CN102019160A - Polylactic acid-capsaicin nano-capsule and preparation method thereof - Google Patents
Polylactic acid-capsaicin nano-capsule and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a polylactic acid-capsaicin nano-capsule and preparation method thereof. The method comprises the following steps: (1) preparing a dichloromethane solution of polylactic acid and capsaicin; (2) preparing a polyvinyl alcohol aqueous solution; (3) adding the solution in step (1) into the solution in step (2) and performing ultrasonic emulsification to obtain an emulsion; (4) heating the emulsion in step (3) to 40-50 DEG C to obtain a white emulsion and filtering the emulsion by a 100 nm microporous filter membrane to obtain a colloidal solution; (5) centrifuging the colloidal solution in step (4) to obtain a solid and vacuum drying the solid to obtain a polylactic acid nano-capsule. The polylactic acid nano-capsule of the present invention has a small particle size with a distribution of 30-90 nm; and the raw materials are biodegradable, is benefic to environment protection; the preparation process is simple, of low production cost, and easy to carry out. The prepared polylactic acid nano-capsule of capsaicin is applicable to adhesives, paints, electrical wires, cables, communication facilities, medicine, etc.
Description
Technical field
The present invention relates to a kind of polylactic acid nano capsule that contains capsicim and preparation method thereof.
Background technology
Capsicim is a kind of alkaloid that contains the vanilla acid amides.The natural capsicum element by capsicim, Dihydrocapsaicin, fall serial congener such as Dihydrocapsaicin, high Dihydrocapsaicin, high capsicim family and formed, wherein anti--8-methyl-N-vanillyl-6-nonene base acid amides has strong acid and excitant most, is main chemical compositions pungent in the pepper fruit.Place in plague of rats wildness; electric wire, cable, communications service, packaging material, cereal etc. usually can take place be damaged situation; all adopted poisonous expelling mouse agent in the past; but they not only destroy environment; and poor stability; special packaging material for feed, grain, foodstuff must nontoxic material safe in utilization.Therefore in addition, capsicim also shows the effect of stronger inhibition botrytis cinerea, can be used for preventing and treating the disease and pest behind the fruit and vegetable picking, and fresh-keeping with respect to the organic synthesis medicine has great advantage.
But,, can be unfavorable for operator's use because of its strong acid if directly capsicim is joined in the macromolecular material; In addition, the permanence of its effect also can be affected.
Nano capsule also claims milimicron vesicle, has been new developing technology since the eighties in 20th century, is the new material that has nano-scale in the microcapsules.The Nano capsule that is formed by polymer has outstanding advantage with respect to common microcapsules, enjoys people's attention because of its particular performances.It has been applied to fields such as medicine, spices, fire retardant, oil product and food seasoning.
Nano capsule is better than general other microparticle formulation part and is: 1. because material therefor is convenient to further finishing, improves envelop rate, is changed distribution and target, can transfer initiatively target to by passive target; 2. from present material therefor, its finished product stability is good, is convenient to processing and sterilization; 3. as select for use suitable material can reach good biocompatibility, can degradation in vivo, toxic and side effect is little; 4. can be made into slow-releasing granules, the prolong drug curative effect; 5. may delay composition in some body the destruction of medicine is increased curative effect.
Up to the present, the preparation method of Nano capsule mainly contains complex phase emulsion method, the precipitation method, self-emulsifying solvent diffusion method etc.Wherein, the complex phase emulsion method removes the solvent in the wall material by heating and solvent extraction for the first emulsification system with wall material solution and the formation of the core aqueous solution is distributed in the aqueous medium with micro-droplet status then gradually, and the wall capsule is separated out and will be formed to solute; The precipitation method are that the interface disturbance phenomenon that produces during by organic facies and water immiscible phase and the conversion of dicyandiamide solution make wall material parcel core form nano level particulate, and along with the volatilization of solvent constantly to interfacial migration, precipitation.
But, above-mentioned method, exist an obvious defects to be that core is not dissolved in the water, but form the aqueous solution with the suspension state, and its granular size directly influences final capsule grain diameter size, and therefore prepared capsule grain diameter is bigger, the nano particle ratio is little, wider distribution, and seal weak effect, the medicine carrying amount is low.
Summary of the invention
The technical issues that need to address of the present invention are to disclose a kind of polylactic acid nano capsule that contains capsicim and preparation method thereof, to overcome the defective that prior art exists.
Method of the present invention comprises the steps:
(1) dichloromethane solution of preparation PLA and capsicim, in the solution, the weight concentration of PLA is 2～6%, the weight concentration of capsicim is 1～3%;
Preferably, the weight average molecular weight of described PLA is 80,000～100,000;
(2) preparation polyvinyl alcohol water solution, the weight concentration of polyvinyl alcohol is 1～8%;
(3) solution with step (1) adds in the solution of step (2), and ultrasonic emulsification 2～3 hours obtains emulsion;
The weight ratio of the solution of the solution of step (1) and step (2) is: 1: 3～5;
(4) emulsion with step (3) is heated to 40～50 ℃, stirs 2～3 hours, flings to carrene, gets white emulsion, and adopts the filtering with microporous membrane of 100nm, promptly gets the colloidal solution of light blue opalescence;
(5) with the colloidal solution of step (4), 15000～25000 rev/mins of following centrifugations after 0.5～1.5 hour, the solid of acquisition, 70～90 ℃ of following vacuum drying 2～3 hours, vacuum is 120pa～130pa, obtains described polylactic acid nano capsule;
Described PLA is a kind of the have good biocompatibility and synthesized polymer material of biodegradable.This line style thermoplasticity biodegradable aliphatic polyester is to be initial raw material with the starch that extracts in some plants such as corn, wheat, cassava, decomposition obtains glucose through enzyme, become lactic acid through behind the lactobacillus-fermented again, obtain the high-purity PLA through chemical synthesis then.CO can thoroughly be resolved in the discarded back of polylactic acid article under the effect of microorganism, water, bronsted lowry acids and bases bronsted lowry in soil or water
2And H
2O under sun photosynthesis, becomes the initiation material of starch again subsequently, can not produce environment and pollute, thereby be a kind of Biodegradable material of complete Natural Circulation type.
The invention has the advantages that: the particle diameter of PLA capsule is thin, and particle diameter is distributed as 30～90nm, and adjustable; Used raw material are biodegradable, environmental protection; Preparation technology is simple, production cost is low, easy to implement.Adopt the polylactic acid nano capsule of the capsicim of this method preparation, can be widely used in aspects such as adhesive, coating, electric wire, cable, communications service and medicine.
The specific embodiment
Embodiment 1
(1) PLA and capsicim are added in the carrene, stirring at room 3 hours is dissolved it fully, gets PLA-capsicim solution, and wherein, the weight concentration of PLA is 2%, and the weight concentration of capsicim is 1%, and the weight average molecular weight of PLA is 80,000;
(2) 1 gram polyvinyl alcohol is mixed with 99 gram water, keep 20 ℃ of water temperatures, make its swollen 1.5 hours, be heated to 85 ℃ again, and continue 3 hours, it is fully dissolved, in solution, do not have fine particle, obtain polyvinyl alcohol water solution;
(3) PLA-capsicim solution with 10 grams adds in the 30 gram poly-vinyl alcohol solutions, and ultrasonic emulsification 2 hours obtains emulsion.This emulsion is heated to 40 ℃, stirred 3 hours, fling to carrene, get white emulsion, and adopt the filtering with microporous membrane of 100nm, promptly get the colloidal solution of light blue opalescence.
In centrifuge, 15000 rev/mins are following after centrifugal 1.5 hours with this colloidal solution, the solid of acquisition, and 70 ℃ of following vacuum drying 3 hours, vacuum was 120pa, finally obtained polylactic acid nano capsule of the present invention.
Average size of products sees Table 1.
Embodiment 2
(1) PLA and capsicim are added in the carrene, stirring at room 4 hours is dissolved it fully, gets PLA-capsicim solution, and wherein, the weight concentration of PLA is 4%, and the weight concentration of capsicim is 2%, and the weight average molecular weight of PLA is 90,000;
(2) 5 gram polyvinyl alcohol are mixed with the water of 95 grams, keep 25 ℃ of water temperatures, make its swollen 1 hour, be heated to 90 ℃ again, and continue 2.5 hours, it is fully dissolved, in solution, do not have fine particle, obtain polyvinyl alcohol water solution;
(3) PLA-capsicim solution with 10 grams adds in the 40 gram poly-vinyl alcohol solutions, and ultrasonic emulsification 2.5 hours obtains emulsion.This emulsion is heated to 45 ℃, stirred 2.5 hours, fling to carrene, get white emulsion, and adopt the filtering with microporous membrane of 100nm, promptly get the colloidal solution of light blue opalescence.
With this colloidal solution in centrifuge, 20000 rev/mins down after centrifugal 1 hour, the solid of acquisition, 80 ℃ of following vacuum drying 2.5 hours, vacuum is 125pa, finally obtains polylactic acid nano capsule of the present invention.
Average size of products sees Table 1.
Embodiment 3
(1) PLA and capsicim are added in the carrene, stirring at room 5 hours is dissolved it fully, gets PLA-capsicim solution, and wherein, the weight concentration of PLA is 6%, and the weight concentration of capsicim is 3%, and the weight average molecular weight of PLA is 100,000;
(2) 8 gram polyvinyl alcohol are mixed with the water of 92 grams, keep 30 ℃ of water temperatures, make its swollen 0.5 hour, be heated to 95 ℃ again, and continue 2 hours, it is fully dissolved, in solution, do not have fine particle, obtain polyvinyl alcohol water solution;
(3) PLA-capsicim solution with 10 grams adds in the 50 gram poly-vinyl alcohol solutions, and ultrasonic emulsification 3 hours obtains emulsion.This emulsion is heated to 50 ℃, stirred 2 hours, fling to carrene, get white emulsion, and adopt the filtering with microporous membrane of 100nm, promptly get the colloidal solution of light blue opalescence.
With this colloidal solution in centrifuge, 25000 rev/mins down after centrifugal 0.5 hour, the solid of acquisition, 90 ℃ of following vacuum drying 2 hours, vacuum is 130pa, finally obtains polylactic acid nano capsule of the present invention.
Average size of products sees Table 1.
The average grain diameter of table 1 sample
| Embodiment | Average grain diameter (nm) |
| 1 | 30～50 |
| 2 | 50～70 |
| 3 | 70～90 |
Claims (8)
1. the preparation method of PLA-capsicim Nano capsule is characterized in that, comprises the steps:
(1) dichloromethane solution of preparation PLA and capsicim;
(2) preparation polyvinyl alcohol water solution;
(3) solution with step (1) adds in the solution of step (2), and ultrasonic emulsification obtains emulsion;
(4) with the emulsion heating of step (3), fling to carrene, get white emulsion, and adopt the filtering with microporous membrane of 100nm, the colloidal solution of light blue opalescence must be arranged;
(5) with the colloidal solution of step (4), centrifugation, the solid of acquisition, vacuum drying obtains described polylactic acid nano capsule.
2. method according to claim 1 is characterized in that, in the solution of step (1), the weight concentration of PLA is 2～6%, and the weight concentration of capsicim is 1～3%.
3. method according to claim 1 is characterized in that, in the aqueous solution of step (2), the weight concentration of polyvinyl alcohol is 1～8%.
4. method according to claim 2 is characterized in that, in the aqueous solution of step (2), the weight concentration of polyvinyl alcohol is 1～8%.
5. according to each described method of claim 1～4, it is characterized in that in the step (3), the solution of step (1) is added in the solution of step (2), ultrasonic emulsification 2～3 hours obtains emulsion.
6. method according to claim 5 is characterized in that, in the step (3), the weight ratio of the solution of the solution of step (1) and step (2) is: 1: 3～5.
7. method according to claim 5 is characterized in that, the weight average molecular weight of described PLA is 80,000～100,000.
8. according to the PLA-capsicim Nano capsule of each described method preparation of claim 1～7.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102919226A (en) * | 2012-12-03 | 2013-02-13 | 贵州省烟草科学研究院 | Abscisic acid nano-emulsion and preparation method thereof |
| CN102960337A (en) * | 2012-12-03 | 2013-03-13 | 贵州省烟草科学研究院 | Butralin nano emulsion and preparation method thereof |
| CN103437191A (en) * | 2013-08-02 | 2013-12-11 | 南京天脉健康管理有限公司 | Nano cannabis sativa oil microcapsule, nano cannabis sativa oil microcapsule fabric, preparation method of nano cannabis sativa oil microcapsule fabric and prepared product |
| CN107156119A (en) * | 2017-06-23 | 2017-09-15 | 中国农业科学院农业环境与可持续发展研究所 | A kind of nano-pesticide formulation and preparation method thereof |
| CN107173433A (en) * | 2017-07-04 | 2017-09-19 | 苏州农业职业技术学院 | A kind of fruit antistaling agent containing capsaicine |
| CN107258778A (en) * | 2017-06-23 | 2017-10-20 | 中国农业科学院农业环境与可持续发展研究所 | The preparation method of pesticide nano capsules |
| CN107306942A (en) * | 2017-06-23 | 2017-11-03 | 中国农业科学院农业环境与可持续发展研究所 | The preparation method of control release type nano-pesticide formulation |
| CN107347881A (en) * | 2017-06-23 | 2017-11-17 | 中国农业科学院农业环境与可持续发展研究所 | A kind of pesticide nano capsules and preparation method thereof |
| CN107815047A (en) * | 2017-09-29 | 2018-03-20 | 当涂县瑞龙果树种植专业合作社 | A kind of agricultural solid mulch film of slow release chemical fertilizer type water resistance and preparation method thereof |
| CN108102195A (en) * | 2017-12-28 | 2018-06-01 | 成都新柯力化工科技有限公司 | A kind of cable insulation material and preparation method containing self-repairing microcapsule |
| CN112262851A (en) * | 2020-11-23 | 2021-01-26 | 广东省农业科学院植物保护研究所 | Acetamiprid microcapsule suspending agent |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102919226A (en) * | 2012-12-03 | 2013-02-13 | 贵州省烟草科学研究院 | Abscisic acid nano-emulsion and preparation method thereof |
| CN102960337A (en) * | 2012-12-03 | 2013-03-13 | 贵州省烟草科学研究院 | Butralin nano emulsion and preparation method thereof |
| CN102960337B (en) * | 2012-12-03 | 2015-03-18 | 贵州省烟草科学研究院 | Butralin nano emulsion and preparation method thereof |
| CN103437191A (en) * | 2013-08-02 | 2013-12-11 | 南京天脉健康管理有限公司 | Nano cannabis sativa oil microcapsule, nano cannabis sativa oil microcapsule fabric, preparation method of nano cannabis sativa oil microcapsule fabric and prepared product |
| CN103437191B (en) * | 2013-08-02 | 2015-07-08 | 南京天脉健康管理有限公司 | Nano cannabis sativa oil microcapsule, nano cannabis sativa oil microcapsule fabric, preparation method of nano cannabis sativa oil microcapsule fabric and prepared product |
| CN107306942A (en) * | 2017-06-23 | 2017-11-03 | 中国农业科学院农业环境与可持续发展研究所 | The preparation method of control release type nano-pesticide formulation |
| CN107258778A (en) * | 2017-06-23 | 2017-10-20 | 中国农业科学院农业环境与可持续发展研究所 | The preparation method of pesticide nano capsules |
| CN107156119A (en) * | 2017-06-23 | 2017-09-15 | 中国农业科学院农业环境与可持续发展研究所 | A kind of nano-pesticide formulation and preparation method thereof |
| CN107347881A (en) * | 2017-06-23 | 2017-11-17 | 中国农业科学院农业环境与可持续发展研究所 | A kind of pesticide nano capsules and preparation method thereof |
| CN107347881B (en) * | 2017-06-23 | 2021-03-19 | 中国农业科学院农业环境与可持续发展研究所 | Pesticide nanocapsule and preparation method thereof |
| CN107258778B (en) * | 2017-06-23 | 2021-03-19 | 中国农业科学院农业环境与可持续发展研究所 | Preparation method of pesticide nanocapsule |
| CN107173433A (en) * | 2017-07-04 | 2017-09-19 | 苏州农业职业技术学院 | A kind of fruit antistaling agent containing capsaicine |
| CN107815047A (en) * | 2017-09-29 | 2018-03-20 | 当涂县瑞龙果树种植专业合作社 | A kind of agricultural solid mulch film of slow release chemical fertilizer type water resistance and preparation method thereof |
| CN108102195A (en) * | 2017-12-28 | 2018-06-01 | 成都新柯力化工科技有限公司 | A kind of cable insulation material and preparation method containing self-repairing microcapsule |
| CN108102195B (en) * | 2017-12-28 | 2020-10-23 | 石连娥 | Cable insulation material containing self-repairing microcapsules and preparation method |
| CN112262851A (en) * | 2020-11-23 | 2021-01-26 | 广东省农业科学院植物保护研究所 | Acetamiprid microcapsule suspending agent |
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Application publication date: 20110420 |