CN104740141B - A kind of antimicrobial spray and preparation method thereof - Google Patents

A kind of antimicrobial spray and preparation method thereof Download PDF

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Publication number
CN104740141B
CN104740141B CN201510180437.2A CN201510180437A CN104740141B CN 104740141 B CN104740141 B CN 104740141B CN 201510180437 A CN201510180437 A CN 201510180437A CN 104740141 B CN104740141 B CN 104740141B
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antimicrobial spray
ethyl
ethyl alcohol
parts
antimicrobial
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CN104740141A (en
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陈泽楚
陈锦涛
李婷
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Guangdong Taibao Medical Science Technology Co Ltd
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Guangdong Taibao Medical Science Technology Co Ltd
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Abstract

The present invention provides a kind of antimicrobial spray and preparation method thereof, according to parts by weight includes: 0.2 ~ 1 part of water soluble chitosan, 0.05 ~ 0.1 part of ethyl-para-hydroxybenzoate, 0.5 ~ 3 part of medicinal glycerin, 0.1 ~ 0.5 part of Alose, 1 ~ 5 part of ethyl alcohol, 95 ~ 99 parts of purified water.It fetches water first soluble chitosan, Alose and purified water, is mixed and stirred for 10min to uniform;Then ethyl-para-hydroxybenzoate, medicinal glycerin and ethyl alcohol are taken, first ethyl-para-hydroxybenzoate is dissolved with ethyl alcohol, add medicinal glycerin, 5 min are stirred to uniform, two kinds of solution obtained above is mixed, and stirs 5 min to uniform, adjusts the pH value of mixed solution to 5 ~ 7 with ammonium hydroxide, then it is sub-packed in spray bottle, the antimicrobial spray is obtained after radiation sterilization.The antimicrobial spray film-formation result prepared using this method is good, and places for a long time, and the molecular mass of carboxymethyl chitosan will not obvious degradation.

Description

A kind of antimicrobial spray and preparation method thereof
Technical field
The present invention relates to medical preparation fields more particularly to a kind of antimicrobial spray and preparation method thereof.
Background technique
Chitosan is chitin through a kind of deacetylated macromolecule glycosaminoglycan obtained, at present in the world unique band sun from The macromolecule alkalinity polysaccharide polymer of son.Chitosan is not soluble in water, can only be dissolved in weak acid, but its modified product, such as carboxylic first The modified obtained carboxymethyl chitosan of baseization can be directly dissolved in water, considerably increase its application range.It is abundant on strand Hydroxyl and amino make it easily occur to chemically react and have multiple functions, have hemostasis, analgesic, promote wound healing, reduce scar The excellent performances such as trace, antibacterial, good physiological compatibility and biodegradability.The antibacterial action of chitosan is mainly manifested in Have to bacterial strains such as staphylococcus epidermis, staphylococcus aureus, Escherichia coli, pseudomonas aeruginosa, Candida albicans There is inhibiting effect.The antibacterial principle of chitosan mainly includes following several respects: first is that due to the polycation of chitosan, easily In the negatively charged group effect of fungal cell surface, to change the mobility and permeability of pathogen cell membrane;Second is that dry Disturb the duplication and transcription of DNA;Third is that blocking pathogen metabolism.Chitosan and its derivative has following function: (1) chitosan can To promote the growth of epithelial cell and normal fibroblast, accelerating wound healing;(2) glycan has red blood cell obvious and direct Adhesion and agglutination, can promote platelet adhesion reaction and aggregation, quick-acting haemostatic powder;(3) chitosan is sprayed onto surface of a wound film forming, is The surface of a wound creates slightly sour, anaerobic or hypoxemia, appropriate wet, relative closure ideal healing environment, while chitosan can be absorbed Inflammatory substances-blood the bradykinin for leading to pain in wound, plays analgesic activity.
Ethyl-para-hydroxybenzoate is that the Antimicrobial preservative effect obtained after P-hydroxybenzoic acid (phenolic acid) carboxyl esterification is better than The substance of phenolic acid.The chain carrier of the substance has α, beta-unsaturated carbonyl structure, by ketonic oxygen and α-carbon group in molecule At the electronic relay system at a distance of about 0.25 ran, what is formed between carbonyl p electronics and adjacent ethylene linkage pi-electron grips effect altogether, With strong electronics buffer capacity, thus there is stronger antibacterial activity;Ester compounds exist simultaneously with molecular forms, in electricity Property, it penetrates readily through the cell membrane of microorganism and generates bacteriostasis.
Currently, the illness rate of gynecological disease is higher, for example vaginitis, cervicitis, cervical erosion etc. are all that women is common more Morbidity, now in rising year by year trend, and phenomena such as clinically common light degree Ⅱ burn and scald, canker sore, trauma surface infestation Also increase year by year.The antibacterial agent of the treatment surface of a wound and gynecological disease that occur in the market, which is substantially all, to be had the following problems: (1) being selected Chitosan be only dissolve in weak acid, cannot be directly dissolved in water, most of using acetic acid as solvent, such chitosan anti-bacteria Effect is relatively good, but chitosan is placed for a long time in weak acid, is easy to make the main chain of chitosan molecule to degrade, leads to molecule matter Amount decline;(2) using single chitosan as the main component of antibacterial agent, although chitosan is protected as externally used antimicrobial agent and the surface of a wound Managing agent has preferable effect, but the Shortcomings in terms of killing intractable pathogenic bacteria;(3) most of product in the treatment surface of a wound and When certain gynecological diseases, since retention time is short, the performance of dressing function is greatly reduced;(4) most of chitosan class antibacterial After the sterilizing of agent product, with the increase of resting period, the stability of product property declines.(5) most of antibacterial agent is that Chinese medicine mentions Object is taken to configure, there are formula components complexity, products without reparation conditioning functions for these products.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of antimicrobial sprays and preparation method thereof, are prepared using this method Antimicrobial spray film-formation result it is good, cracking can form one layer of soft transparent membrane on the surface of a wound and therapentic part surface layer, can So that spray permanence plays a role in wound repairing and therapentic part, and place for a long time, the molecule of carboxymethyl chitosan Quality will not obvious degradation.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of antimicrobial spray includes: 0.2 ~ 1 part of water soluble chitosan according to parts by weight, ethyl-para-hydroxybenzoate 0.05 ~ 0.1 part, 0.5 ~ 3 part of medicinal glycerin, 0.1 ~ 0.5 part of Alose, 1 ~ 5 part of ethyl alcohol, 95 ~ 99 parts of purified water.
Further, the water soluble chitosan is carboxymethyl chitosan.
Further, the purity of the medicinal glycerin is greater than 99.8%.
Further, the concentration of the ethyl alcohol is 95%.
The preparation method of the antimicrobial spray, comprising the following steps:
S1. it fetches water soluble chitosan, Alose and purified water, is mixed and stirred for 10min to uniform;
S2. ethyl-para-hydroxybenzoate, medicinal glycerin and ethyl alcohol are taken, is first dissolved ethyl-para-hydroxybenzoate with ethyl alcohol, Add medicinal glycerin, 5 min of stirring are to uniform;
S3. solution made from solution made from S1 and S2 is mixed, and stirs 5 min to uniform, adjusted and mixed with ammonium hydroxide Then the pH value of solution is sub-packed in spray bottle to 5 ~ 7, the antimicrobial spray is obtained after radiation sterilization.
Further, the water soluble chitosan is carboxymethyl chitosan.
Further, the purity of the medicinal glycerin is greater than 99.8%.
Further, the concentration of the ethyl alcohol is 95%.
Compared with prior art, the present invention having the following beneficial effects:
Antimicrobial spray prepared by the present invention can it is cracking the surface of a wound and therapentic part surface layer formed one layer it is soft transparent Film prevents the infection of the surface of a wound, is conducive to spray and persistently plays a role, wound repairing and therapentic part;P-hydroxybenzoic acid second The addition of ester makes the property of antimicrobial spray become highly stable, will not have floccule precipitating to occur because long-time is stored;The spray Agent have good antibacterial effect, the germs such as fungi, mould, bacterium, virus can be killed, can be used for either shallow burn and scald, bedsore, The infection of the skin wounds such as canker sore, gynecological disease, operation and trauma wound.
Specific embodiment
The present invention is a kind of antimicrobial spray, according to parts by weight includes: 0.2 ~ 1 part of water soluble chitosan, para hydroxybenzene first 0.05 ~ 0.1 part of acetoacetic ester, 0.5 ~ 3 part of medicinal glycerin, 0.1 ~ 0.5 part of Alose, 1 ~ 5 part of ethyl alcohol, 95 ~ 99 parts of purified water.
Further detailed description, but implementation of the invention are done to specific preparation method of the invention below with reference to embodiment Mode is without being limited thereto.
Embodiment 1
A kind of antimicrobial spray includes following components: 0.2 part of water soluble chitosan, P-hydroxybenzoic acid according to parts by weight 0.05 part of ethyl ester, 0.5 part of medicinal glycerin, 0.1 part of Alose, 1 part of ethyl alcohol, 95 parts of purified water.
The production technology of the antimicrobial spray the following steps are included:
The first step weighs water soluble chitosan, Alose, purified water according to said ratio, is mixed and stirred for 10min extremely Uniformly, solution A is prepared;
Second step weighs ethyl-para-hydroxybenzoate, medicinal glycerin, ethyl alcohol according to said ratio, first will be to hydroxyl with ethyl alcohol The dissolution of yl benzoic acid ethyl ester, then adds glycerol, and 5 min of stirring are prepared into B solution to uniform.
Above-mentioned solution A and B solution are mixed 5 min to uniform by third step, with ammonium hydroxide adjust the pH value of mixed solution to 5.5, it is then sub-packed in spray bottle, the antimicrobial spray is obtained after radiation sterilization.
Embodiment 2
A kind of antimicrobial spray includes following components: 1 part of water soluble chitosan, P-hydroxybenzoic acid second according to parts by weight 0.1 part of ester, 3 parts of medicinal glycerin, 0.5 part of Alose, 5 parts of ethyl alcohol, 99 parts of purified water.
The production technology of the antimicrobial spray the following steps are included:
The first step weighs water soluble chitosan, Alose, purified water according to said ratio, is mixed and stirred for 10min extremely Uniformly, solution A is prepared;
Second step weighs ethyl-para-hydroxybenzoate, medicinal glycerin, ethyl alcohol according to said ratio, first will be to hydroxyl with ethyl alcohol The dissolution of yl benzoic acid ethyl ester, then adds glycerol, and 5 min of stirring are prepared into B solution to uniform.
Above-mentioned solution A and B solution are mixed 5 min to uniform by third step, with ammonium hydroxide adjust the pH value of mixed solution to 5.5, it is then sub-packed in spray bottle, the antimicrobial spray is obtained after radiation sterilization.
Embodiment 3
A kind of antimicrobial spray includes following components: 1 part of water soluble chitosan, P-hydroxybenzoic acid second according to parts by weight 0.1 part of ester, 3 parts of medicinal glycerin, 0.5 part of Alose, 3 parts of ethyl alcohol, 97 parts of purified water.
The production technology of the antimicrobial spray the following steps are included:
The first step weighs water soluble chitosan, Alose, purified water according to said ratio, is mixed and stirred for 10min extremely Uniformly, solution A is prepared;
Second step weighs ethyl-para-hydroxybenzoate, medicinal glycerin, ethyl alcohol according to said ratio, first will be to hydroxyl with ethyl alcohol The dissolution of yl benzoic acid ethyl ester, then adds glycerol, and 5 min of stirring are prepared into B solution to uniform.
Above-mentioned solution A and B solution are mixed 5 min to uniform by third step, with ammonium hydroxide adjust the pH value of mixed solution to 5.5, it is then sub-packed in spray bottle, the antimicrobial spray is obtained after radiation sterilization.
Embodiment 4
Experimental group: a kind of antimicrobial spray includes following components: 0.8 part of water soluble chitosan, to hydroxyl according to parts by weight 0.07 part of ethyl benzoate, 2 parts of medicinal glycerin, 0.3 part of Alose, 3 parts of ethyl alcohol, 97 parts of purified water.
Control group 1: a kind of antimicrobial spray includes following components according to parts by weight: 0.07 part of ethyl-para-hydroxybenzoate, 2 parts of medicinal glycerin, 0.3 part of Alose, 3 parts of ethyl alcohol, 97 parts of purified water.
Control group 2: a kind of antimicrobial spray includes following components: 0.8 part of water soluble chitosan, medicinal according to parts by weight 2 parts of glycerol, 0.3 part of Alose, 3 parts of ethyl alcohol, 97 parts of purified water.
Control group 3: a kind of antimicrobial spray includes following components: 0.8 part of water soluble chitosan, to hydroxyl according to parts by weight 0.07 part of yl benzoic acid ethyl ester, 0.5 part of Alose, 3 parts of ethyl alcohol, 97 parts of purified water.
Control group 4: a kind of antimicrobial spray includes following components: 0.2 part of water soluble chitosan, medicinal according to parts by weight 0.5 part of glycerol, 0.1 part of Alose, 3 parts of ethyl alcohol, 47 parts of purified water.
Control group 5: a kind of antimicrobial spray includes following components: 1 part of water soluble chitosan, medicinal sweet according to parts by weight Oily 3 parts, 0.5 part of Alose, 3 parts of ethyl alcohol, 97 parts of purified water.
Control group 6: a kind of antimicrobial spray includes following components: 1 part of water soluble chitosan, medicinal sweet according to parts by weight Oily 3 parts, 0.5 part of Alose, 3 parts of ethyl alcohol, 47 parts of purified water.
The production technology of the antimicrobial spray the following steps are included:
The first step weighs water soluble chitosan, Alose, purified water according to said ratio, is mixed and stirred for 10min extremely Uniformly, solution A is prepared;
Second step weighs ethyl-para-hydroxybenzoate, medicinal glycerin, ethyl alcohol according to said ratio, first will be to hydroxyl with ethyl alcohol The dissolution of yl benzoic acid ethyl ester, then adds glycerol, and 5 min of stirring are prepared into B solution to uniform.
Above-mentioned solution A and B solution are mixed 5 min to uniform by third step, with ammonium hydroxide adjust the pH value of mixed solution to 5.5, it is then sub-packed in spray bottle, the antimicrobial spray is obtained after radiation sterilization.
To verify whether antimicrobial spray of the present invention reaches expected invention effect, antimicrobial spray of the present invention is surveyed Examination, test result are as follows:
Effect 1: antibacterial effect
Cause some pathogenic bacteria of gynaecology and infected wound mainly to include staphylococcus aureus, is bacillus subtilis, white Color candida albicans, Escherichia coli, Gardnerella, gonococcus etc., this experiment are sprayed with above-mentioned 1 ~ 3 antibacterial of pathogenic bacteria testing example The antibacterial effect of agent, test result are as follows:
As can be seen from the above table, antimicrobial spray prepared by the present invention has good antibacterial effect to most of pathogenic bacteria.
Effect 2: cell toxicity test
As can be seen from the above table, antimicrobial spray prepared by the present invention has good biocompatibility, and safety non-toxic, It can use safely.
Effect 3: film-formation result
Using the volunteer of health as subjects, number is 9 people, by experimental group in implementation column 1 ~ 3 and embodiment 4 and right It is uniformly applied to the identical position of subjects, applying amount 1mL according to the spray of group 1 ~ 3, application area is the cm of 2 cm × 3, is applied Phenomenon and feeling after smearing after 1 min, 10 min, 30 min record are smeared;It will be implemented using casting filming therapy simultaneously Casting film-forming measures thin after natural drying on a glass for column 1 ~ 3 and the spray of experimental group and control group 1 ~ 3 in embodiment 4 The penetrability of film, and log, as a result as follows:
By embodiment 1 ~ 5 as can be seen that antimicrobial spray prepared by the present invention has good film-formation result, and penetrability Preferably;By comparative experiments group and control group 1 it can be found that the film forming of the spray depends on the film forming of chitosan; By comparative experiments group and control group 2 it can be found that after ethyl-para-hydroxybenzoate is added, due to ethyl-para-hydroxybenzoate point Contain a large amount of hydroxyl in son, can in chitosan molecule amino and carboxyl react, the two is with good bio-compatible Property, cause the film generated that there is good mechanical performance, not only film surface has good elasticity, but also has good moisture-inhibiting Property;By comparative experiments group and control group 3 it can be found that the addition of glycerol is conducive to film surface moistening effect after increase film forming, have Conducive to the healing environment wet to wound offer.
Effect 4: stability test
After the product radiation sterilization of control group 2,4,5,6 in embodiment 1 ~ 3 and embodiment 4, it is placed in 20 ± 5 DEG C of conditions Under, the transparency of spray is observed after 0,3,6,12 month respectively, and measure the Weight-average molecular matter of carboxymethyl chitosan in spray Amount, as a result as shown in the table:
As can be seen from the above table, antimicrobial spray prepared by the present invention has good stability, will not store because of long-time And there is floccule precipitating to occur.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair The restriction of embodiments of the present invention;For those of ordinary skill in the art, may be used also on the basis of the above description To make other variations or changes in different ways, there is no necessity and possibility to exhaust all the enbodiments;It is all this Made any modifications, equivalent replacements, and improvements etc., should be included in the claims in the present invention within the spirit and principle of invention Protection scope within.

Claims (7)

1. a kind of antimicrobial spray, which is characterized in that the antimicrobial spray is made of the raw material of following parts by weight: water soluble shells are poly- 0.2~1 part of sugar, 0.05~0.1 part of ethyl-para-hydroxybenzoate, 0.5~3 part of medicinal glycerin, 0.1~0.5 part of Alose, second 1~5 part of alcohol, 95~99 parts of purified water;The water soluble chitosan is carboxymethyl chitosan.
2. antimicrobial spray according to claim 1, which is characterized in that the purity of the medicinal glycerin is greater than 99.8%.
3. antimicrobial spray according to claim 1, which is characterized in that the concentration of the ethyl alcohol is 95%.
4. a kind of preparation method of antimicrobial spray as described in claim 1, which is characterized in that the method includes following steps It is rapid:
S1. it fetches water soluble chitosan, Alose and purified water, is mixed and stirred for 10min to uniform;
S2. ethyl-para-hydroxybenzoate, medicinal glycerin and ethyl alcohol are taken, is first dissolved ethyl-para-hydroxybenzoate with ethyl alcohol, then plus Enter medicinal glycerin, stirring 5min is to uniform;
S3. solution made from solution made from S1 and S2 is mixed, and stirs 5min to uniform, adjust mixed solution with ammonium hydroxide Then pH value is sub-packed in spray bottle to 5~7, the antimicrobial spray is obtained after radiation sterilization.
5. the preparation method of antimicrobial spray according to claim 4, which is characterized in that the water soluble chitosan is carboxylic first Base enclosure glycan.
6. the preparation method of antimicrobial spray according to claim 4, which is characterized in that the purity of the medicinal glycerin is greater than 99.8%.
7. the preparation method of antimicrobial spray according to claim 4, which is characterized in that the concentration of the ethyl alcohol is 95%.
CN201510180437.2A 2015-04-16 2015-04-16 A kind of antimicrobial spray and preparation method thereof Expired - Fee Related CN104740141B (en)

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CN105477010A (en) * 2015-11-30 2016-04-13 济南舜祥医药科技有限公司 Antibacterial nursing spray
CN106421216A (en) * 2016-11-17 2017-02-22 无锡明盛纺织机械有限公司 Anti-bacteria spraying agent and preparation method thereof
CN112426377B (en) * 2020-10-27 2022-08-26 浙江理工大学 Water-soluble antibacterial spray and application thereof
CN112618168A (en) * 2021-01-14 2021-04-09 重庆嘉肯科技有限公司 Nano-silver antibacterial sanitary towel and production method thereof

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CN1233664C (en) * 2003-12-23 2005-12-28 孝感学院 Method for preparing water soluble chitosan
CN101380447A (en) * 2008-10-16 2009-03-11 周小萍 Chitose foaming agent for treating gynecologic disease and preparation method thereof
CN102058876A (en) * 2010-12-18 2011-05-18 甘少磊 Cervix antibacterial repair complex and preparation method thereof
CN102846655A (en) * 2012-10-17 2013-01-02 天津工业大学 Formulation and preparation method of antibacterial spray
CN103961486A (en) * 2014-05-14 2014-08-06 长沙美东医药科技有限公司 Lidocaine compound preparation and aerosol thereof

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