CN103170286A - Method for preparing melissa officinalis L. essential oil and beta-cyclodextrin molecule microcapsule - Google Patents
Method for preparing melissa officinalis L. essential oil and beta-cyclodextrin molecule microcapsule Download PDFInfo
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- CN103170286A CN103170286A CN2013100347417A CN201310034741A CN103170286A CN 103170286 A CN103170286 A CN 103170286A CN 2013100347417 A CN2013100347417 A CN 2013100347417A CN 201310034741 A CN201310034741 A CN 201310034741A CN 103170286 A CN103170286 A CN 103170286A
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Abstract
The invention discloses a method for preparing a melissa officinalis L. essential oil and beta-cyclodextrin molecule microcapsule and aims to improve the physical and chemical properties and the stability of the melissa officinalis L. essential oil and expand the application range of the melissa officinalis L. essential oil. The method comprises the following steps of: adding ethanol solution of the melissa officinalis L. essential oil into saturated aqueous solution of beta-cyclodextrin slowly, wherein the molar ratio of citral in the melissa officinalis L. essential oil to beta-cyclodextrin is 1:2, and the volume ratio of the melissa officinalis L. essential oil to ethanol is 3:100; oscillating the solutions for 3 hours at a rotating speed of 160r/min at the temperature of 30 DEGC for complete reaction, preserving a product of reaction at the temperature of 4 DEG C for 4 hours, standing, and precipitating; and filtering the obtained solution, and drying a precipitate at the temperature of 50-70 DEG C for 4 hours to obtain the melissa officinalis L. essential oil and beta-cyclodextrin molecule microcapsule. By encapsulating beta-cyclodextrin and the melissa officinalis L. essential oil, the powder of the molecule microcapsule has extremely good optical and thermal stability; the range of application of the melissa officinalis L. essential oil is expanded; and the method is simple and highly practical.
Description
Technical field
The present invention relates to the preparation method of a kind of lemon mint essential oil-beta-schardinger dextrin-molecular microcapsule.
Background technology
Lemon mint (Melissa officinalis L.) is the Labiatae herbaceos perennial, originates in two sides, European Mediterranean, and the middle and south of China, southwest and Taiwan Province also have wild species to distribute, less cultivation.Herb has pure and fresh citris aromas, is a kind of characteristic fragrant plant of dietotherapeutic.Do vegetables edible, human body is had health care, can eat raw as cold vegetable dish in sauce, also can make the flavoring of salad batching, meat soup.Make medicinal plant, lemon mint and honey mixed edible have the effect that promotes digestion, alleviates throat pain, and fresh balm is made tea to drink and can treat chronic bronchitis, flu, have calm, Cure for insomnia, the effect such as hypotensive.In addition, modern pharmacology studies show that, lemon mint all has larger using value at aspects such as treatment moderate A Cihaimo disease, antimigraine, rheumatism.
The lemon mint essential oil has strong citris aromas, and its main component is citral.The biologically actives such as that this essential oil has is antibiotic, anti-tumor oxidation have a wide range of applications in the fields such as food, medicine and cosmetics.The main component citral of essential oil is not only applicable to allocate edible lemon extract, simultaneously still synthetic irisone, methylionone, V
AAnd V
EImportant source material.But because the lemon mint essential oil is volatile, and, run into light, heat, oxygen etc. and have unstability, for its application brings significant limitation.Therefore, being badly in need of seeking some effective means addresses these problems.
Summary of the invention
The objective of the invention is for the technological deficiency that exists in prior art, and a kind of preparation method of lemon mint essential oil molecular microcapsule is provided, so that improve physicochemical property and the stability thereof of lemon mint essential oil, enlarge its range of application.
For realizing that the technical scheme that purpose of the present invention adopts is:
The preparation method of a kind of lemon mint essential oil-beta-schardinger dextrin-molecular microcapsule is characterized in that, comprises the steps:
(1) slowly add lemon mint essential oil ethanolic solution in the saturated beta-schardinger dextrin-aqueous solution, wherein, in the lemon mint essential oil, the mol ratio of citral and beta-schardinger dextrin-is 1:2; In described lemon mint essential oil ethanolic solution, the volume ratio of lemon mint essential oil and ethanol is 3:100;
(2) mentioned solution after 3-4h fully reacts completely, in approximately preserving under 4 ℃ of conditions, is made the microcapsules precipitation of generation in vibration under room temperature condition at 100-200r/min;
(3) with step (2) gained solution filter, sediment is dry 4h under constant temperature 50-70 ℃ condition, obtains lemon mint essential oil-beta-schardinger dextrin-molecular microcapsule.
The preparation process of the described saturated beta-schardinger dextrin-aqueous solution is: with beta-schardinger dextrin-be placed in water in, ultrasonic and control temperature at 25-35 ℃ to dissolving fully, the mass volume ratio of described beta-schardinger dextrin-and water is 1:25.
The time of preserving under 4 ℃ of conditions is 24h at least, makes the microcapsules precipitation of generation.
There is essential oil for fear of surface of microcapsule, filters the gained sediment and clean 2-3 time with benzinum, and then freeze-day with constant temperature.
Compared with prior art, the invention has the beneficial effects as follows:
1, method of the present invention, by determining the relationship between quantities between the process conditions of embedding temperature, each step and each component, utilize the ability of the hydrophobicity cavity generation inclusion complex of beta-schardinger dextrin-, make beta-schardinger dextrin-and lemon mint essential oil carry out embedding, namely improve physicochemical property and the stability thereof of lemon mint essential oil by the molecular microcapsule technology, the molecular microcapsule powder that obtains has fabulous light, heat endurance, has enlarged the application of lemon mint essential oil.
2, method of the present invention has prepared the microcapsules of beta-schardinger dextrin-and lemon mint essential oil by saturated water solution method, the preparation method is simple, practical.
3, method of the present invention, in the embedding process, temperature is controlled at 30 ℃ of left and right, to improve embedding rate.Because the embedding reaction is exothermic reaction, excess Temperature can suppress the carrying out of embedding reaction, and the too low meeting of temperature is too much separated out the cyclodextrin in saturated cyclodextrin solution affects embedding rate.
Description of drawings
Figure 1 shows that the heat endurance of beta-schardinger dextrin--lemon mint essential oil microcapsules and beta-schardinger dextrin--lemon mint essential oil physical mixture;
Figure 2 shows that the anti-photodissociation of beta-schardinger dextrin--lemon mint essential oil microcapsules and beta-schardinger dextrin--lemon mint essential oil physical mixture;
Figure 3 shows that the solid diffuse reflection ultraviolet spectrogram of beta-schardinger dextrin-and beta-schardinger dextrin--lemon mint essential oil microcapsules; Wherein curve 1 is beta-schardinger dextrin-, and curve 2 is beta-schardinger dextrin--lemon mint essential oil microcapsules.
The specific embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
(1) the 10g beta-schardinger dextrin-is placed in 250mL water, ultrasonic and control temperature is extremely dissolved fully at 25-35 ℃, obtains the saturated beta-schardinger dextrin-aqueous solution.
(2) with 0.3mL lemon mint essential oil, join in the 10mL absolute ethyl alcohol and dissolve, make lemon mint essential oil ethanolic solution.
(3) get the saturated beta-schardinger dextrin-aqueous solution 100mL that step (1) obtains, slowly add the lemon mint essential oil ethanolic solution of step (2) gained.Wherein, in the lemon mint essential oil, the mol ratio of citral and beta-schardinger dextrin-is 1:2.
(4) after 3-4h fully reacts completely, in approximately preserving 24h under 4 ℃ of conditions, the microcapsules of generation are staticly settled in vibration under room temperature condition at 100-200r/min step (3) gained solution.
(5) with step (4) gained solution filter, there is essential oil for fear of surface of microcapsule, filter the gained sediment and clean 2-3 time with benzinum, then in thermostatic drying chamber under 60 ℃ of conditions dry 4h, obtain lemon mint essential oil-beta-schardinger dextrin-molecular microcapsule.
One, the stability experiment of microcapsules:
1, heat endurance experiment:
1. directly fully mix the physical mixture that obtains beta-schardinger dextrin-and lemon mint essential oil drip 2 lemon mint essential oils in the 1.5g beta-schardinger dextrin-after.
2. take respectively 1. each three parts of gained physical mixtures of embodiment 1 gained lemon mint essential oil-beta-schardinger dextrin-molecular microcapsule of 0.2g and step, be placed in respectively the thermostatic drying chamber of 40 ℃, 60 ℃, 80 ℃, after placing 12h, the 20mg that takes a sample respectively adds the ultrasonic 10min of 20mL absolute ethyl alcohol, gets the absorbance that supernatant is measured the 244nm place after standing.The essential oil retention rate of setting under initial room-temperature (approximately 20 ℃) is 100%, calculates essential oil retention rate at each temperature.Result of the test as shown in Figure 1.
As shown in Figure 1, when temperature rises to 80 ℃ gradually from 20 ℃, in physical mixture, the content of lemon mint essential oil (in citral) drops to 33.6%, and in microscapsule powder, the content of lemon mint essential oil remains unchanged substantially, and the essential oil retention rate is still more than 90%.The heat endurance that the microcapsules that method of the present invention obtains are described obviously is better than physical mixture.
2, anti-photodissociation experiment:
1. directly fully mix the physical mixture that obtains beta-schardinger dextrin-and lemon mint essential oil drip 2 lemon mint essential oils in the 1.5g beta-schardinger dextrin-after.
2. take respectively solid microscapsule powder and the step physical mixture 1. of 0.5g embodiment 1, irradiation is 7 days under room temperature daylight, and the 20mg that takes a sample respectively adds the ultrasonic 10min of 20mL absolute ethyl alcohol, gets the absorbance that supernatant is measured the 244nm place after standing.When being set in the 0th day, the essential oil retention rate is 100%, calculates the essential oil retention rate in sample every day.Result of the test as shown in Figure 2.
As shown in Figure 2, in microscapsule powder the variation of the content of lemon mint essential oil (in citral) in 7 days little, and the physical mixture of beta-schardinger dextrin-and lemon mint essential oil is in the time of the 7th day, the essential oil retention rate has dropped to 31.6%.These microcapsules that prove absolutely that method of the present invention obtains have stronger anti-photodissociation.
Two, being determined as follows of citral content in microscapsule powder:
Accurately take 0.03g solid microscapsule powder and insert in 50mL tool plug conical flask, standing after sonic oscillation 10min after adding 30mL ethanol dissolving, get supernatant and measure ultraviolet absorptivity at 244nm place, according to the content of calibration curve calculating citral.
Three, the evaluation of solid microcapsules
Utilize ultraviolet spectroscopy to measure the solid uv drs collection of illustrative plates of beta-schardinger dextrin-, embodiment 1 gained lemon mint essential oil-beta-schardinger dextrin-molecular microcapsule, result as shown in Figure 3.Owing to cleaning 3 times with benzinum before lemon mint essential oil-beta-schardinger dextrin-molecular microcapsule drying, therefore can think and exist without essential oil on lemon mint essential oil-beta-schardinger dextrin-molecular microcapsule surface, if contain the characteristic peak of the functional group of composition in essential oil in the solid uv drs collection of illustrative plates of lemon mint essential oil-beta-schardinger dextrin-molecular microcapsule, provable essential oil is by the beta-schardinger dextrin-embedding.Fig. 3 shows, compare with the solid uv drs collection of illustrative plates of simple beta-schardinger dextrin-, the solid microcapsules of lemon mint essential oil and beta-schardinger dextrin-have obvious solid uv drs peak at 244nm wavelength place, this characteristic peak with the principal component citral of lemon mint essential oil is consistent, proves that the lemon mint essential oil is by cyclodextrin embedding.
Method of the present invention has prepared the microcapsules of beta-schardinger dextrin-and lemon mint essential oil by saturated water solution method, this powder characterizes by outer (with integrating sphere device) diffuse reflection method of solid violet, and conclusive evidence contains citral.Investigate through stability experiment, the lemon mint essential oil that obtains-beta-schardinger dextrin-molecular microcapsule has fabulous light, heat endurance, and the method is simple to operate, the practical function highly significant.
The above is only the preferred embodiment of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (5)
1. the preparation method of lemon mint essential oil-beta-schardinger dextrin-molecular microcapsule, is characterized in that, comprises the steps:
(1) slowly add lemon mint essential oil ethanolic solution in the saturated beta-schardinger dextrin-aqueous solution, wherein, in the lemon mint essential oil, the mol ratio of citral and beta-schardinger dextrin-is 1:2; In described lemon mint essential oil ethanolic solution, the volume ratio of lemon mint essential oil and ethanol is 3:100;
(2) mentioned solution after 3-4h fully reacts completely, is preserved under 4 ℃ of conditions in vibration under room temperature condition at 100-200r/min, made the microcapsules precipitation of generation;
(3) with step (2) gained solution filter, filter the gained sediment dry under constant temperature 50-70 ℃ condition, obtain lemon mint essential oil-beta-schardinger dextrin-molecular microcapsule.
2. the preparation method of lemon mint essential oil according to claim 1-beta-schardinger dextrin-molecular microcapsule, it is characterized in that, the preparation process of the described saturated beta-schardinger dextrin-aqueous solution is: beta-schardinger dextrin-is placed in water, and ultrasonic and control temperature is extremely dissolved fully at 25-35 ℃.
3. the preparation method of lemon mint essential oil according to claim 2-beta-schardinger dextrin-molecular microcapsule, is characterized in that, the mass volume ratio of described beta-schardinger dextrin-and water is 1:25.
4. the preparation method of lemon mint essential oil according to claim 1 and 2-beta-schardinger dextrin-molecular microcapsule, is characterized in that, the time of preserving under 4 ℃ of conditions is 24h at least, makes the microcapsules precipitation of generation.
5. the preparation method of lemon mint essential oil according to claim 1 and 2-beta-schardinger dextrin-molecular microcapsule, is characterized in that, has essential oil for fear of surface of microcapsule, filter the gained sediment and clean 2-3 time with benzinum, and then freeze-day with constant temperature.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103394313A (en) * | 2013-07-31 | 2013-11-20 | 湖南农业大学 | Method for preparing microcapsules of terpene-removed citrus peel essential oil |
| CN103396891A (en) * | 2013-07-30 | 2013-11-20 | 桂林兴安安明食品有限公司 | Method for extracting essential oil by taking jackfruit peel as raw material |
| CN103910911A (en) * | 2014-03-27 | 2014-07-09 | 华侨大学 | Preparation method of long-acting antibacterial edible film with sustained release effect |
| CN104907022A (en) * | 2015-05-15 | 2015-09-16 | 浙江纺织服装职业技术学院 | Composite type aromatic microcapsule and silver-loaded aromatic microcapsule preparation method |
| CN104921406A (en) * | 2015-07-06 | 2015-09-23 | 陕西科技大学 | Preparation method for antifungal and deodorized insole |
| 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 |
| CN107051342A (en) * | 2017-04-21 | 2017-08-18 | 贺州学院 | A kind of preparation method of navel orange pericarp 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 |
| CN108741408A (en) * | 2018-04-19 | 2018-11-06 | 金华市博益飞科技有限公司 | Insole and preparation method thereof with health-care efficacy |
| CN108782924A (en) * | 2018-05-11 | 2018-11-13 | 中玺（天津）枣业技术工程中心 | Jujube maltose and preparation method thereof |
| CN108813165A (en) * | 2018-05-29 | 2018-11-16 | 福建农业职业技术学院 | Pig Lavender feed addictive and preparation method thereof |
| CN112451506A (en) * | 2020-12-10 | 2021-03-09 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of essential oil sustained-release capsule |
| CN117243227A (en) * | 2023-09-19 | 2023-12-19 | 西昌学院 | Preparation method and application of lemon grass-thyme composite essential oil microcapsule |
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| CN103396891A (en) * | 2013-07-30 | 2013-11-20 | 桂林兴安安明食品有限公司 | Method for extracting essential oil by taking jackfruit peel as raw material |
| CN103394313A (en) * | 2013-07-31 | 2013-11-20 | 湖南农业大学 | Method for preparing microcapsules of terpene-removed citrus peel essential oil |
| CN103910911A (en) * | 2014-03-27 | 2014-07-09 | 华侨大学 | Preparation method of long-acting antibacterial edible film with sustained release effect |
| CN103910911B (en) * | 2014-03-27 | 2016-10-05 | 华侨大学 | A kind of preparation method of the long acting antibiotic edible film having slow releasing function |
| CN104907022A (en) * | 2015-05-15 | 2015-09-16 | 浙江纺织服装职业技术学院 | Composite type aromatic microcapsule and silver-loaded aromatic microcapsule preparation method |
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| CN104921406A (en) * | 2015-07-06 | 2015-09-23 | 陕西科技大学 | Preparation method for antifungal and deodorized insole |
| CN105062689B (en) * | 2015-08-26 | 2018-12-04 | 江西中烟工业有限责任公司 | A kind of preparation method and application of compound plant essential oil and its microcapsule product |
| 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 |
| CN107051342A (en) * | 2017-04-21 | 2017-08-18 | 贺州学院 | A kind of preparation method of navel orange pericarp 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 |
| CN108741408A (en) * | 2018-04-19 | 2018-11-06 | 金华市博益飞科技有限公司 | Insole and preparation method thereof with health-care efficacy |
| CN108782924A (en) * | 2018-05-11 | 2018-11-13 | 中玺（天津）枣业技术工程中心 | Jujube maltose and preparation method thereof |
| CN108813165A (en) * | 2018-05-29 | 2018-11-16 | 福建农业职业技术学院 | Pig Lavender feed addictive and preparation method thereof |
| CN112451506A (en) * | 2020-12-10 | 2021-03-09 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of essential oil sustained-release capsule |
| CN117243227A (en) * | 2023-09-19 | 2023-12-19 | 西昌学院 | Preparation method and application of lemon grass-thyme composite essential oil microcapsule |
| CN117243227B (en) * | 2023-09-19 | 2024-04-05 | 西昌学院 | Preparation method and application of lemon grass-thyme composite essential oil microcapsule |
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Application publication date: 20130626 |