CN102559383B - Preparation method of elsholtzia volatile oil microcapsule - Google Patents
Preparation method of elsholtzia volatile oil microcapsule Download PDFInfo
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- CN102559383B CN102559383B CN 201110393870 CN201110393870A CN102559383B CN 102559383 B CN102559383 B CN 102559383B CN 201110393870 CN201110393870 CN 201110393870 CN 201110393870 A CN201110393870 A CN 201110393870A CN 102559383 B CN102559383 B CN 102559383B
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- cyclodextrin
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- herba moslae
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Abstract
The invention discloses a preparation method of an elsholtzia volatile oil microcapsule, belonging to the field of food spice processing. The preparation method is characterized in that the method comprises the steps of: firstly, taking beta-cyclodextrin as a wall material, adding the beta-cyclodextrin into hot water to prepare beta-cyclodextrin water solution, stirring for standby application until the beta-cyclodextrin is completely dissolved; secondly, during the stirring, adding a core material-elsholtzia volatile oil into the water solution, and homogenizing to obtain emulsion; afterwards, placing the emulsion into ultrasonic equipment for ultrasonic treatment; and finally, carrying out refrigerating, leaching and freeze-drying to obtain an elsholtzia volatile oil microcapsule product. The elsholtzia volatile oil microcapsule prepared in the invention is solid powder; through the method, the elsholtzia volatile oil can be isolated from the outside air, so that the volatization of the elsholtzia volatile oil can avoided and the storage time of the elsholtzia volatile oil can be effectively prolonged; and the operation is simple, convenient, rapid and practicable.
Description
Technical field
The invention belongs to food spice manufacture field, relate to a kind of preparation method of Herba Moslae volatile oil microcapsule.
Background technology
Elscholtiza (Herba Moslae) is the dry aerial parts of labiate Mosla chinensis Maxim. (Moslachinensis Maxim) or HERBA ELSHOLTZIAE (Mosla chinensis Maxim.cv Jiangxiangru).The former practises title " Chinese mosla ", and the latter practises title " HERBA ELSHOLTZIAE ".Elscholtiza is conventional Chinese medicine, has the effect of relieving the exterior syndrome by diaphoresis and middle dampness elimination.The clinical summer-heat damp cold that is usually used in, fever with aversion to cold, it is lossless to have a headache, and stomachache is vomited and diarrhoea, diseases such as dysuria.Recent research result shows that its effective constituent mainly is volatile oil, and that its volatile oil has is analgesic, analgesia, sedative effect, immuno-potentiation, anti-microbial effect and antivirus action.
Microcapsulary refers to utilize natural or synthesized polymer material, and with dispersed solids, liquid, or even gaseous matter wraps up, and forms the technology of the fine particle with semipermeability or sealing cyst membrane.The process of parcel is micro encapsulation, and the fine particle of formation is called microcapsule.Can realize many purposes behind the micro encapsulation: the physical properties (color, outward appearance, apparent density, solvability) of improving enveloped matter, make material avoid the influence of environment, improve Stability of Substance, shielding taste and smell, reduce material toxicity, inconsistent material is isolated, control the release of material as required, etc.
Herba Moslae volatile oil is in storage process, and some volatile component can change, and particularly when temperature was high, its harmful variation was more obvious.Therefore in order to expand its range of application, avoid loss of effective components, adopt microcapsulary that volatile oil is become pressed powder by liquid state, keep its fragrance ingredient greatly, thereby enlarge it in the range of application of foodstuffs industry.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of Herba Moslae volatile oil microcapsule, i.e. a kind of method of utilizing ultrasonic wave to prepare the Herba Moslae volatile oil microcapsule.
For achieving the above object, the present invention adopts following technical scheme: at first be the wall material with the beta-cyclodextrin, it is joined the mass ratio that is prepared into beta-cyclodextrin and water in 65 ℃～85 ℃ the hot water is the solution of 8g/100g～12g/100g, stirs that to treat to dissolve fully the back standby; Next mass ratio of controlling beta-cyclodextrin and core-Herba Moslae volatile oil is 8g/100g～12g/100g, after while stirring Herba Moslae volatile oil being joined above-mentioned solution, adopting the beta-cyclodextrin aqueous solution that high-pressure homogeneous equipment will add Herba Moslae volatile oil is that 60 ℃～90 ℃, pressure are homogeneous 2～3 times under the condition of 15MPa～25MPa in temperature, each homogeneous 3min～5min gets emulsion; Then this emulsion is put into ultrasonic device, ultrasonic 60min～90min under the condition of control ultrasonic power 50W～100W, 50 ℃～70 ℃ of ultrasonic temperature and dutycycle 5s/5s; Subsequently the emulsion after ultrasonic being put into temperature is that 0 ℃～4 ℃ refrigerator and cooled are hidden 24h, and the refrigeration liquid after the refrigeration is adopted the middling speed filter paper filtering under vacuum tightness 0.08MPa～0.10MPa and 5 ℃～35 ℃ conditions of temperature, gets filter cake; At last with filter cake freeze drier vacuum tightness less than 20Pa, condenser temperature-45 ℃～-60 ℃ conditions under drying totally, get the Herba Moslae volatile oil microcapsule product.The microcapsule embedded rate of Herba Moslae volatile oil is greater than 70%.
Owing to adopted above technical scheme, the present invention has the following advantages:
1, the prepared Herba Moslae volatile oil microcapsule of the present invention are a kind of pressed powders, and this method can separate the air of Herba Moslae volatile oil with the external world, has avoided the volatilization of Herba Moslae volatile oil, can prolong the shelf time of Herba Moslae volatile oil effectively;
2, the present invention utilizes ultrasonic wave to prepare the Herba Moslae volatile oil microcapsule, and is easy and simple to handle, quick, feasible.
Embodiment
Embodiment 1:
At first be the wall material with the beta-cyclodextrin, it is joined the mass ratio that is prepared into beta-cyclodextrin and water in 80 ℃ the hot water is the solution of 9g/100g, stirs that to treat to dissolve fully the back standby; Next mass ratio of controlling beta-cyclodextrin and core-Herba Moslae volatile oil is 9g/g, after while stirring Herba Moslae volatile oil being joined above-mentioned solution, adopting the beta-cyclodextrin aqueous solution that high-pressure homogeneous equipment will add Herba Moslae volatile oil is that 70 ℃, pressure are homogeneous 3 times under the condition of 18MPa in temperature, each homogeneous 3min gets emulsion; Then this emulsion is put into ultrasonic device, ultrasonic 60min under the condition of control ultrasonic power 100W, 50 ℃ of ultrasonic temperature and dutycycle 5s/5s; Subsequently the emulsion after ultrasonic being put into temperature is that 1 ℃ of refrigerator and cooled is hidden 24h, and the refrigeration liquid after the refrigeration is adopted the middling speed filter paper filtering under vacuum tightness 0.08MPa and 28 ℃ of conditions of temperature, gets filter cake; At last with filter cake freeze drier vacuum tightness less than 20Pa, condenser temperature-55 ℃ condition under drying totally, get the Herba Moslae volatile oil microcapsule product.
The mensuration of microcapsule sample embedding rate:
(1) mensuration of microcapsule product surface volatile oil:
Accurately take by weighing the 2g microcapsule product, divide 3 addings with the sherwood oil of 50ml, each evenly vibration, filter, merging filtrate concentrates with the Rotary Evaporators rotation, draws the quality of product surface volatile oil with the loss of weight method.
(2) mensuration of the total oil of microcapsule product:
Make solvent with sherwood oil, accurately take by weighing microcapsule product 2g, measure its total volatile oil content with the Soxhlet extraction process.
(3) calculating of embedding rate
To carry out the mensuration of embedding rate by the Herba Moslae volatile oil microcapsule product of above-mentioned prepared, the result is 75.43%.
Embodiment 2:
At first be the wall material with the beta-cyclodextrin, it is joined the mass ratio that is prepared into beta-cyclodextrin and water in 90 ℃ the hot water is the solution of 11g/100g, stirs that to treat to dissolve fully the back standby; Next mass ratio of controlling beta-cyclodextrin and core-Herba Moslae volatile oil is 11g/g, after while stirring Herba Moslae volatile oil being joined above-mentioned solution, adopting the beta-cyclodextrin aqueous solution that high-pressure homogeneous equipment will add Herba Moslae volatile oil is 85 ℃, pressure 25MPa, homogeneous 2 times under the condition of pressure 20MPa for the second time for the first time in temperature, each homogeneous 3min gets emulsion; Then this emulsion is put into ultrasonic device, ultrasonic 70min under the condition of control ultrasonic power 100W, 70 ℃ of ultrasonic temperature and dutycycle 5s/5s; Subsequently the emulsion after ultrasonic being put into temperature is that 4 ℃ of refrigerator and cooled are hidden 24h, and the refrigeration liquid after the refrigeration is adopted the middling speed filter paper filtering under vacuum tightness 0.09MPa and 25 ℃ of conditions of temperature, gets filter cake; At last with filter cake freeze drier vacuum tightness less than 20Pa, condenser temperature-50 ℃ condition under drying totally, get the Herba Moslae volatile oil microcapsule product.Its embedding rate is 78.81% after measured.
Embodiment 3:
At first be the wall material with the beta-cyclodextrin, it is joined the mass ratio that is prepared into beta-cyclodextrin and water in 85 ℃ the hot water is the solution of 8g/100g, stirs that to treat to dissolve fully the back standby; Next mass ratio of controlling beta-cyclodextrin and core-Herba Moslae volatile oil is 12g/g, after while stirring Herba Moslae volatile oil being joined above-mentioned solution, adopting the beta-cyclodextrin aqueous solution that high-pressure homogeneous equipment will add Herba Moslae volatile oil is that 70 ℃, pressure are homogeneous 2 times under the condition of 15MPa in temperature, each homogeneous 5min gets emulsion; Then this emulsion is put into ultrasonic device, ultrasonic 80min under the condition of control ultrasonic power 50W, 60 ℃ of ultrasonic temperature and dutycycle 5s/5s; Subsequently the emulsion after ultrasonic being put into temperature is that 2 ℃ of refrigerator and cooled are hidden 24h, and the refrigeration liquid after the refrigeration is adopted the middling speed filter paper filtering under vacuum tightness 0.10MPa and 30 ℃ of conditions of temperature, gets filter cake; At last with filter cake freeze drier vacuum tightness less than 20Pa, condenser temperature-45 ℃ condition under drying totally, get the Herba Moslae volatile oil microcapsule product.Its embedding rate is 72.88% after measured.
Claims (1)
1. the preparation method of Herba Moslae volatile oil microcapsule, it is characterized in that: at first be the wall material with the beta-cyclodextrin, it is joined the mass ratio that is prepared into beta-cyclodextrin and water in 65 ℃～85 ℃ the hot water is the solution of 8g/100g～12g/100g, stirs that to treat to dissolve fully the back standby; Next mass ratio of controlling beta-cyclodextrin and core one Herba Moslae volatile oil is 8g/g～12g/g, Herba Moslae volatile oil is joined above-mentioned solution after, homogeneous gets emulsion; Then this emulsion is put into ultrasonic device, ultrasonic 60min～90min under the condition of control ultrasonic power 50W～100W, 50 ℃～70 ℃ of ultrasonic temperature and dutycycle 5s/5s; Refrigeration at last, suction filtration, lyophilize get the Herba Moslae volatile oil microcapsule product; The microcapsule embedded rate of Herba Moslae volatile oil is greater than 70%;
Described homogeneous is that to adopt the beta-cyclodextrin aqueous solution that high-pressure homogeneous equipment will add Herba Moslae volatile oil be that 60 ℃～90 ℃, pressure are homogeneous 2～3 times under the condition of 15MPa～25MPa, homogeneous 3min～5min at every turn in temperature;
Described refrigeration is that the emulsion after ultrasonic is put into temperature is that 0 ℃～4 ℃ refrigerator and cooled are hidden 24h;
Described suction filtration is that the refrigeration liquid after the refrigeration is adopted the middling speed filter paper filtering under vacuum tightness 0.08MPa～0.10MPa and 5 ℃～35 ℃ conditions of temperature, gets filter cake;
Described lyophilize be with filter cake freeze drier vacuum tightness less than 20Pa, condenser temperature-45 ℃～-60 ℃ conditions under drying totally, get the Herba Moslae volatile oil microcapsule product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110393870 CN102559383B (en) | 2011-11-26 | 2011-11-26 | Preparation method of elsholtzia volatile oil microcapsule |
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| CN 201110393870 CN102559383B (en) | 2011-11-26 | 2011-11-26 | Preparation method of elsholtzia volatile oil microcapsule |
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| CN102559383A CN102559383A (en) | 2012-07-11 |
| CN102559383B true CN102559383B (en) | 2013-08-07 |
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| CN103170286A (en) * | 2013-01-30 | 2013-06-26 | 天津商业大学 | Method for preparing melissa officinalis L. essential oil and beta-cyclodextrin molecule microcapsule |
| CN114984873A (en) * | 2022-06-10 | 2022-09-02 | 云南中烟工业有限责任公司 | Preparation method of response surface method optimized aroma-enhancing component microcapsule |
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