CN104189046A - Method for preparing artemisia volatile oil microcapsule - Google Patents
Method for preparing artemisia volatile oil microcapsule Download PDFInfo
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- CN104189046A CN104189046A CN201410445649.4A CN201410445649A CN104189046A CN 104189046 A CN104189046 A CN 104189046A CN 201410445649 A CN201410445649 A CN 201410445649A CN 104189046 A CN104189046 A CN 104189046A
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- volatile oil
- herba artemisiae
- artemisiae annuae
- cyclodextrin
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Abstract
The invention relates to a method for preparing an artemisia volatile oil microcapsule, and in particular relates to a method for preparing an artemisia volatile oil microcapsule by using ultrasonic waves. The preparation method is characterized by comprising the following steps: adding beta-cyclodextrin which serves as a wall material to prepare a beta-cyclodextrin aqueous solution, and uniformly stirring until the beta-cyclodextrin is completely dissolved, thus obtaining a solution for later use; stirring, adding artemisia volatile oil, serving as a core material, to the solution, and uniformly dispersing the artemisia volatile oil to obtain an emulsion; ultrasonically processing the obtained emulsion in an ultrasonic device; and refrigerating, carrying out suction filtering and freeze-drying to obtain the finished artemisia volatile oil microcapsule. The prepared artemisia volatile oil microcapsule disclosed by the invention is solid powder; the method can effectively inhibit volatilization of the artemisia volatile oil and prolong preservation time of the artemisia volatile oil, so that the artemisia volatile oil has long-lasting fragrance; in addition, by preparing the artemisia volatile oil microcapsule through ultrasonic processing, the method is simple and convenient to operate and is quick and feasible.
Description
Technical field
The present invention relates to a kind of method of preparing Herba Artemisiae Annuae volatile oil microcapsule, be specifically related to a kind of method of utilizing ultrasound wave to prepare Herba Artemisiae Annuae volatile oil microcapsule.
Background technology
Herba Artemisiae Annuae formal name used at school Herba Artemisiae annuae, belongs to Compositae Chamomile family artemisia, is China's Chinese medicine, has very high medical value.Cold in nature, bitter in the mouth, pungent, returns liver, has special aroma.There is clearing away summer-heat, remove steaming, cut the effects such as cruel, be mainly used in the diseases such as pathogenic summer-heat heating, fever due to yin deficiency, night fever abating at dawn, hectic fever due to YIN-deficiency consumptive disease heat, malaria cold and heat, jaundice due to damp-heat.Herba Artemisiae Annuae volatile oil is one of main active of Herba Artemisiae Annuae, is a kind of light yellow transparent liquid, has strong aromatic odor, have antibacterial, relieving asthma, the pharmacological action such as antipyretic, cough-relieving.The clinical various diseases such as neural dermatitis, fungus that are used for the treatment of, can induce people's liver cancerous cell generation apoptosis.
The most of compositions of volatile oil are volatile organic compound, and volatile in direct use procedure, some thermal sensitivity compositions and heliosensitivity composition are unstable, thereby destroy the biological activity of material.
Microcapsule technology refers to utilizes natural or synthesized polymer material, by the solid, the liquid that disperse, or even gaseous matter parcel, form the technology that there is semi permeability or seal the fine particle of cyst membrane.These fine particles are called as microcapsule.The ability of utilizing the hydrophobic cavity generation inclusion complex of cyclodextrin, can make many active component and cyclodextrin generate complex, reaches stable by inclusion complex physico-chemical property, reduces oxidation, passivation heliosensitivity and thermal sensitivity, reduces volatile object.
Summary of the invention
The object of the present invention is to provide a kind of method of preparing Herba Artemisiae Annuae volatile oil microcapsule.
The present invention includes following steps:
A. by wall material
β-cyclodextrin joins in the hot water of 60 ~ 90 ℃ and is prepared into
βthe mass ratio of-cyclodextrin and water is the solution of 6g/100g ~ 15g/100g, stirs, standby until completely dissolved;
B. get core Herba Artemisiae Annuae volatile oil, determine
β-cyclodextrin and core Herba Artemisiae Annuae volatile oil mass ratio 8g/g ~ 15g/g, join core Herba Artemisiae Annuae volatile oil in above-mentioned solution while stirring, and Herba Artemisiae Annuae volatile oil is uniformly dispersed, and homogenizing obtains emulsion;
C. the emulsion obtaining is put in ultrasonic device, control ultrasonic power is that 50 ~ 100W, ultrasonic temperature are 60 ~ 80 ℃, and model of action is powerful cavitation 3s buffering 2s, and be 40 ~ 60min action time;
D. by the emulsion after ultrasonic, under 0 ~ 5 ℃ of condition, after cold preservation 24h, in vacuum, be under 0.06 ~ 0.10MPa and 10 ~ 25 ℃ of conditions of temperature, to adopt Medium speed filter paper to filter, obtain filter cake;
E. filter cake is dry under freezer dryer vacuum 10 ~ 20Pa, condenser temperature-40 ℃ ~-50 ℃ of conditions, obtain Herba Artemisiae Annuae volatile oil microcapsule product, embedding rate is greater than 75%.
Homogenizing described in step b of the present invention is to adopt high pressure homogenize equipment to add Herba Artemisiae Annuae volatile oil
β-cyclodextrin aqueous solution is homogenizing 3 ~ 5 times under 70 ~ 90 ℃, the condition of pressure 10 ~ 20MPa in temperature, each 5 ~ 7min.
Beneficial effect of the present invention is: the method effectively suppresses the volatilization of Herba Artemisiae Annuae volatile oil, extends the holding time of Herba Artemisiae Annuae volatile oil, and lasting is lasting, and utilizes ultrasound wave to prepare Herba Artemisiae Annuae volatile oil microcapsule, easy and simple to handle, quick, feasible.
Below in conjunction with the specific embodiment, further illustrate the present invention, but the scope of protection of present invention is not limited to following embodiment.
the specific embodiment:
Embodiment 1:
By wall material
β-cyclodextrin joins in the hot water of 90 ℃ and is prepared into
βthe mass ratio of-cyclodextrin and water is the solution of 15g/100g, stirs, standby until completely dissolved; Get core Herba Artemisiae Annuae volatile oil, determine
β-cyclodextrin and core Herba Artemisiae Annuae volatile oil mass ratio 15g/g, join core Herba Artemisiae Annuae volatile oil in above-mentioned solution while stirring, adopts high pressure homogenize equipment to add Herba Artemisiae Annuae volatile oil
β-cyclodextrin aqueous solution homogenizing 3 times under the condition of 90 ℃ of temperature, pressure 20MPa, each 5min, obtains emulsion; The emulsion obtaining is put in ultrasonic device, controls ultrasonic power 100W, 80 ℃ of ultrasonic temperature, model of action and be ultrasonic 60min under the condition of powerful cavitation 3s buffering 2s; By the emulsion after ultrasonic, under 0 ℃ of condition, after cold preservation 24h, in vacuum, be under 0.10MPa and 25 ℃ of conditions of temperature, to adopt Medium speed filter paper to filter, obtain filter cake; Filter cake is dry under freezer dryer vacuum 20Pa, condenser temperature-50 ℃ condition, obtain Herba Artemisiae Annuae volatile oil microcapsule product.
The mensuration of microcapsule sample embedding rate:
(1) mensuration of microcapsule product surface oil:
Accurately take 2g microcapsule product and be placed in dry conical flask of weighing, divide the petroleum ether concussion that adds 50ml for 3 times, each evenly vibration, filtration, merging filtrate, Rotary Evaporators rotation is concentrated, draws the quality of product surface oil with weight reduction.
(2) mensuration of the total oil of microcapsule product:
With petroleum ether, make solvent, accurately take microcapsule product 2g, with Soxhlet extraction process, measure its total oil content.
(3) calculating of embedding rate
Embedding rate=(quality of quality/microcapsule product total volatile oil of 1-microcapsule product surface volatile oil) * 100%
Herba Artemisiae Annuae volatile oil microcapsule product prepared by above-mentioned technique carries out the mensuration of embedding rate, and result is 76.88%.
Embodiment 2:
By wall material
β-cyclodextrin joins in the hot water of 80 ℃ and is prepared into
βthe mass ratio of-cyclodextrin and water is the solution of 10g/100g, stirs, standby until completely dissolved; Get core Herba Artemisiae Annuae volatile oil, determine
β-cyclodextrin and core Herba Artemisiae Annuae volatile oil mass ratio 10g/g, join core Herba Artemisiae Annuae volatile oil in above-mentioned solution while stirring, adopts high pressure homogenize equipment to add Herba Artemisiae Annuae volatile oil
β-cyclodextrin aqueous solution homogenizing 5 times under the condition of 80 ℃ of temperature, pressure 15MPa, each 7min, obtains emulsion; The emulsion obtaining is put in ultrasonic device, controls ultrasonic power 75W, ultrasonic temperature 70 C, model of action and be ultrasonic 50min under the condition of powerful cavitation 3s buffering 2s; By the emulsion after ultrasonic, under 2 ℃ of conditions, after cold preservation 24h, in vacuum, be under 0.08MPa and 20 ℃ of conditions of temperature, to adopt Medium speed filter paper to filter, obtain filter cake; Filter cake is dry under freezer dryer vacuum 15Pa, condenser temperature-45 ℃ condition, obtain Herba Artemisiae Annuae volatile oil microcapsule product, embedding rate is 77.24%.
Embodiment 3:
By wall material
β-cyclodextrin joins in the hot water of 60 ℃ and is prepared into
βthe mass ratio of-cyclodextrin and water is the solution of 6g/100g, stirs, standby until completely dissolved; Get core Herba Artemisiae Annuae volatile oil, determine
β-cyclodextrin and core Herba Artemisiae Annuae volatile oil mass ratio 8g/g, join core Herba Artemisiae Annuae volatile oil in above-mentioned solution while stirring, adopts high pressure homogenize equipment to add Herba Artemisiae Annuae volatile oil
β-cyclodextrin aqueous solution homogenizing 4 times under the condition of temperature 70 C, pressure 10MPa, each 6min, obtains emulsion; The emulsion obtaining is put in ultrasonic device, controls ultrasonic power 50W, ultrasonic temperature 60 C, model of action and be ultrasonic 40min under the condition of powerful cavitation 3s buffering 2s; By the emulsion after ultrasonic, under 5 ℃ of conditions, after cold preservation 24h, in vacuum, be under 0.06MPa and 15 ℃ of conditions of temperature, to adopt Medium speed filter paper to filter, obtain filter cake; Filter cake is dry under freezer dryer vacuum 10Pa, condenser temperature-40 ℃ condition, obtain Herba Artemisiae Annuae volatile oil microcapsule product, embedding rate is 75.19%.
Claims (2)
1. a method of preparing Herba Artemisiae Annuae volatile oil microcapsule, is characterized in that, comprises the following steps:
A. by wall material
β-cyclodextrin joins in the hot water of 60 ~ 90 ℃ and is prepared into
βthe mass ratio of-cyclodextrin and water is the solution of 6g/100g ~ 15g/100g, stirs, standby until completely dissolved;
B. get core Herba Artemisiae Annuae volatile oil, determine
β-cyclodextrin and core Herba Artemisiae Annuae volatile oil mass ratio 8g/g ~ 15g/g, join core Herba Artemisiae Annuae volatile oil in above-mentioned solution while stirring, and Herba Artemisiae Annuae volatile oil is uniformly dispersed, and homogenizing obtains emulsion;
C. the emulsion obtaining is put in ultrasonic device, control ultrasonic power is that 50 ~ 100W, ultrasonic temperature are 60 ~ 80 ℃, and model of action is powerful cavitation 3s buffering 2s, and be 40 ~ 60min action time;
D. by the emulsion after ultrasonic, under 0 ~ 5 ℃ of condition, after cold preservation 24h, in vacuum, be under 0.06 ~ 0.10MPa and 10 ~ 25 ℃ of conditions of temperature, to adopt Medium speed filter paper to filter, obtain filter cake;
E. filter cake is dry under freezer dryer vacuum 10 ~ 20Pa, condenser temperature-40 ℃ ~-50 ℃ of conditions, obtain Herba Artemisiae Annuae volatile oil microcapsule product, embedding rate is greater than 75%.
2. a kind of method of preparing Herba Artemisiae Annuae volatile oil microcapsule according to claim 1, is characterized in that, the homogenizing described in step b is to adopt high pressure homogenize equipment to add Herba Artemisiae Annuae volatile oil
β-cyclodextrin aqueous solution is homogenizing 3 ~ 5 times under 70 ~ 90 ℃, the condition of pressure 10 ~ 20MPa in temperature, each 5 ~ 7min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410445649.4A CN104189046A (en) | 2014-09-04 | 2014-09-04 | Method for preparing artemisia volatile oil microcapsule |
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| CN201410445649.4A CN104189046A (en) | 2014-09-04 | 2014-09-04 | Method for preparing artemisia volatile oil microcapsule |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106036901A (en) * | 2016-06-06 | 2016-10-26 | 福建省武平县英源食用菌有限公司 | Method for improving quality of aqueous extracts of shiitake mushrooms and increasing drying speed of aqueous extracts of shiitake mushrooms on basis of vacuum freezing |
| CN112694953A (en) * | 2020-12-28 | 2021-04-23 | 张家港威胜生物医药有限公司 | Sweet wormwood soap and preparation method thereof |
| CN114028270A (en) * | 2021-11-22 | 2022-02-11 | 中华全国供销合作总社南京野生植物综合利用研究所 | Artemisia apiacea essential oil-dioscorea opposita polysaccharide microcapsule and application thereof in oral care field |
-
2014
- 2014-09-04 CN CN201410445649.4A patent/CN104189046A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106036901A (en) * | 2016-06-06 | 2016-10-26 | 福建省武平县英源食用菌有限公司 | Method for improving quality of aqueous extracts of shiitake mushrooms and increasing drying speed of aqueous extracts of shiitake mushrooms on basis of vacuum freezing |
| CN112694953A (en) * | 2020-12-28 | 2021-04-23 | 张家港威胜生物医药有限公司 | Sweet wormwood soap and preparation method thereof |
| CN114028270A (en) * | 2021-11-22 | 2022-02-11 | 中华全国供销合作总社南京野生植物综合利用研究所 | Artemisia apiacea essential oil-dioscorea opposita polysaccharide microcapsule and application thereof in oral care field |
| CN114028270B (en) * | 2021-11-22 | 2024-01-30 | 中华全国供销合作总社南京野生植物综合利用研究所 | Sweet wormwood essential oil-rhizoma dioscoreae polysaccharide microcapsule and application thereof in field of oral care |
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Application publication date: 20141210 |