CN102579399A - Preparation method of antibacterial Chinese mugwort oil microcapsules - Google Patents
Preparation method of antibacterial Chinese mugwort oil microcapsules Download PDFInfo
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- CN102579399A CN102579399A CN2012100739368A CN201210073936A CN102579399A CN 102579399 A CN102579399 A CN 102579399A CN 2012100739368 A CN2012100739368 A CN 2012100739368A CN 201210073936 A CN201210073936 A CN 201210073936A CN 102579399 A CN102579399 A CN 102579399A
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Abstract
The invention relates to a preparation method of antibacterial Chinese mugwort oil microcapsules, which comprises the steps of using gelatine as a wall material to emulsify Chinese mugwort, adding water to dilute, adjusting potential of hydrogen (pH) to be below an isoelectric point of the gelatine to be adsorbed with Arabic gum of negative charges, forming microcapsule rudiment, then performing low temperature jelly, adding a cross-linking agent in a coagulation microcapsule, performing chemical cross-linking treatment of the microcapsule, and achieving the microcapsule. The prepared antibacterial Chinese mugwort oil microcapsules have the basically same antibacterial performance as Chinese mugwort oil. On the same condition, the Chinese mugwort oil hardly has antibacterial performance after placed for 30 days. The prepared Chinese mugwort oil microcapsules still have strong antibacterial performance after placed for 40 days, thereby achieving the purpose of sustained release and enabling application prospect to be wide.
Description
Technical field
The present invention relates to a kind of microcapsule preparation method, be specifically related to the method for preparing of a kind of mugwort oil/gelatin and arabic gum complex coacervation antibiotic property microcapsule.
Technical background
Radix Artemisia ordosicae; Be the perennial wild herb of Compositae artemisia, the Radix Artemisia ordosicae quintessence oil physiologically active ingredient kind of therefrom extracting is more, and wherein many monoterpenes and sesquiterpenoids chemical substance all have antibacterial activity; It meets people's green consumption idea as a kind of antibacterial mildew inhibitor of natural, environmental protection.But, limited application because the unstability of Radix Artemisia ordosicae quintessence oil makes its duration of efficacy short.Microcapsule technology makes it see through cyst wall and slowly discharges through essential oil is coated, and improves pressure-sensitive, heliosensitivity and the thermal sensitivity of Radix Artemisia ordosicae quintessence oil, improves product specification and added value.
Microcapsule technology is to utilize one type of material as filmogen another kind of material to be coated, and forms a kind of technology of microencapsulation.The microcapsule size usually in nanometer to micron order, along with the nanometer Development of Preparation Technology, the microcapsule of preparation nanoscale particle diameter obtains broad research.Microcapsule is generally the nucleocapsid structure of monolayer, and the core that cyst membrane coated also can be the multinuclear shape, and be wrapped in the inner material of microcapsule and be called the capsule heart, active substance, core etc., the outside coating film of microcapsule is called wall material, cyst wall, housing etc.Material is carried out micro encapsulation can improve Stability of Substance, the rate of release of control core improves the physical property that is coated material, is convenient to handle etc.
Gelatin is a kind of effective protecting colloid, can stop crystal or ionic gathering, and have excellent biological compatibility, biodegradable and moulding property, is important wall material raw material in the preparation microcapsule.Prepare the method that the gelatin microcapsule selects for use usually single coacervation, complex coacervation, freeze-drying, spray drying method etc. are arranged.Carboxyl on the gelatin side chain, amino and hydroxyl make it have higher chemism, can carry out modification to gelatin through the whole bag of tricks, obtain many gelatin excellent properties that both kept, the new material that has new features again.The cold state etc. of prolonging utilizes acrylamide that gelatin is carried out graft modification, and with the microcapsule of single coacervation preparation, research shows the increase with the grafted gelatin molecular weight; The microcapsule particle size distribution broadens; Along with reducing of grafted gelatin molecular weight, the particle size distribution of microcapsule is more concentrated, more trends towards normal distribution.Through the blend of other natural macromolecular material and gelatin, its biocompatibility, controlled degradation property have obviously been improved, like chitosan etc.
Summary of the invention
Technical problem to be solved by this invention is; A kind of method for preparing of antibiotic property mugwort oil microcapsule is provided; Utilize mugwort oil/gelatin and arabic gum complex coacervation, and prepare mugwort oil microcapsule with good anti-microbial property and better slow release effect through Selection of technological conditions.
For achieving the above object, the technical scheme that the present invention adopts is:
A kind of method for preparing of antibiotic property mugwort oil microcapsule is characterized in that preparation process is following:
The first step: prepare mass concentration respectively and be 3%～5% aqueous gelatin solution and mass concentration and be each 150～250ml of arabic gum aqueous solution of 3%～5%, and two kinds of solution are mixed;
Second step: 4～8g mugwort oil is added in the mixed solution that the first step obtains, low whipping speed 300～500r/min, temperature is under 40～55 ℃, stirs 20～40min, and the mugwort oil mixed and dispersed in above-mentioned mixed solution, is obtained emulsion;
The 3rd step: in second emulsion that obtain of step, add deionized water 70～150ml, low whipping speed is under 300～500r/min condition, stirs 30～50min, obtains diluent;
The 4th step: the pH value of the 3rd diluent that obtain of step is transferred to 3.8～5.0 obtain pre-polymerization liquid;
The 5th step: low whipping speed is under 300～500r/min condition, makes the temperature natural of the 4th pre-polymerization liquid that obtains of step be reduced to 0～5 ℃, and is incubated 40～60min, obtains coagulation liquid;
The 6th step: go on foot the glutaraldehyde 2～5g that adds in the coagulation liquid that obtains as crosslinking and curing agent the 5th, mix homogeneously obtains consolidation liquid;
The 7th step: the consolidation liquid that the 6th step was obtained is warming up to 45 ℃, and low whipping speed is that 400～500r/min reacted 1.5～3 hours down then; Reaction is reduced to 20～25 ℃ with system temperature after finishing, and uses washed with isopropyl alcohol, sucking filtration, and drying at room temperature promptly obtains microcapsule.
Said gelatin preferred molecular weight is 5～250,000 gelatin.
The mass concentration of said aqueous gelatin solution and arabic gum aqueous solution all is preferably 4%.
The pH value of diluent preferably transfers to 3.8 in the 4th step.
The addition of glutaraldehyde is preferably 2g in the 6th step.
Good effect of the present invention is:
The first, the prepared mugwort oil microcapsule of the present invention has and the essentially identical anti-microbial property of mugwort oil; But mugwort oil does not almost have antibiotic property under the same terms after placing 30 days; And the prepared mugwort oil microcapsule of the present invention still has stronger antibiotic property after placing 40 days; Reached the purpose that microcapsule slowly discharges, made microcapsule that application prospect widely arranged.
The second, the present invention has implemented the chemical crosslinking processing to capsular cyst wall, and the compactness that has improved cyst wall reaches the tolerance to solution acid-basicity, has heightened the stability that the mugwort oil microcapsule is used.Prepared mugwort oil microcapsule particle size distribution is even, and smooth surface, rule have excellent mechanical intensity, are difficult for breaking.
Three, method of the present invention is simple, and the preparation process does not have to pollute to environment basically.
Description of drawings
Fig. 1 is the surface sweeping Electronic Speculum picture of the embodiment of the invention two prepared mugwort oil microcapsules.
The specific embodiment
Further specify the present invention below in conjunction with embodiment.
Embodiment one
The first step: prepare mass concentration respectively and be 3% aqueous gelatin solution and mass concentration and be each 200ml of arabic gum aqueous solution of 3%, and two kinds of solution are mixed.
Second step: the 4g mugwort oil is added in the mixed solution that the first step obtains, low whipping speed 300r/min, temperature is under 40 ℃, stirs 25min, and the mugwort oil mixed and dispersed in above-mentioned mixed solution, is obtained emulsion.
The 3rd step: in second emulsion that obtain of step, add deionized water 100ml, low whipping speed is under the 300r/min condition, stirs 20min, obtains diluent.
The 4th step: the pH value of the 3rd diluent that obtain of step is transferred to 3.8 obtain pre-polymerization liquid.
The 5th step: low whipping speed is under the 300r/min condition, makes the temperature natural of the 4th pre-polymerization liquid that obtains of step be reduced to 2 ℃, and insulation 40min, obtains coagulation liquid.
The 6th step: go on foot the glutaraldehyde 4g that adds in the coagulation liquid that obtains as crosslinking and curing agent the 5th, mix homogeneously obtains consolidation liquid.
The 7th step: the consolidation liquid that the 6th step was obtained is warming up to 45 ℃, and low whipping speed is that 400r/min reacted 2 hours down then.Reaction is reduced to 20 ℃ with system temperature after finishing, with washed with isopropyl alcohol surface of microcapsule mugwort oil, and sucking filtration, drying at room temperature promptly obtains microcapsule.
Embodiment two
The first step: prepare mass concentration respectively and be 4% aqueous gelatin solution and mass concentration and be each 150ml of arabic gum aqueous solution of 3%, and two kinds of solution are mixed.
Second step: the 4g mugwort oil is added in the mixed solution that the first step obtains, low whipping speed 400r/min, temperature is under 45 ℃, stirs 20min, and the mugwort oil mixed and dispersed in above-mentioned mixed solution, is obtained emulsion.
The 3rd step: in second emulsion that obtain of step, add deionized water 70ml, low whipping speed is under the 400r/min condition, stirs 40min, obtains diluent.
The 4th step: the pH value of the 3rd diluent that obtain of step is transferred to 3.8 obtain pre-polymerization liquid.
The 5th step: low whipping speed is under the 300r/min condition, makes the temperature natural of the 4th pre-polymerization liquid that obtains of step be reduced to 0 ℃, and insulation 50min, obtains coagulation liquid.
The 6th step: go on foot the glutaraldehyde 2g that adds in the coagulation liquid that obtains as crosslinking and curing agent the 5th, mix homogeneously obtains consolidation liquid.
The 7th step: the consolidation liquid that the 6th step was obtained is warming up to 45 ℃, and low whipping speed is that 400r/min reacted 1.5 hours down then.Reaction is reduced to 20 ℃ with system temperature after finishing, with washed with isopropyl alcohol surface of microcapsule mugwort oil, and sucking filtration, drying at room temperature promptly obtains microcapsule.
Embodiment three
The first step: prepare mass concentration respectively and be 5% aqueous gelatin solution and mass concentration and be each 250ml of arabic gum aqueous solution of 5%, and two kinds of solution are mixed.
Second step: the 8g mugwort oil is added in the mixed solution that the first step obtains, low whipping speed 500r/min, temperature is under 55 ℃, stirs 40min, and the mugwort oil mixed and dispersed in above-mentioned mixed solution, is obtained emulsion.
The 3rd step: in second emulsion that obtain of step, add deionized water 150ml, low whipping speed is under the 500r/min condition, stirs 30min, obtains diluent.
The 4th step: the pH value of the 3rd diluent that obtain of step is transferred to 5.0 obtain pre-polymerization liquid.
The 5th step: low whipping speed is under the 500r/min condition, makes the temperature natural of the 4th pre-polymerization liquid that obtains of step be reduced to 5 ℃, and insulation 60min, obtains coagulation liquid.
The 6th step: go on foot the glutaraldehyde 5g that adds in the coagulation liquid that obtains as crosslinking and curing agent the 5th, mix homogeneously obtains consolidation liquid.
The 7th step: the consolidation liquid that the 6th step was obtained is warming up to 45 ℃, and low whipping speed is that 500r/min reacted 3 hours down then.Reaction is reduced to 25 ℃ with system temperature after finishing, with washed with isopropyl alcohol surface of microcapsule mugwort oil, and sucking filtration, drying at room temperature promptly obtains microcapsule.
It below is the experimental data of the prepared mugwort oil microcapsule of embodiment two.
With mugwort oil microcapsule product exsiccant under the room temperature with to be placed on 45 ℃ and humidity with the mugwort oil of its core equivalent be to carry out the antibiotic property experiment after cultivating a period of time in 70% the constant temperature and humidity incubator.
Table 1 mugwort oil microcapsule is to supplying the antibiotic rate (%) of examination strain
Tab.1?Inhibition?rate?of?artemisia?argyllem?oil?microcapsules（%）
| Sample | Escherichia coli | Staphylococcus aureus | Aspergillus flavus |
| Mugwort oil | 99 | 99 | 98 |
| Blank microcapsule | 1 | 0 | 0 |
| The mugwort oil microcapsule | 99 | 98 | 97 |
The mensuration of table 2 mugwort oil microcapsule antibacterial lasting effect
Tab.2?Residual?effect?of?artemisia?argyllem?oil?microcapsules
In the table, R
1Represent mugwort oil; R
2Represent the mugwort oil microcapsule of the embodiment of the invention two preparations.
The mugwort oil microcapsule of above-mentioned instance two preparations is carried out the antibiotic property test, and the result sees table 1.Find out that from table 1 the mugwort oil microcapsule of the present invention's preparation is best to colibacillary fungistatic effect, reaches 99%, and staphylococcus aureus and Aspergillus flavus are also had good antibacterial effect, compares with the antibiotic property of mugwort oil, is more or less the same.Blank microcapsule does not find to have antibiotic property, explain that what in microcapsule, play the antibiotic property effect is mugwort oil, and coating does not influence the antibiotic property of mugwort oil basically.
Antibiotic lasting effect result sees table 2.Find out that from table 2 mugwort oil does not almost have antibiotic property under the same terms after placing 30 days, and the mugwort oil microcapsule still there is stronger antibiotic property after placing 40 days, has reached the purpose that microcapsule slowly discharges, make microcapsule that application prospect widely arranged.
Wherein the antibiotic property experimental technique is following.
The strain of escherichia coli and staphylococcus aureus is after cultivating 24 h; Utilize the plane to cultivate counting method the concentration of each bacterium bacterium liquid is transferred to 5 * 105 CFUml-1; Pipette 0.5 mL culture fluid with pipet and put into the conical flask that blank culture fluid, blank microcapsule and mugwort oil microcapsule culture fluid are housed successively; Good and the wrapping of plug, the above-mentioned sample of shaken cultivation in the shaken cultivation case takes out behind 24 h.The antibacterial liquid of drawing 0.5 mL with liquid-transfering gun is placed in the sterilized water; Shake up vibration, be diluted to certain concentration, pipette the 1mL diluent with liquid-transfering gun and be put in culture dish with sterilized water; The agar Nutrient medium poured in the culture dish shake up; After waiting to solidify, upside down is cultivated 24h in 37 ℃ incubator, observes.Aspergillus flavus is adopted identical method, just culture dish is placed on 28 ℃ and observes behind the cultivation 48h down.To contain 30～300 clump count in the plate as clump count sum bioassay standard, every kind of dilution factor is done three groups of parallel tests, the meansigma methods of getting 3 plate clump counts.The calculating antibiotic rate=(A-B)/B * 100%, wherein A is blank correlated clump count; B is the clump count of the mixed liquor of certain hour cultivation.
As can be seen from Figure 1 the prepared microcapsule outer wall is smooth closely knit, has good containment.
Claims (6)
1. the method for preparing of an antibiotic property mugwort oil microcapsule is characterized in that preparation process is following:
The first step: prepare mass concentration respectively and be 3%～5% aqueous gelatin solution and mass concentration and be each 150～250ml of arabic gum aqueous solution of 3%～5%, and two kinds of solution are mixed;
Second step: 4～8g mugwort oil is added in the mixed solution that the first step obtains, low whipping speed 300～500r/min, temperature is under 40～55 ℃, stirs 20～40min, and the mugwort oil mixed and dispersed in above-mentioned mixed solution, is obtained emulsion;
The 3rd step: in second emulsion that obtain of step, add deionized water 70～150ml, low whipping speed is under 300～500r/min condition, stirs 30～50min, obtains diluent;
The 4th step: the pH value of the 3rd diluent that obtain of step is transferred to 3.8～5.0 obtain pre-polymerization liquid;
The 5th step: low whipping speed is under 300～500r/min condition, makes the temperature natural of the 4th pre-polymerization liquid that obtains of step be reduced to 0～5 ℃, and is incubated 40～60min, obtains coagulation liquid;
The 6th step: go on foot the glutaraldehyde 2～5g that adds in the coagulation liquid that obtains as crosslinking and curing agent the 5th, mix homogeneously obtains consolidation liquid;
The 7th step: the consolidation liquid that the 6th step was obtained is warming up to 45 ℃, and low whipping speed is that 400～500r/min reacted 1.5～3 hours down then; Reaction is reduced to 20～25 ℃ with system temperature after finishing, and uses washed with isopropyl alcohol, sucking filtration, and drying at room temperature promptly obtains microcapsule.
2. the method for preparing of antibiotic property mugwort oil microcapsule according to claim 1 is characterized in that: the molecular weight of said gelatin is 5～250,000.
3. the method for preparing of antibiotic property mugwort oil microcapsule according to claim 1 is characterized in that: the mass concentration of said aqueous gelatin solution is 4%.
4. the method for preparing of antibiotic property mugwort oil microcapsule according to claim 1 is characterized in that: the mass concentration of said arabic gum aqueous solution is 4%.
5. the method for preparing of antibiotic property mugwort oil microcapsule according to claim 1 is characterized in that: the pH value of diluent transfers to 3.8 in the 4th step.
6. the method for preparing of antibiotic property mugwort oil microcapsule according to claim 1 is characterized in that: the addition of glutaraldehyde is 2g in the 6th step.
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| CN114768697A (en) * | 2022-04-03 | 2022-07-22 | 湖州市食品药品检验研究院(湖州市药品和医疗器械不良反应监测中心、湖州市医疗器械监督检验中心、湖州市食品认证审评和粮油质量监测中心) | Preparation process and preparation device of cinnamon essential oil microcapsules |
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Application publication date: 20120718 |