CN105168132A - Cinnamaldehyde nanoemulsion bacteriostatic agent and preparation method thereof - Google Patents
Cinnamaldehyde nanoemulsion bacteriostatic agent and preparation method thereof Download PDFInfo
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Abstract
The invention provides a cinnamaldehyde nanoemulsion bacteriostatic agent and a preparation method thereof. The cinnamaldehyde nanoemulsion bacteriostatic agent takes 0.9-1.2% of cinnamaldehyde as an antibacterial ingredient and is prepared into nanoemulsion from 9-10% of surfactants, 4-5% of cosurfactants, 11-13% of oil and water, thereby being excellent in water solubility and making use of the cinnamaldehyde for preventing and controlling pathogenic microorganisms in a water body possible. Compared with the prior art, the cinnamaldehyde nanoemulsion bacteriostatic agent and the preparation method thereof have the advantages that environmental pollution caused by use of antibiotics and chemical disinfectants can be avoided; the cinnamaldehyde nanoemulsion bacteriostatic agent has good bacteriostatic and bactericidal effects, and pathogenic bacteria are less prone to production of drug tolerance; the preparation method is simple, net content of the cinnamaldehyde is high, quality of the cinnamaldehyde is stable, and accordingly, the cinnamaldehyde nanoemulsion bacteriostatic agent is suitable for large-scale production; the cinnamaldehyde nanoemulsion bacteriostatic agent, which is soluble in water and stable in property after dissolving in water, can be widely applied to disinfection of an aquaculture pond water body and prevention and control of common aquaculture fish pathogenic bacteria.
Description
Technical field
The present invention relates to technical field of aquaculture, be specifically related to cinnamic aldehyde nano-emulsion antibacterial and preparation method thereof.
Background technology
In aquaculture technology, diseases prevention and treatment are the important means ensureing output, in the common disease of aquatic animal, the disease harm caused because of pathogenic microorganism is the most serious, this type of disease has infectiousness, easily eruption and prevalence on the one hand, in addition, this type of disease even causes comparatively greatly aquatic animal dead to yield effect.Be main for the protective agents of various aquatic animal pathogenic bacterium mainly with antibiotic and chemosterilant in prior art, although use this class methods Be very effective, but a large amount of inputs and unreasonable use thereof can produce toxic and side effects to aquaculture object, pathogenic bacterium drug resistance is strengthened, have certain residual in water body, life-time service can cause certain pollution for cultivation object, breeding water body and ecological environment around, increases publilc health risk.
Cinnamic aldehyde is the main component of Chinese medicine Cortex Cinnamomi volatile oil, have another name called cinnamaldehyde, cinnamic aldehyde, phenyl cinnamic aldehyde, 3-phenyl-2-acrylic aldehyde, there is good bacteriostasis and sterilization effect, pathogen pollution-free to breeding environment and not easily the various biological functions such as drug resistance are produced to it, but because cinnamic aldehyde is the oxidizable volatile oily liquids being insoluble in water, affect it to preserve and Clinical practice, make it be restricted in practical application.
It is 1 ~ 100nm that aqueous phase, oil phase, surfactant and cosurfactant are normally formed particle diameter by proper proportion by the preparation of nanoemulsion medicine, has the preparation technology of the stable transparent or semitransparent system of low viscosity, isotropic thermodynamics and kinetics.This technique contribute to improving hydrophobic drug dissolubility, strengthen drug effect and bioavailability, go back realizing controlled-release medicine simultaneously, avoid drug degradation and leakage.
Summary of the invention
The present invention is intended to the technological deficiency for prior art, provides a kind of cinnamic aldehyde nano-emulsion antibacterial, to solve the technical problem generally environment for the pathogenic bacterium protective agents of water body environment in prior art to negative effect.
Another technical problem that the present invention solves is the pathogenic bacterium protective agents for water body environment in prior art, the technical problem of lower, the easy generation drug resistance of antimicrobial efficiency.
The present invention solve a technical problem be again cinnamic aldehyde as water body pathogenic bacterium protective agents, the technical problem that dispersibility is not good.
The present invention solve another technical problem be cinnamic aldehyde as pathogenic bacterium protective agents, the technical problem of its oxidizable inefficacy.
The present invention again by providing a kind of cinnamic aldehyde nano-emulsion antibacterial preparation method, to solve the lower technical problem of described cinnamic aldehyde nano-emulsion antibacterial preparation efficiency.
For realizing above technical purpose, the present invention by the following technical solutions:
A kind of cinnamic aldehyde nano-emulsion antibacterial, comprises the composition of following percetage by weight: surfactant 9 ~ 10%, cosurfactant 4 ~ 5%, oil phase 11 ~ 13%, cinnamic aldehyde 0.9 ~ 1.2%, water surplus.
Preferably, described surfactant is Tween 80.
Preferably, described cosurfactant is ethanol.
Preferably, described oil phase is ethyl acetate.
Preferably, the particle diameter of cinnamic aldehyde nano-emulsion antibacterial is 5 ~ 20nm, and mean diameter is 10.7nm.
Preferably, wherein the content of cinnamic aldehyde is 20.11mg/mL.
Present invention also offers a kind of preparation method of above-mentioned cinnamic aldehyde nano-emulsion antibacterial, comprise the following steps:
1) surfactant and the cosurfactant of getting formula ratio mix, and obtain the first mixture;
2) get step 1) described in the first mixture and the oil phase of formula ratio mix, obtain the second mixture;
3) under agitation to step 2) described second mixture drips the water of formula ratio, obtains blank nano-emulsion;
4) under agitation to step 3) add the cinnamic aldehyde of formula ratio in described blank nano-emulsion, namely mixing obtains cinnamic aldehyde nano-emulsion antibacterial.
Preferred on the method basis, step 1) in surfactant and cosurfactant mass ratio be 2:1.
Preferred on the method basis, step 2) in the mass ratio of the first mixture and oil phase be (5 ~ 6): (3 ~ 4).
Preferred on the method basis, step 1) or step 2) described in mixing, utilize magnetic stirring apparatus to realize.
In above technical scheme, described surfactant, refer to the material of the interface state generation significant change that can make its solution system after a class adds, surfactant includes but not limited to dodecylbenzene sodium sulfonate, quaternary ammonium compound, lecithin in the present invention, aminoacid, betanin, fatty glyceride, class of department, tween etc.Described cosurfactant refers to the surface activity and hydrophile-lipophile balance that can change surfactant, thus affect the composition of the phase of system, include but not limited to ethanol, normal propyl alcohol, isopropyl alcohol, n-butyl alcohol, isobutanol, n-amyl alcohol, isoamyl alcohol, 1-hexanol, 2-hexanol, 1-capryl alcohol, sec-n-octyl alcohol, Alcohols,fusel, n nonylphenol etc.Oil phase refers to all kinds of oil-phase components that can be used for forming emulsion.
Being prepared by antimicrobial component cinnamic aldehyde of novelty of the present invention becomes nanoemulsions, water solublity is significantly promoted, can be used as the pathogenic microorganism protective agents of water body environment.Specifically, the present invention is directed to the environment for use of this microemulsion and preferred suitable surfactant, the cosurfactant composition of cinnamic aldehyde self-characteristic, the product of preparation is outstanding in water solublity, active constituent content etc., can give full play to biocidal efficacies.In optimal technical scheme, surfactant being preferably Tween 80, cosurfactant being preferably ethanol, oil phase is preferably ethyl acetate, is find that the product utilizing above-mentioned special component to prepare is better in dispersibility, self physical property etc.; Particle diameter is preferably 10 ~ 100 nanometers and more contributes to product dissolving; Cinnamic aldehyde content is preferably 20.11mg/mL and fully can ensures biocidal efficacies.
Compared with prior art, the technology of the present invention advantage major embodiment is in the following areas:
(1) use cinnamic aldehyde nano-emulsion antibacterial of the present invention, can avoid because using the chemical control such as antibiotic and chemosterilant aquatic animal pathogenic bacterium produced pollution water body environment, making aquaculture object produce toxic and side effects, make the bad phenomenon such as pathogenic bacterium drug resistance enhancing;
(2) cinnamic aldehyde used in the present invention is the main component of Chinese medicine Cortex Cinnamomi volatile oil, and toxic and side effects is low, does not pollute environment, there is good bacteriostasis and sterilization effect and pathogen not easily to its produce drug resistance;
(3) nano-emulsion preparation technology of the present invention is simple to operate, the high and stable in properties of cinnamic aldehyde net content, reduces production cost, is applicable to factorial praluction;
(4) the cinnamic aldehyde nano-emulsion antibacterial prepared by the present invention, water soluble, and the water-soluble rear property of medicine is stablized, and can be applicable to the dipping sterilization of aquatic animal and the prevention and control of aquatic animal common pathogen.。
Accompanying drawing explanation
Fig. 1 is cinnamic aldehyde nano-emulsion antibacterial grain size distribution prepared by the embodiment of the present invention 1.
Fig. 2 is the schematic arrangement of cinnamic aldehyde.
Detailed description of the invention
Below will be described in detail the specific embodiment of the present invention.In order to avoid too much unnecessary details, in the examples below to belonging to known structure or function will not be described in detail.
The approximating language used in following examples can be used for quantitative expression, shows to allow quantity to have certain variation when not changing basic function.Therefore, this exact value itself is not limited to the numerical value that the language such as " approximately ", " left and right " is revised.In certain embodiments, " approximately " represents and allows its numerical value revised to change in the positive and negative scope of 10 (10%), such as, and any numerical value that what " about 100 " represented can be between 90 to 110.In addition, in the statement of " about first numerical value is to second value ", revise the first and second numerical value two numerical value approximately simultaneously.In some cases, approximating language may be relevant with the precision of gauge.
Apart from outside definition, technology used in following examples and scientific terminology have the identical meanings generally understood with those skilled in the art of the invention.
Embodiment 1
1, the formula of cinnamic aldehyde nano-emulsion antibacterial and preparation thereof
A kind of cinnamic aldehyde nano-emulsion antibacterial, its raw materials quality percentage ratio forms: surfactant (Tween 80), cosurfactant (ethanol), oil phase (ethyl acetate), water (distilled water), cinnamic aldehyde are respectively 10%, 4%, 11.8%, 73%, 1.2%.
Its preparation flow is as follows:
Under room temperature, first accurately measure 3000mg Tween 80 and 1500mg ethanol, fully mix under the effect of 600r/min magnetic agitation, obtain mixture A; Then accurately measure 3600mg ethyl acetate fully to mix under the effect of 600r/min magnetic agitation with mixture A, obtain mixture B; Then in mixture B, dropwise distilled water is added while stirring, until after system becomes muddiness gradually by the clarification oil phase that viscosity is less, adding again along with distilled water, mixed liquor become suddenly uncommon and bright till, now obtain mixture C (blank nano-emulsion); Under the effect of 600r/min magnetic agitation, in mixture C, slowly add cinnamic aldehyde 200mg, the cinnamic aldehyde nano-emulsion antibacterial that namely forming property is stable, wherein cinnamic aldehyde content is 20.11mg/ml.
2, cinnamic aldehyde nano-emulsion antibacterial property checking test
(1) outward appearance
By perusal, whether prepared cinnamic aldehyde nano-emulsion antibacterial color is bright, and whether viscosity is less, and whether system is even.Observe and find, nano-emulsion outward appearance is the homogeneous system of faint yellow clear, meets appearance test requirement.
(2) stability test
By prepared cinnamic aldehyde nano-emulsion antibacterial high speed centrifugation 40min under 4000r/min, observe without lamination, illustrate that it has good stability.
(3) particle size distribution inspection
Utilize laser granulometry to detect to cinnamic aldehyde nano-emulsion antibacterial, as shown in Figure 1, nano-emulsion particle size distribution is between 5 ~ 20nm, and mean diameter is 10.74nm for testing result.
3, cinnamic aldehyde nano-emulsion antibacterial drug sensitive experiment
With 4 kinds of common aquatic animal pathogenic bacterium---Edwardsiella tarda, Aeromonas sobria, eel pseudomonas septica, Aeromonas hydrophila, for subjects, adopt Odontothrips loti to compare the fungistatic effect of cinnamic aldehyde nano-emulsion and cinnamic aldehyde.Oxford cup is put into respectively on the solid medium being coated with above-mentioned pathogenic bacterium, in the cup of Oxford, add the cinnamic aldehyde nano-emulsion antibacterial containing cinnamic aldehyde 20.11mg/mL respectively, each 200 μ L of the cinnamic aldehyde diluent (diluting with dehydrated alcohol) with concentration.With dehydrated alcohol and blank nano-emulsion for matched group, in two other Oxford cup, add the dehydrated alcohol of 200 μ L and blank nano-emulsion respectively.Culture dish just to be put in incubator 28 DEG C cultivate 24h after, observe antibacterial situation and measure antibacterial circle diameter.The results are shown in Table 1.
Table 1 cinnamic aldehyde nano-emulsion antibacterial In vitro chemo-drug sensitive test result
As can be seen from Table 1, matched group occurs without inhibition zone, illustrates that dehydrated alcohol and blank nano-emulsion do not affect the fungistatic effect of cinnamic aldehyde.Cinnamic aldehyde nano-emulsion antibacterial and cinnamic aldehyde diluent have fungistatic effect to 4 kinds of pathogenic bacterium.Be independent sample T with SPSS18.0 software to processed group to check, significant difference (representing with *) during P<0.05, P<0.01 time difference heteropole significantly (representing with * *).Can find out that the fungistatic effect pole of cinnamic aldehyde nano-emulsion antibacterial is significantly higher than the cinnamic aldehyde (P<0.01) of non-nanorize.
4, cinnamic aldehyde nano-emulsion and cinnamic aldehyde are tested the minimal inhibitory concentration of above-mentioned 4 kinds of pathogenic bacterium
Prepared cinnamic aldehyde nano-emulsion doubling dilution is diluted to variable concentrations, and cinnamic aldehyde solution dehydrated alcohol is diluted to same concentrations, draw cinnamic aldehyde nano-emulsion and each 200 μ L of cinnamic aldehyde diluent, be added in the Oxford cup of different culture dish respectively, in incubator after 28 DEG C of cultivation 24h, measure antibacterial circle diameter.When inhibition zone narrows down to Oxford cup equal diameters, concentration is now minimal inhibitory concentration.
Table 2 cinnamic aldehyde nano-emulsion antibacterial is to the minimal inhibitory concentration of 4 kinds of pathogenic bacterium
As can be seen from Table 2, the antibacterial strength ratio cinnamic aldehyde of cinnamic aldehyde nano-emulsion to Edwardsiella tarda, Aeromonas sobria, eel pseudomonas septica, Aeromonas hydrophila improves 37.5%, 37.5%, 36.4%, 50.0% respectively.
Embodiment 2
A kind of cinnamic aldehyde nano-emulsion antibacterial, is characterized in that the composition comprising following percetage by weight: Tween 80 9%, ethanol 4%, ethyl acetate 11%, cinnamic aldehyde 0.9%, water surplus.
The particle diameter of this cinnamic aldehyde nano-emulsion antibacterial is 10nm.
The preparation method of cinnamic aldehyde nano-emulsion antibacterial described in this, comprises the following steps:
1) surfactant and the cosurfactant of getting formula ratio mix, and obtain the first mixture;
2) get step 1) described in the first mixture and the oil phase of formula ratio mix, obtain the second mixture;
3) under agitation to step 2) described second mixture drips the water of formula ratio, obtains blank nano-emulsion;
4) under agitation to step 3) add the cinnamic aldehyde of formula ratio in described blank nano-emulsion, namely mixing obtains cinnamic aldehyde nano-emulsion antibacterial.
Step 1) or step 2) described in mixing, utilize magnetic stirring apparatus to realize.
Embodiment 3
A kind of cinnamic aldehyde nano-emulsion antibacterial, comprises the composition of following percetage by weight: Tween 80 10%, ethanol 5%, ethyl acetate 13%, cinnamic aldehyde 1.2%, water surplus.
The particle diameter of this cinnamic aldehyde nano-emulsion antibacterial is 100nm.
The preparation method of cinnamic aldehyde nano-emulsion antibacterial described in this, comprises the following steps:
1) surfactant and the cosurfactant of getting formula ratio mix, and obtain the first mixture;
2) get step 1) described in the first mixture and the oil phase of formula ratio mix, obtain the second mixture;
3) under agitation to step 2) described second mixture drips the water of formula ratio, obtains blank nano-emulsion;
4) under agitation to step 3) add the cinnamic aldehyde of formula ratio in described blank nano-emulsion, namely mixing obtains cinnamic aldehyde nano-emulsion antibacterial
Embodiment 4
A kind of cinnamic aldehyde nano-emulsion antibacterial, comprises the composition of following percetage by weight: class 809.5% of department, n-butyl alcohol 4.5%, silicone oil 12%, water surplus; Wherein also comprise the cinnamic aldehyde of 20.11mg/mL.
The particle diameter of this cinnamic aldehyde nano-emulsion antibacterial is 50nm.
The preparation method of this cinnamic aldehyde nano-emulsion antibacterial, comprises the following steps:
1) surfactant and the cosurfactant of getting formula ratio mix, and obtain the first mixture;
2) get step 1) described in the first mixture and the oil phase of formula ratio mix, obtain the second mixture;
3) under agitation to step 2) described second mixture drips the water of formula ratio, obtains blank nano-emulsion;
4) under agitation to step 3) add the cinnamic aldehyde of formula ratio in described blank nano-emulsion, namely mixing obtains cinnamic aldehyde nano-emulsion antibacterial.
Embodiment 5
A kind of cinnamic aldehyde nano-emulsion antibacterial, comprises the composition of following percetage by weight: stearic acid 9.8%, isoamyl alcohol 4.2%, ethyl-ethyl palmitate 11.5%, water surplus; Wherein also comprise the cinnamic aldehyde of 20.11mg/mL.
The particle diameter of this cinnamic aldehyde nano-emulsion antibacterial is 80nm.
The preparation method of this cinnamic aldehyde nano-emulsion antibacterial, comprises the following steps:
1) surfactant and the cosurfactant of getting formula ratio mix, and obtain the first mixture;
2) get step 1) described in the first mixture and the oil phase of formula ratio mix, obtain the second mixture;
3) under agitation to step 2) described second mixture drips the water of formula ratio, obtains blank nano-emulsion;
4) under agitation to step 3) add the cinnamic aldehyde of formula ratio in described blank nano-emulsion, namely mixing obtains cinnamic aldehyde nano-emulsion antibacterial.
Step 1) or step 2) described in mixing, utilize magnetic stirring apparatus to realize.
Embodiment 6
A preparation method for cinnamic aldehyde nano-emulsion antibacterial described in claim 1, comprises the following steps:
1) surfactant and the cosurfactant of getting formula ratio mix, and obtain the first mixture;
2) get step 1) described in the first mixture and the oil phase of formula ratio mix, obtain the second mixture;
3) under agitation to step 2) described second mixture drips the water of formula ratio, obtains blank nano-emulsion;
4) under agitation to step 3) add the cinnamic aldehyde of formula ratio in described blank nano-emulsion, namely mixing obtains cinnamic aldehyde nano-emulsion antibacterial.
Step 1) in surfactant and cosurfactant mass ratio be 2:1.
Step 2) in the mass ratio of the first mixture and oil phase be 5.5:3.5.
Above embodiments of the invention have been described in detail, but described content is only preferred embodiment of the present invention, not in order to limit the present invention.All make in application range of the present invention any amendment, equivalent to replace and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a cinnamic aldehyde nano-emulsion antibacterial, is characterized in that the composition comprising following percetage by weight: surfactant 9 ~ 10%, cosurfactant 4 ~ 5%, oil phase 11 ~ 13%, cinnamic aldehyde 0.9 ~ 1.2%, water surplus.
2. cinnamic aldehyde nano-emulsion antibacterial according to claim 1, is characterized in that described surfactant is Tween 80.
3. cinnamic aldehyde nano-emulsion antibacterial according to claim 1, is characterized in that described cosurfactant is ethanol.
4. cinnamic aldehyde nano-emulsion antibacterial according to claim 1, is characterized in that described oil phase is ethyl acetate.
5. cinnamic aldehyde nano-emulsion antibacterial according to claim 1, is characterized in that the particle diameter of cinnamic aldehyde nano-emulsion antibacterial is 5 ~ 20nm.
6. cinnamic aldehyde nano-emulsion antibacterial according to claim 1, is characterized in that the content of wherein cinnamic aldehyde is 20.11mg/mL.
7. a preparation method for cinnamic aldehyde nano-emulsion antibacterial described in claim 1, is characterized in that comprising the following steps:
1) surfactant and the cosurfactant of getting formula ratio mix, and obtain the first mixture;
2) get step 1) described in the first mixture and the oil phase of formula ratio mix, obtain the second mixture;
3) under agitation to step 2) described second mixture drips the water of formula ratio, obtains blank nano-emulsion;
4) under agitation to step 3) add the cinnamic aldehyde of formula ratio in described blank nano-emulsion, namely mixing obtains cinnamic aldehyde nano-emulsion antibacterial.
8. method according to claim 7, is characterized in that step 1) in surfactant and cosurfactant mass ratio be 2:1.
9. method according to claim 7, is characterized in that step 2) in the mass ratio of the first mixture and oil phase be (5 ~ 6): (3 ~ 4).
10. method according to claim 7, is characterized in that step 1) or step 2) described in mixing, utilize magnetic stirring apparatus to realize.
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Cited By (7)
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| CN108938565A (en) * | 2018-08-17 | 2018-12-07 | 南京福科帝生物科技有限公司 | A kind of trans-cinnamic aldehyde nano-emulsion and preparation method thereof |
| CN110670349A (en) * | 2019-09-18 | 2020-01-10 | 广州贝诺生物科技有限公司 | 5-methyl-2-isopropyl phenol micro-nano composition with mite-removing and bacteriostatic activity |
| CN112806514A (en) * | 2021-01-29 | 2021-05-18 | 浙江工业大学 | Cinnamaldehyde pickering emulsion for inhibiting aspergillus ochraceus growth and producing toxin and preparation method thereof |
| CN114403293A (en) * | 2022-01-25 | 2022-04-29 | 中国科学院兰州化学物理研究所 | Preparation method of plant particle synergistically stabilized cinnamaldehyde emulsion |
| CN115260149A (en) * | 2021-04-30 | 2022-11-01 | 中国石油天然气股份有限公司 | Bactericide and preparation method thereof |
| CN116076491A (en) * | 2022-12-12 | 2023-05-09 | 云南中医药大学 | Preparation method of enhanced lemon grass volatile oil antibacterial active agent |
| CN118272483A (en) * | 2024-05-23 | 2024-07-02 | 江西农业大学 | Detection method for sub-antibacterial concentration of cinnamaldehyde nanoemulsion bacteriostat |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108938565A (en) * | 2018-08-17 | 2018-12-07 | 南京福科帝生物科技有限公司 | A kind of trans-cinnamic aldehyde nano-emulsion and preparation method thereof |
| CN110670349A (en) * | 2019-09-18 | 2020-01-10 | 广州贝诺生物科技有限公司 | 5-methyl-2-isopropyl phenol micro-nano composition with mite-removing and bacteriostatic activity |
| CN112806514A (en) * | 2021-01-29 | 2021-05-18 | 浙江工业大学 | Cinnamaldehyde pickering emulsion for inhibiting aspergillus ochraceus growth and producing toxin and preparation method thereof |
| CN115260149A (en) * | 2021-04-30 | 2022-11-01 | 中国石油天然气股份有限公司 | Bactericide and preparation method thereof |
| CN115260149B (en) * | 2021-04-30 | 2023-09-26 | 中国石油天然气股份有限公司 | Bactericide and preparation method thereof |
| CN114403293A (en) * | 2022-01-25 | 2022-04-29 | 中国科学院兰州化学物理研究所 | Preparation method of plant particle synergistically stabilized cinnamaldehyde emulsion |
| CN116076491A (en) * | 2022-12-12 | 2023-05-09 | 云南中医药大学 | Preparation method of enhanced lemon grass volatile oil antibacterial active agent |
| CN118272483A (en) * | 2024-05-23 | 2024-07-02 | 江西农业大学 | Detection method for sub-antibacterial concentration of cinnamaldehyde nanoemulsion bacteriostat |
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Application publication date: 20151223 |