50 ℃, the microwave frequency is 2.3GHz, and the microwave power is 500W; the ultrasonic frequency was 35kHz and the ultrasonic power was 600W.
2) Pretreatment of
Adding chitosan with the deacetylation degree of 90% into 10 times of absolute ethyl alcohol, and uniformly dispersing to prepare a first liquid; adding succinic anhydride into 22 times of absolute ethyl alcohol by weight, and stirring until the succinic anhydride is completely dissolved to prepare a second liquid; heating the first liquid to 60 ℃, and preserving heat; dropwise adding the second liquid at a dropwise adding rate of 8mL/min under stirring; after the second liquid is added dropwise, preserving heat and stirring for 9 hours, and centrifugally separating to obtain a solid; washing the solid with 10 times of deionized water for 3 times, standing at 50deg.C, and drying to obtain pretreated product.
Wherein the weight ratio of the first liquid to the second liquid is 1:3.
3) Coating
Adding the pretreated matter into deionized water, and uniformly dispersing to prepare a third liquid; uniformly mixing the third liquid with silver ammonia solution, heating to 60 ℃, and preserving heat; under the stirring condition, dripping the active ingredient solution at the dripping rate of 5mL/min, and finishing dripping the active ingredient solution; dripping glucuronic acid solution at a dripping rate of 3mL/min, and continuing to keep the temperature and stir for 50min after the dripping of the glucuronic acid solution is completed; centrifugal separation at 15000rpm for 15min to obtain solid; washing the solid with 10 times of deionized water for 3 times, standing at 50deg.C, and drying to obtain the final product.
In the third liquid, the weight ratio of the pretreatment to the deionized water is 1.5:100.
The concentration of the silver ammonia solution is 9mmol/L.
The volume ratio of the third liquid to the silver ammonia solution is 2.5:1.
The active ingredient content in the active ingredient solution was 6wt%.
The concentration of glucuronic acid solution was 1.2mg/mL.
The volume ratio of the silver ammonia solution, the active ingredient solution and the glucuronic acid solution is 1:0.5:0.8.
4) Formulations
Deionized water, tween 80, hyaluronic acid, a coating and glycerin are uniformly mixed, the pH value is regulated to 7.0 by adopting disodium hydrogen phosphate-sodium dihydrogen phosphate buffer solution, and then the osmotic pressure is regulated to 300mOsm/L by adopting sodium chloride, so that the nasal cavity nursing liquid is prepared.
Wherein the weight ratio of deionized water, tween 80, hyaluronic acid, coating and glycerin is 110:0.8:2:5:3.
Comparative example 1
The technical scheme of the embodiment 2 is adopted, and the difference is that: extracting active ingredients, and omitting the addition of the active ingredients in the subsequent steps.
Comparative example 2
The technical scheme of the embodiment 2 is adopted, and the difference is that: 1) The coating step is omitted; 2) The preparation steps are modified, deionized water, tween 80, hyaluronic acid, active ingredients, pretreatment, nano silver antibacterial agent and glycerin are uniformly mixed, the pH value is regulated to 6.0 by adopting disodium hydrogen phosphate-sodium dihydrogen phosphate buffer solution, and then osmotic pressure is regulated to 295mOsm/L by adopting sodium chloride, so that the nasal cavity nursing liquid is prepared. Wherein, the weight ratio of deionized water, tween 80, hyaluronic acid, active ingredients, pretreatment, nano silver antibacterial agent and glycerin is 105:0.6:1.5:2.5:2.5:5:2.5.
The nasal cavity care solutions of examples 1 to 3 and comparative examples 1 to 2 were subjected to cilia irritation test, specifically: selecting 6 Chinese big toads with similar ages and weight of 45-50g, numbering the Chinese big toads as No. 1-6, supine fixing, washing by using normal saline, separating the palate mucous membrane (the area is 3mm x 3 mm) between two eyes of the Chinese big toads, spreading the palate mucous membrane on a glass slide to enable one surface with the mucous membrane to be upwards arranged, sucking water on the mucous membrane surface by using water absorbing paper, continuously sweeping the mucous membrane for 3min by using hot air at 35 ℃, respectively dripping 0.2mL of nasal cavity nursing liquid of examples 1-3 and comparative examples 1-2 into the mucous membrane No. 1-5, and dripping 0.2mL of normal saline into the mucous membrane No. 6 to serve as blank control samples; after standing for 30min, the cilia were covered with a glass and observed for cilia swinging under a microscope at 10 x 40 times, then placed under an environment at a temperature of 25 ℃ and a relative humidity of 60%, and the cilia were observed to stop swinging, and the cilia duration swinging time was recorded.
The longer the continuous swing time of cilia is, the lower the irritation and toxicity of the nasal cavity nursing liquid to the cilia of the mucous membrane are represented, and the better the cilia exercise function is recovered, the nasal cavity nursing liquid can be used for nursing and repairing the cilia of the mucous membrane.
The specific results are as follows:
further, in vitro bacteriostasis tests were carried out on the nasal cavity care solutions of examples 1 to 3 and comparative examples 1 to 2, respectively, specifically: the nasal cavity nursing solutions of the examples 1-3 and the comparative examples 1-2 are respectively diluted to 50 percent and 25 percent, and the nasal cavity nursing solution diluted to 50 percent and the nasal cavity nursing solution diluted to 25 percent are adopted for in vitro bacteriostasis activity tests; the test bacteria are staphylococcus aureus, escherichia coli and streptococcus pneumoniae; specific test methods refer to the relevant content in the test of determining the minimum inhibitory concentration of 2.1.7.3, the disinfection technical Specification. The specific results are as follows:
further, the nasal cavity care solutions of examples 1 to 3 and comparative examples 1 to 2 were tested for their application effects and effective application amounts, respectively, and specifically: 25 male and female volunteers with moderate rhinitis, 50 total, are selected from those with ages between 20 and 40. The randomization was divided into 5 groups, and each group was kept to consist of 5 male volunteers, 5 female volunteers. The nasal cavity nursing solutions of the examples 1-3 and the comparative examples 1-2 are adopted for cleaning and nursing the nasal cavities at two sides respectively, the cleaning and nursing are carried out for 2 times a day, after the continuous application is carried out for 7 days, the application effect is investigated, and the corresponding number of people is counted; and counting the single effective application amount.
Wherein, regarding the administration effect, the following three categories are included: has obvious effect, is effective and is ineffective. The obvious effect is that the nasal obstruction and headache symptoms caused by rhinitis are obviously improved, and the nose is obviously unobstructed. Effectively relieves nasal obstruction and headache symptoms caused by rhinitis, and the nose is smoother than before administration. The failure is that rhinitis symptoms are not changed obviously.
The specific results are as follows:
it can be seen that the nasal cavity care solution of the embodiments 1-3 of the present invention extracts dandelion active ingredients by setting the step of extracting active ingredients, and prepares active ingredients; simultaneously, a pretreatment step is set, and succinic anhydride is adopted to pretreat chitosan; preparing a pretreatment substance; and after the pretreatment substance is used for coating the active ingredients, the active ingredients are used in the preparation and matched with specific raw materials, so that the nasal cavity can be effectively cleaned and nursed under the condition of low dosage (85-90 mL); the nasal mucosa is not stimulated, so that the nasal mucosa can be nursed and repaired, and the possible problems of damage of nasal cilia and the like are effectively avoided; the antibacterial performance is good.
The percentages used in the present invention are mass percentages unless otherwise indicated.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the nasal cavity nursing liquid is characterized by comprising the following steps of: extracting active ingredients, pre-treating, coating and preparing;
the method comprises the steps of extracting active ingredients, drying and crushing dandelion herb, performing microwave-ultrasonic synergistic extraction for 2 times by adopting ethanol solution, merging extracting solutions, and spray drying to obtain the active ingredients;
the pretreatment, namely putting chitosan into absolute ethyl alcohol with the weight being 8-10 times that of the chitosan, and uniformly dispersing to prepare a first liquid; adding succinic anhydride into 20-22 times of absolute ethyl alcohol by weight, and stirring until the succinic anhydride is completely dissolved to prepare a second liquid; heating the first liquid to 50-60 ℃, and preserving heat; dropwise adding a second liquid under stirring; after the second liquid is added dropwise, preserving heat and stirring for 7-9 hours, and centrifugally separating to obtain a solid; washing the solid by deionized water and drying to obtain the pretreated product.
2. The method for preparing a nasal cavity care solution according to claim 1, wherein the coating comprises the steps of putting a pretreated substance into deionized water, and uniformly dispersing to prepare a third liquid; uniformly mixing the third liquid with silver ammonia solution, heating to 50-60 ℃, and preserving heat; dripping the active ingredient solution under the stirring condition, and after the dripping of the active ingredient solution is completed; dripping glucuronic acid solution, and continuing to keep the temperature and stir for 20-50min after the dripping of the glucuronic acid solution is completed; centrifugal separation to obtain solid; washing and drying the solid by deionized water to obtain a coating;
the preparation adopts the coating to prepare the nasal cavity nursing liquid.
3. The method for preparing a nasal care solution according to claim 1, wherein deionized water, tween 80, hyaluronic acid, a coating and glycerin are uniformly mixed, the pH value is adjusted to 5.8-7.0 by adopting disodium hydrogen phosphate-sodium dihydrogen phosphate buffer solution, and then the osmotic pressure is adjusted to 290-300mOsm/L by adopting sodium chloride to prepare the nasal care solution.
4. The method for preparing a nasal care solution according to claim 1, wherein the volume percentage concentration of the ethanol solution in the extracted active ingredient is 65-75%;
in the microwave-ultrasonic collaborative extraction process, the extraction temperature is controlled to be 40-50 ℃, the microwave frequency is 2.1-2.3GHz, and the microwave power is 400-500W; the ultrasonic frequency is 30-35kHz, and the ultrasonic power is 500-600W.
5. The method for preparing a nasal care solution according to claim 1, wherein in the pretreatment, the degree of deacetylation of chitosan is 80-90%;
the dropping speed of the second liquid is 5-8mL/min;
the weight ratio of the first liquid to the second liquid is 1:2.5-3.
6. The method for preparing a nasal care solution according to claim 2, wherein, in the coating,
the content of the active ingredient in the active ingredient solution is 4-6wt%;
the concentration of the glucuronic acid solution is 1-1.2mg/mL;
the dropping rate of the active ingredient solution is 3-5mL/min;
the dripping rate of the glucuronic acid solution is 1-3mL/min.
7. The method for preparing a nasal cavity care solution according to claim 2, wherein in the coating, the ratio of the pretreatment to deionized water in the third liquid is 1-1.5:100 by weight;
the concentration of the silver ammonia solution is 7-9mmol/L;
the volume ratio of the third liquid to the silver ammonia solution is 2.2-2.5:1.
8. The method for preparing a nasal cavity care solution according to claim 2, wherein in the coating, the volume ratio of the silver-ammonia solution, the active ingredient solution and the glucuronic acid solution is 1:0.4-0.5:0.7-0.8.
9. The method for preparing a nasal care solution according to claim 3, wherein the weight ratio of deionized water, tween 80, hyaluronic acid, coating and glycerin in the preparation is 100-110:0.5-0.8:1-2:4-5:2-3.
10. A nasal care solution prepared by the preparation method of any one of claims 1 to 9.
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