CN103394313A - Method for preparing microcapsules of terpene-removed citrus peel essential oil - Google Patents
Method for preparing microcapsules of terpene-removed citrus peel essential oil Download PDFInfo
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- CN103394313A CN103394313A CN201310328642XA CN201310328642A CN103394313A CN 103394313 A CN103394313 A CN 103394313A CN 201310328642X A CN201310328642X A CN 201310328642XA CN 201310328642 A CN201310328642 A CN 201310328642A CN 103394313 A CN103394313 A CN 103394313A
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Abstract
The invention discloses a method for preparing microcapsules of terpene-removed citrus peel essential oil. The method comprises the following steps of: on the basis of selecting the terpene-removed citrus peel essential oil as a core material; weighing beta-cyclodextrin serving as a wall material in a ratio of the core material to the wall material of (1:4)-(1:6), adding deionized water in a volume ratio of the beta-cyclodextrin to the water of (1:7)-(1:9), stirring in a water bath of 50-70 DEG C to dissolve the beta-cyclodextrin to obtain a saturated beta-cyclodextrin solution, and cooling to 40-60 DEG C; taking the terpene removed citrus peel essential oil, and dissolving the essential oil into anhydrous ethanol in a volume ratio of the essential oil to the ethanol of (1:15)-(1:25) to obtain an essential oil and ethanol solution; dropwise adding the essential oil and ethanol solution into the saturated beta-cyclodextrin solution with stirring, and sealing in the shade, thereby obtaining a capsule solution at the embedding temperature of 40-60 DEG C; taking the capsule solution out, cooling to room temperature, standing for 20-40 hours at the temperature of 4-10 DEG C, filtering in vacuum, performing freeze drying at the temperature of between 40 DEG C below zero and 60 DEG C below zero to a constant weight, thus obtaining a white microcapsule product.
Description
Technical field
The present invention relates to a kind of essential oil, particularly a kind of microcapsule preparation method that takes off terpene orange peel essential oil.
Background technology
The orange peel essential oil is the class in natural essence spices, and pure and fresh pleasant natural citrus fragrance is arranged.The oxygenatedchemicals that the main component of orange peel essential oil is comprised of monoterpene class, sesquiterpene and higher alcohols, aldehydes, ketone, ester class, phenols, acids etc., wherein the content with citrene is the highest.Yet, citrene is a kind of monocyclic monoterpene alkene, it is little to essential oil fragrance component contribution, but its chemical property is active, in processing and store improperly under condition, meet oxygen and illumination meeting and be oxidized to rapidly the citrene peroxide, and this class peroxide is unstable, can further convert a series of smell substances such as carvol, carveol to, thereby causes the quality of essential oil to descend, storage life shortens, and use is affected.
In order to improve the stability of orange peel essential oil, can adopt the method for embedding,, with the citrus essential oil microencapsulation, to reduce contacting of citrus essential oil and air, thereby alleviate degree of oxidation, raising stability.But, due to the complicated component of citrus essential oil, can't be disposable that all the components is all embedded, need first the citrene of one-component is carried out embedding, and then with citrus essential oil, remove to replace citrene in microcapsules, to improve the embedding effect.This process, need the technique of the series of complexes such as emulsification, high temperature drying, makes the embedding process of citrus essential oil complicated, and the embedding weak effect, and product stability is also bad.
In addition, traditional essential oil microcapsules preparation section adopts emulsion process, and this method consisted of two steps: the first step, add a certain amount of emulsifying agent and stabilizing agent, and, with wall material and essential oil mixing and emulsifying, form " wall material-essential oil " emulsification system; Second step, the emulsion after high-pressure homogeneous, then by spray-drying, obtain microcapsule product.This method adds the emulsifying agents such as gelatin, maltodextrin, Arabic gum to do the wall material usually, then through high-pressure homogeneous one-tenth emulsified solution.These had both made production cost increase, and had increased again processing step.Spray-drying also has a shortcoming, and the temperature of hot-air inlets is up to 120～160 ℃, and after atomization drying, outlet temperature is generally 100 ℃ of left and right.Excess Temperature, the cyst wall surface easily produces depression, slight crack, hole, impels essential oil volatilization and oxidation deterioration, has reduced the microcapsules quality, has shortened storage period.In addition, also have direct drying method, this method is to adopt drying box to carry out drying at 50 ℃～60 ℃ wet microcapsules, and the microcapsule embedded rate that this method obtains is relatively not high, and the dry needed time is long, and the fragrance component loss is large.
Summary of the invention
Technical problem to be solved by this invention is; not enough for above-mentioned prior art; provide that a kind of technique is simple, embedding is effective, stability is high, drying means is proper, the fragrance component loss less, the microcapsule preparation method that takes off terpene orange peel essential oil of with low cost, storage endurance; to reduce as far as possible the production cost of microcapsules; the oxidation deterioration that effectively suppresses essential oil; improve the embedding effect of microcapsules; extend shelf time; to better preserving essential oil; protect its fragrance component; expand its range of application, realize the mass industrialized production of essential oil microcapsules.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is: a kind of microcapsule preparation method that takes off terpene orange peel essential oil, it comprises the following steps:
1) choose and take off terpene orange peel essential oil as core;
2) prepare beta-schardinger dextrin-solution: using beta-schardinger dextrin-as the wall material, is 1:4～1:6(volume ml in the ratio of core and wall material: quality g), take beta-schardinger dextrin-; Be 1:7～1:9 by beta-schardinger dextrin-and deionized water volume ratio, add deionized water, stir under 50～70 ℃ of bath temperatures, make its dissolving, obtain the beta-schardinger dextrin-saturated solution, and it is standby to be cooled to 40～60 ℃ of insulations;
3) prepare the essential oil ethanolic solution: get and take off terpene orange peel essential oil,, in taking off terpene orange peel essential oil and the absolute ethyl alcohol volume ratio is the ratio of 1:15～1:25, use anhydrous alcohol solution, make the essential oil ethanolic solution;
4) inclusion: the essential oil ethanolic solution at the uniform velocity and slowly is added drop-wise in the beta-schardinger dextrin-saturated solution, while dripping, stirs, lucifuge sealing 1.5h～2.0h, embedding under 40～60 ℃ of water bath condition, make capsule solution;
5) capsule solution is taken out, after being cooled to room temperature, be placed on standing 20～40h in 4～10 ℃ of environment, after vacuum filtration,, in-40～-60 ℃ of freeze dryings to constant weight, obtain the white microcapsule product.
In such scheme, the described terpene orange peel essential oil that takes off comprises the essential oil that extracts from mandarin orange, tangerine, orange, shaddock, lemon and golden orange peel, then removes the orange peel essential oil that obtains after terpene substances.
The core raw material that the present invention uses is a kind of orange peel essential oil after removing citrene (taking off terpene).Citrene is separated from essential oil, helped to improve essential oil oxytolerant, fast light, heat-resisting ability, slow down essential oil generation qualitative change, improve essential oil stability and aroma quality, extend the storage time of essential oil, the orange peel essential oil can be effectively utilized.
The wall material raw material that the present invention uses is beta-schardinger dextrin-, it is by 7 D(+)-cyclic oligomer that glucopyranose forms, that its molecule is is wide at the top and narrow at the bottom, the tubular article of both ends open, hollow, have in chamber hydrophobic, peripheral hydrophilic special molecular structure, thereby it is even to have inclusion, in conjunction with firm, the product hygroscopicity is low, is difficult for the characteristics of moisture absorption caking.In addition, beta-schardinger dextrin-solubility is low, easily crystallization, separation, purification, and avirulent, easily biological-degradable, and also production cost is lower.
The preparation method that the present invention uses is a kind of non-emulsification vacuum freeze drying microcapsule preparation method.The present invention changes into the essential oil of liquid state solid-state, core is hedged off from the outer world, prevent that it is subjected to the extraneous factors such as ultraviolet ray, oxygen break outer and go bad, improve the stability of core to light, heat, oxygen, also can reduce core volatilization loss, and it is complete that fragrance is kept, thereby extend the essential oil storage time and improve the stability of using, and enlarges the range of application of essential oil.This method does not need the emulsifying process, wall material raw material emulsifier-free, production cost is lower, the drawbacks such as essential oil volatilization while having avoided high temperature in preparation process, material loss, fragrance are poor, embedding is effective, does not need expensive complicated equipment, highly stable under the inclusion compound drying regime, more than 1 year, also can keep the distinctive fragrance of essential oil and fragrance at the room temperature condition sealed type storage, be that a kind of technique is simple, practical, the preparation method of good stability.
With respect to existing essential oil microcapsules preparation method, it mainly directly utilizes essential oil (through taking off terpene, not processing), for raw material, after its emulsifying homogeneous, then to carry out spray-drying or convection drying, and the operating procedure step is many, the embedding weak effect.In addition, HTHP is not suitable for volatile orange peel essential oil, and its fragrance component is easy oxidation deterioration, volatilization loss under HTHP.
We, through repetition test research, have obtained a kind of non-emulsification vacuum freeze drying of terpene essential oil microcapsule preparation method that takes off.Ethanol and the impact of the parameters such as essential oil volume ratio, amount of water, wall/core ratio, embedding temperature, inclusion time on microcapsule embedded effect have also been studied simultaneously.The microcapsules of the present invention's preparation are compared with the microcapsules of conventional method preparation, not only save a large amount of solvents, and embedding are effective, and the essential oil loss is less, and the orange peel essential oil microcapsules embedding rate that obtains is high, particle size uniformity good, good stability, and the holding time is long.
Compared with prior art, the present invention has the following advantages:
1, essential oil is processed through taking off terpene, reduced be heated in the preparation process, influence of light and the oxidation deterioration that causes, kept the character of essential oil, stability and the fragrance component utilization rate of essential oil have been improved, product has higher productive rate, and mobility of particle and dissolubility are good, extended pot life.
2, technique is simple, and handling safety is easily controlled.The preparation technology of this invention does not need the technical process such as high pressure is sheared, high-pressure homogeneous, emulsification; In related technique, do not need the process equipments such as homogenizer, reduced simultaneously energy consumption for drying, and not with an organic solvent, security is good, be fit to suitability for industrialized production.
3, need not add other auxiliary material, cost is low.The microcapsules that the present invention produces, wall material raw material is beta-schardinger dextrin-, emulsifier-free, production cost is lower.
4, the microcapsules rate is high, and fragrance remaining time was more than 1 year, and after dissolving, fragrance discharges fast.
5, product easy to use, be convenient to store, transportation and application.The microcapsules that the present invention produces are powder-product, use at normal temperatures Packing treatment, keep in Dark Place and get final product.
Detect through experiment, the microcapsules performance rating situation of taking off terpene orange peel essential oil of using the present invention to produce is as shown in table 1:
Table 1 takes off terpene citrus essential oil microcapsules index
Specific embodiment
Embodiment 1:
Take the 10.00g beta-schardinger dextrin-, with the 80mL deionized water, stir and make its dissolving under 70 ℃ of bath temperatures, obtain the beta-schardinger dextrin-saturated solution, be cooled to 50 ℃ of insulations standby.Get 2mL and take off terpene Pon orange peel essential oil, by the volume ratio of 1: 20 with anhydrous alcohol solution after, at the uniform velocity and dropwise join in beta-schardinger dextrin-solution, the limit edged stirs, the lucifuge sealing, after inclusion 2h, solution is being taken out under 50 ℃ of bath temperatures, after solution is chilled to room temperature, be placed on standing 24h in 4 ℃ of refrigerators, vacuum filtration,, with being dried to constant weight after appropriate absolute ethanol washing in-40 ℃ of freeze driers, obtain the white microcapsule product.
Embodiment 2:
Take the 8.00g beta-schardinger dextrin-, with the 72mL deionized water, stir and make its dissolving under 60 ℃ of bath temperatures, obtain the beta-schardinger dextrin-saturated solution, be cooled to 40 ℃ of insulations standby.Get 2mL and take off terpene tangerine orange peel essential oil, by the volume ratio of 1: 25 with anhydrous alcohol solution after, at the uniform velocity and dropwise join in beta-schardinger dextrin-solution, the limit edged stirs, the lucifuge sealing, after inclusion 1.5h, solution is being taken out under 60 ℃ of bath temperatures, after solution is chilled to room temperature, be placed on standing 30h in 8 ℃ of refrigerators, vacuum filtration,, with being dried to constant weight after appropriate absolute ethanol washing in-50 ℃ of freeze driers, obtain the white microcapsule product.
Embodiment 3:
Take the 10.00g beta-schardinger dextrin-, with the 70mL deionized water, stir and make its dissolving under 65 ℃ of bath temperatures, obtain the beta-schardinger dextrin-saturated solution, be cooled to 50 ℃ of insulations standby.Get 2mL and take off terpene sweet orange peel essential oil, by the volume ratio of 1: 15 with anhydrous alcohol solution after, at the uniform velocity and dropwise join in beta-schardinger dextrin-solution, the limit edged stirs, the lucifuge sealing, after inclusion 1.5h, solution is being taken out under 45 ℃ of bath temperatures, after solution is chilled to room temperature, be placed on standing 40h in 10 ℃ of refrigerators, vacuum filtration,, with being dried to constant weight after appropriate absolute ethanol washing in-60 ℃ of freeze driers, obtain the white microcapsule product.
The microcapsules product that embodiment 1～3 gained microcapsules product and traditional diamond-making technique are made compares, and obtains result as shown in table 2.
Table 2
Claims (2)
1. a microcapsule preparation method that takes off terpene orange peel essential oil, is characterized in that comprising the following steps:
1) choose and take off terpene orange peel essential oil as core;
2) prepare beta-schardinger dextrin-solution: using beta-schardinger dextrin-as the wall material, is 1:4～1:6 in the volume mass ratio of core and wall material, takes beta-schardinger dextrin-; Be 1:7～1:9 by beta-schardinger dextrin-and deionized water volume ratio, add deionized water, stir under 50～70 ℃ of water bath condition and make its dissolving, obtain the beta-schardinger dextrin-saturated solution, and it is standby to be cooled to 40～60 ℃ of insulations;
3) prepare the essential oil ethanolic solution: get and take off terpene orange peel essential oil,, in taking off terpene orange peel essential oil and the absolute ethyl alcohol volume ratio is the ratio of 1:15～1:25, use anhydrous alcohol solution, make the essential oil ethanolic solution;
4) inclusion: the essential oil ethanolic solution at the uniform velocity and slowly is added drop-wise in the beta-schardinger dextrin-saturated solution, while dripping, stirs, lucifuge sealing 1.5h～2.0h, embedding under 40～60 ℃ of water bath condition, make capsule solution;
5) capsule solution is taken out, after being cooled to room temperature, be placed on standing 20～40h in 4～10 ℃ of environment, after vacuum filtration,, in-40～-60 ℃ of freeze dryings to constant weight, obtain the white microcapsule product.
2. the microcapsule preparation method that takes off terpene orange peel essential oil according to claim 1, it is characterized in that, the described terpene orange peel essential oil that takes off comprises the essential oil that extracts from mandarin orange, tangerine, orange, shaddock, lemon and golden orange peel, then removes the orange peel essential oil that obtains after terpene substances.
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Cited By (17)
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| CN106562492A (en) * | 2015-10-10 | 2017-04-19 | 普宁市纺织服装科技研究院 | Tangerine powder microcapsule anti-oxidation face mask liner, preparation method and application |
| CN107051342A (en) * | 2017-04-21 | 2017-08-18 | 贺州学院 | A kind of preparation method of navel orange pericarp essential oil microcapsules |
| CN107287033A (en) * | 2017-07-14 | 2017-10-24 | 宝鸡文理学院 | A kind of preparation method of sandalwood essential oil microcapsules |
| CN108531298A (en) * | 2018-04-10 | 2018-09-14 | 上海应用技术大学 | A kind of washing powder and preparation method thereof containing gold bergamot essential oil microcapsules |
| CN109566875A (en) * | 2018-12-07 | 2019-04-05 | 福建农业职业技术学院 | A kind of coating technique of Lavender |
| CN111085142A (en) * | 2019-12-16 | 2020-05-01 | 东莞波顿香料有限公司 | Orange oil nano dispersion, preparation method thereof, transparent beverage and detergent |
| CN111876255A (en) * | 2020-08-31 | 2020-11-03 | 江西中医药大学 | Kumquat essential oil slow-release sachet and manufacturing method and application thereof |
| CN111938018A (en) * | 2020-08-19 | 2020-11-17 | 四川爱邦伟业生物工程有限责任公司 | Preparation method of anti-mildew Chinese herbal medicine feed additive |
| CN112274684A (en) * | 2020-10-30 | 2021-01-29 | 张茂刚 | Air freshener and preparation method thereof |
| CN113854464A (en) * | 2021-09-26 | 2021-12-31 | 哈工大机器人南昌智能制造研究院 | Citrus essential oil capsule and preparation method thereof |
| CN114010800A (en) * | 2021-11-08 | 2022-02-08 | 福建省农业科学院农业质量标准与检测技术研究所 | Preparation method of turmeric essential oil microcapsule |
| CN114711408A (en) * | 2021-12-31 | 2022-07-08 | 南通奥凯生物技术开发有限公司 | Method for preparing microencapsulated shaddock peel oil by freeze drying method |
| CN116492944A (en) * | 2023-06-21 | 2023-07-28 | 云南省农业科学院农产品加工研究所 | Microcapsule wall material and preparation method and application thereof |
| CN117845656A (en) * | 2024-03-08 | 2024-04-09 | 山东东宇鸿翔装饰材料有限公司 | Formaldehyde-cleaning antibacterial melamine impregnated paper and preparation method thereof |
| CN117845656B (en) * | 2024-03-08 | 2024-05-24 | 山东东宇鸿翔装饰材料有限公司 | Formaldehyde-cleaning antibacterial melamine impregnated paper and preparation method thereof |
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| CN103861537B (en) * | 2014-03-20 | 2016-01-06 | 中国热带农业科学院农产品加工研究所 | A kind of preparation method of essential oil microcapsules |
| CN103861537A (en) * | 2014-03-20 | 2014-06-18 | 中国热带农业科学院农产品加工研究所 | Preparation method of essential oil microcapsule |
| CN105062689A (en) * | 2015-08-26 | 2015-11-18 | 江西中烟工业有限责任公司 | Compound plant essential oil, preparing method of microcapsule product thereof and application of microcapsule product |
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| CN114010800A (en) * | 2021-11-08 | 2022-02-08 | 福建省农业科学院农业质量标准与检测技术研究所 | Preparation method of turmeric essential oil microcapsule |
| CN114711408A (en) * | 2021-12-31 | 2022-07-08 | 南通奥凯生物技术开发有限公司 | Method for preparing microencapsulated shaddock peel oil by freeze drying method |
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Application publication date: 20131120 |