CN107854516A - A kind of preparation technology of the peppermint oil with slow release - Google Patents
A kind of preparation technology of the peppermint oil with slow release Download PDFInfo
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- C12P19/18—Preparation of compounds containing saccharide radicals produced by the action of a glycosyl transferase, e.g. alpha-, beta- or gamma-cyclodextrins
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Abstract
The invention discloses a kind of preparation technology of the peppermint oil with slow release, it is related to peppermint oil processing technique field, including cyclodextrin is uniformly admixed together with Semen Castaneae starch, then handled by low-temp low-pressure, obtain modified cyclodextrin and Semen Castaneae starch mixture, modified cyclodextrin and Semen Castaneae starch mixture are added in solvent, the solution or suspension that mass concentration is 40 45% is made, then peppermint oil is added, after being stirred, using ultrasonication, after then stirring 30min, carry out rotary evaporation and dry removing solvent, produce;The present invention is effectively combined after being handled by beta cyclodextrin with Semen Castaneae starch mixture under low-temp low-pressure with peppermint oil, can play a part of good carrier, it is suppressed that the volatilization of peppermint oil.
Description
Technical field
The invention belongs to peppermint oil biological processing technical field, and in particular to a kind of preparation of the peppermint oil with slow release
Technique.
Background technology
Peppermint oil volatile oil as made from peppermint stem and leaf through steam distillation, the de- brain processing in part, not only has stronger
Pharmacological action such as refresh oneself, be antibacterial, wind-dispelling, and there is pleasant fragrance, in medicine, health, food, beverage, dailyization
It is respectively provided with and is widely applied in the fields such as work, the year volume of production and marketing in China is huge, but peppermint oil highly volatile loses, and several in water
Insoluble, dispersiveness is poor, many inconvenience is brought to biological medicine industrial production, the quality of finished product is also not sufficiently stable, caused
Further exploitation is limited to.
Cyclodextrin (Cyclodextrin, abbreviation CD) is amylose in the cyclodextrin glucose base as caused by bacillus
A series of general name of the cyclic oligosaccharides generated under transfer enzyme effect, usually contains 6 ~ 12 D- glucopyranose units.Wherein
Study more and have important practical usage is the molecule containing 6,7,8 glucose units, be referred to as alpha
-, beta-and gama-cyclodextrin.According to the result of X- lines crystal diffraction, infrared spectrum and spectral analysis of the nuclear magnetic resonance, it is determined that
Each D (+)-glucopyranose for forming cyclodextrin molecular is chair conformation.Each glucose unit is bonded with Isosorbide-5-Nitrae-glucosides
Synthesize ring.Because the glycosidic bond for connecting glucose unit can not rotate freely, cyclodextrin is not cylindric molecule but slightly in cone
The annulus of shape.
Cyclodextrin can effectively increase some solubility and dissolution velocity of water-soluble bad medicine in water, be made with it
For carrier, application is relatively broad, although using carrier of the cyclodextrin as peppermint oil, can solve peppermint oil to a certain extent
Volatility problem, still, the amount that simple cyclodextrin carries peppermint oil is relatively fewer, and release is not easy.
The content of the invention
The purpose of the present invention is to be directed to the problem of existing, there is provided a kind of preparation technology of the peppermint oil with slow release.
The present invention is achieved by the following technical solutions:
A kind of preparation technology of the peppermint oil with slow release, is made peppermint oil micro mist, using peppermint oil micro mist as base by peppermint oil
Plinth formula carries out biological medicine application, and the peppermint oil micro mist preparation method is:Cyclodextrin and Semen Castaneae starch are pressed into 7-10:1 matter
It is admixed together to measure ratio uniform, is then handled by low-temp low-pressure, the low temperature is subzero 2 DEG C, and the low pressure is 0.12-
0.14MPa, modified cyclodextrin and Semen Castaneae starch mixture are obtained, modified cyclodextrin and Semen Castaneae starch mixture are added to solvent
In, solution or suspension that mass concentration is 40-45% is made, peppermint oil is then added, after being stirred, using ultrasonic wave
3-5min is handled, after then stirring 30min under 3000r/min rotating speeds, rotary evaporation is carried out and dries removing solvent, produce.
Further, the cyclodextrin is beta-schardinger dextrin, and the preparation method of the beta cyclodextrin is:
(1)After cornstarch is uniformly mixed with water, the cornstarch slurries that mass fraction is 15% are configured to, then by corn
The pH value of farinaceous size is adjusted to 5.5, and 15min is incubated at 30 DEG C, then adds its quality into cornstarch slurries again
0.12% alpha-amylase is heated to 40 DEG C, is incubated 2 hours, then carries out enzyme deactivation, obtains enzymolysis slurry;
(2)Will(1)Gained enzymolysis slurry stirs 30min under 500r/min rotating speeds, then adds debranching enzyme and CGT enzymes thereto,
Debranching enzyme and CGT the enzyme mass ratio is 1:2, the debranching enzyme quality is enzymolysis slurry quality 0.05%, is handled at 42 DEG C
40min, the hexamethylene of enzymolysis slurry quality 50% is added, after 2 hours are sufficiently stirred under 150r/min rotating speeds, is distilled back
Receive hexamethylene, obtain secondary enzymolysis slurries, by the secondary enzymolysis slurries of gained carried out in a manner of primary crystallization crystallisation by cooling and from
The heart separates solid content, and solid content is produced into beta-schardinger dextrin after pure water elutes impurity elimination.
Further, it is described after cyclodextrin is uniformly to be mixed to Semen Castaneae starch for low-temp low-pressure processing, it is added to close
Close in container, the air being passed through in nitrogen exclusion closed container, temperature is reduced to subzero 2 DEG C, then with 0.12-0.14MPa's
Pressure carries out processing 8min, then takes out to be put into 60 DEG C of baking ovens and handles 15min, then naturally cools to room temperature, produces.
Further, the solvent is that ethanol presses 1 with glycerine:2 mass ratios mix.
Further, the ultrasonic power is 500W, frequency 30kHz.
The present invention has advantages below compared with prior art:The present invention is by the way that beta-schardinger dextrin and Semen Castaneae starch mixture are existed
After being handled under low-temp low-pressure, change takes place in particle shape, and beta-schardinger dextrin is with Semen Castaneae starch grain edges lines by smooth change
For irregular shape, there is blister convex, and with the extension of time, the amplitude of change with Semen Castaneae starch particle surface in beta-schardinger dextrin
It is increasing, when treated between reach 8min after, 95% or so particle surface of beta-schardinger dextrin and Semen Castaneae starch mixing quality occurs
Hole and projection, then beta-schardinger dextrin and Semen Castaneae starch mixture are added in solvent again, peppermint oil is added, by stirring
Mix, ultrasonication so that the peppermint oil of addition is quickly adsorbed by beta-schardinger dextrin and Semen Castaneae starch particle, due to β-ring paste
Essence is that surface has hole projection state with Semen Castaneae starch particle 95%, peppermint oil can be significantly adsorbed, then by remaining
5% or so beta-schardinger dextrin and Semen Castaneae starch particle be normal state, can play a part of filling and close so that peppermint oil β-
Cyclodextrin in Semen Castaneae starch mixture with can effectively lock, when in use, due to beta-schardinger dextrin and Semen Castaneae starch just
Normality particle is easier to be decomposed, and so as to open hole sealing, contacts sealing process so that peppermint oil can be released preferably
Put, peppermint oil can be prepared more easily peppermint oil micro mist by the present invention so that it can preferably be applied to biological medicine side
Face product, solubility is significantly improved in water, while dispersiveness is more preferable, is brought greatly to biological medicine industrial production
Facility, the quality stability of finished product is also significantly improved.
Embodiment
Embodiment 1
A kind of preparation technology of the peppermint oil with slow release, is made peppermint oil micro mist, using peppermint oil micro mist as base by peppermint oil
Plinth formula carries out biological medicine application, and the peppermint oil micro mist preparation method is:Cyclodextrin and Semen Castaneae starch are pressed 7:1 mass ratio
Example is uniformly admixed together, is then handled by low-temp low-pressure, and the low temperature is subzero 2 DEG C, and the low pressure is 0.12MPa, is obtained
To modified cyclodextrin and Semen Castaneae starch mixture, modified cyclodextrin and Semen Castaneae starch mixture are added in solvent, matter is made
The solution or suspension that concentration is 40% are measured, then adds peppermint oil, after being stirred, using ultrasonication 3min, then
After stirring 30min under 3000r/min rotating speeds, carry out rotary evaporation and dry removing solvent, produce.
Further, the cyclodextrin is beta-schardinger dextrin, and the preparation method of the beta cyclodextrin is:
(1)After cornstarch is uniformly mixed with water, the cornstarch slurries that mass fraction is 15% are configured to, then by corn
The pH value of farinaceous size is adjusted to 5.5, and 15min is incubated at 30 DEG C, then adds its quality into cornstarch slurries again
0.12% alpha-amylase is heated to 40 DEG C, is incubated 2 hours, then carries out enzyme deactivation, obtains enzymolysis slurry;
(2)Will(1)Gained enzymolysis slurry stirs 30min under 500r/min rotating speeds, then adds debranching enzyme and CGT enzymes thereto,
Debranching enzyme and CGT the enzyme mass ratio is 1:2, the debranching enzyme quality is enzymolysis slurry quality 0.05%, is handled at 42 DEG C
40min, the hexamethylene of enzymolysis slurry quality 50% is added, after 2 hours are sufficiently stirred under 150r/min rotating speeds, is distilled back
Receive hexamethylene, obtain secondary enzymolysis slurries, by the secondary enzymolysis slurries of gained carried out in a manner of primary crystallization crystallisation by cooling and from
The heart separates solid content, and solid content is produced into beta-schardinger dextrin after pure water elutes impurity elimination.
Further, it is described after cyclodextrin is uniformly to be mixed to Semen Castaneae starch for low-temp low-pressure processing, it is added to close
Close in container, the air being passed through in nitrogen exclusion closed container, temperature is reduced to subzero 2 DEG C, then enter with 0.12MPa pressure
Row processing 8min, then takes out to be put into 60 DEG C of baking ovens and handles 15min, then naturally cool to room temperature, produce.
Further, the solvent is that ethanol presses 1 with glycerine:2 mass ratios mix.
Further, the ultrasonic power is 500W, frequency 30kHz.
Embodiment 2
A kind of preparation technology of the peppermint oil with slow release, is made peppermint oil micro mist, using peppermint oil micro mist as base by peppermint oil
Plinth formula carries out biological medicine application, and the peppermint oil micro mist preparation method is:Cyclodextrin and Semen Castaneae starch are pressed 10:1 mass
Ratio uniform is admixed together, is then handled by low-temp low-pressure, and the low temperature is subzero 2 DEG C, and the low pressure is 0.14MPa,
Modified cyclodextrin and Semen Castaneae starch mixture are obtained, modified cyclodextrin and Semen Castaneae starch mixture are added in solvent, are made
Mass concentration is 45% solution or suspension, then adds peppermint oil, after being stirred, using ultrasonication 5min, so
After stirring 30min under 3000r/min rotating speeds afterwards, carry out rotary evaporation and dry removing solvent, produce.
Further, the cyclodextrin is beta-schardinger dextrin, and the preparation method of the beta cyclodextrin is:
(1)After cornstarch is uniformly mixed with water, the cornstarch slurries that mass fraction is 15% are configured to, then by corn
The pH value of farinaceous size is adjusted to 5.5, and 15min is incubated at 30 DEG C, then adds its quality into cornstarch slurries again
0.12% alpha-amylase is heated to 40 DEG C, is incubated 2 hours, then carries out enzyme deactivation, obtains enzymolysis slurry;
(2)Will(1)Gained enzymolysis slurry stirs 30min under 500r/min rotating speeds, then adds debranching enzyme and CGT enzymes thereto,
Debranching enzyme and CGT the enzyme mass ratio is 1:2, the debranching enzyme quality is enzymolysis slurry quality 0.05%, is handled at 42 DEG C
40min, the hexamethylene of enzymolysis slurry quality 50% is added, after 2 hours are sufficiently stirred under 150r/min rotating speeds, is distilled back
Receive hexamethylene, obtain secondary enzymolysis slurries, by the secondary enzymolysis slurries of gained carried out in a manner of primary crystallization crystallisation by cooling and from
The heart separates solid content, and solid content is produced into beta-schardinger dextrin after pure water elutes impurity elimination.
Further, it is described after cyclodextrin is uniformly to be mixed to Semen Castaneae starch for low-temp low-pressure processing, it is added to close
Close in container, the air being passed through in nitrogen exclusion closed container, temperature is reduced to subzero 2 DEG C, then enter with 0.14MPa pressure
Row processing 8min, then takes out to be put into 60 DEG C of baking ovens and handles 15min, then naturally cool to room temperature, produce.
Further, the solvent is that ethanol presses 1 with glycerine:2 mass ratios mix.
Further, the ultrasonic power is 500W, frequency 30kHz.
Embodiment 3
A kind of preparation technology of the peppermint oil with slow release, is made peppermint oil micro mist, using peppermint oil micro mist as base by peppermint oil
Plinth formula carries out biological medicine application, and the peppermint oil micro mist preparation method is:Cyclodextrin and Semen Castaneae starch are pressed 8:1 mass ratio
Example is uniformly admixed together, is then handled by low-temp low-pressure, and the low temperature is subzero 2 DEG C, and the low pressure is 0.13MPa, is obtained
To modified cyclodextrin and Semen Castaneae starch mixture, modified cyclodextrin and Semen Castaneae starch mixture are added in solvent, matter is made
The solution or suspension that concentration is 42% are measured, then adds peppermint oil, after being stirred, using ultrasonication 4min, then
After stirring 30min under 3000r/min rotating speeds, carry out rotary evaporation and dry removing solvent, produce.
Further, the cyclodextrin is beta-schardinger dextrin, and the preparation method of the beta cyclodextrin is:
(1)After cornstarch is uniformly mixed with water, the cornstarch slurries that mass fraction is 15% are configured to, then by corn
The pH value of farinaceous size is adjusted to 5.5, and 15min is incubated at 30 DEG C, then adds its quality into cornstarch slurries again
0.12% alpha-amylase is heated to 40 DEG C, is incubated 2 hours, then carries out enzyme deactivation, obtains enzymolysis slurry;
(2)Will(1)Gained enzymolysis slurry stirs 30min under 500r/min rotating speeds, then adds debranching enzyme and CGT enzymes thereto,
Debranching enzyme and CGT the enzyme mass ratio is 1:2, the debranching enzyme quality is enzymolysis slurry quality 0.05%, is handled at 42 DEG C
40min, the hexamethylene of enzymolysis slurry quality 50% is added, after 2 hours are sufficiently stirred under 150r/min rotating speeds, is distilled back
Receive hexamethylene, obtain secondary enzymolysis slurries, by the secondary enzymolysis slurries of gained carried out in a manner of primary crystallization crystallisation by cooling and from
The heart separates solid content, and solid content is produced into beta-schardinger dextrin after pure water elutes impurity elimination.
Further, it is described after cyclodextrin is uniformly to be mixed to Semen Castaneae starch for low-temp low-pressure processing, it is added to close
Close in container, the air being passed through in nitrogen exclusion closed container, temperature is reduced to subzero 2 DEG C, then enter with 0.13MPa pressure
Row processing 8min, then takes out to be put into 60 DEG C of baking ovens and handles 15min, then naturally cool to room temperature, produce.
Further, the solvent is that ethanol presses 1 with glycerine:2 mass ratios mix.
Further, the ultrasonic power is 500W, frequency 30kHz.
Comparative example 1:Differed only in embodiment 1 and do not add cyclodextrin.
Comparative example 2:Differed only in embodiment 1 and do not add Semen Castaneae starch.
Comparative example 3:Cyclodextrin is differed only in embodiment 1 to handle without low-temp low-pressure with Semen Castaneae starch.
Experiment:
Yinchai Granules are made by identical proportioning in the peppermint oil of untreated peppermint oil, embodiment and comparative example method processing
Agent, detected according to WS3-B-2612-97 standards, its result is as follows;(It is with batch peppermint of peppermint extraction to test peppermint oil
Oil);
Table 1
Holding time(Month) | 6 | 12 | 18 | 24 | 36 | 42 |
Embodiment 1 | Differentiate obvious | Differentiate obvious | Differentiate obvious | Differentiate obvious | Differentiate obvious | Differentiate obvious |
Embodiment 2 | Differentiate obvious | Differentiate obvious | Differentiate obvious | Differentiate obvious | Differentiate obvious | Differentiate obvious |
Embodiment 3 | Differentiate obvious | Differentiate obvious | Differentiate obvious | Differentiate obvious | Differentiate obvious | Differentiate obvious |
Comparative example 1 | Differentiate obvious | Differentiate obvious | Differentiate weak aobvious | Differentiate weak aobvious | Differentiate weak aobvious | Differentiate nothing |
Comparative example 2 | Differentiate obvious | Differentiate obvious | Differentiate weak aobvious | Differentiate weak aobvious | Differentiate nothing | Differentiate nothing |
Comparative example 3 | Differentiate obvious | Differentiate obvious | Differentiate weak aobvious | Differentiate nothing | Differentiate nothing | Differentiate nothing |
Control group | Differentiate obvious | Differentiate obvious | Differentiate nothing | Differentiate nothing | Differentiate nothing | Differentiate nothing |
As can be seen from Table 1, the peppermint oil micro mist for preparing of present invention quality before the deadline and curative effect have obtained sufficient guarantor
Card.
Claims (5)
1. a kind of preparation technology of the peppermint oil with slow release, it is characterised in that peppermint oil micro mist is made in peppermint oil, with thin
Formula carries out biological medicine application based on lotus oil micro mist, and the peppermint oil micro mist preparation method is:Cyclodextrin and chestnut are formed sediment
Powder presses 7-10:1 mass ratio is uniformly admixed together, is then handled by low-temp low-pressure, and the low temperature is subzero 2 DEG C, described
Low pressure is 0.12-0.14MPa, obtains modified cyclodextrin and Semen Castaneae starch mixture, and modified cyclodextrin is mixed with Semen Castaneae starch
Thing is added in solvent, and solution or suspension that mass concentration is 40-45% is made, then adds peppermint oil, is stirred
Afterwards, using ultrasonication 3-5min, after then stirring 30min under 3000r/min rotating speeds, carry out rotary evaporation and dry removing
Solvent, produce.
A kind of 2. preparation technology of the peppermint oil with slow release as claimed in claim 1, it is characterised in that the cyclodextrin
For beta-schardinger dextrin, the preparation method of the beta cyclodextrin is:
(1)After cornstarch is uniformly mixed with water, the cornstarch slurries that mass fraction is 15% are configured to, then by corn
The pH value of farinaceous size is adjusted to 5.5, and 15min is incubated at 30 DEG C, then adds its quality into cornstarch slurries again
0.12% alpha-amylase is heated to 40 DEG C, is incubated 2 hours, then carries out enzyme deactivation, obtains enzymolysis slurry;
(2)Will(1)Gained enzymolysis slurry stirs 30min under 500r/min rotating speeds, then adds debranching enzyme and CGT enzymes thereto,
Debranching enzyme and CGT the enzyme mass ratio is 1:2, the debranching enzyme quality is enzymolysis slurry quality 0.05%, is handled at 42 DEG C
40min, the hexamethylene of enzymolysis slurry quality 50% is added, after 2 hours are sufficiently stirred under 150r/min rotating speeds, is distilled back
Receive hexamethylene, obtain secondary enzymolysis slurries, by the secondary enzymolysis slurries of gained carried out in a manner of primary crystallization crystallisation by cooling and from
The heart separates solid content, and solid content is produced into beta-schardinger dextrin after pure water elutes impurity elimination.
3. a kind of preparation technology of the peppermint oil with slow release as claimed in claim 1, it is characterised in that described through too low
After cyclodextrin is uniformly to be mixed to Semen Castaneae starch for warm low pressure processing, it is added in closed container, is passed through nitrogen and excludes closed appearance
Air in device, temperature is reduced to subzero 2 DEG C, then processing 8min is carried out with 0.12-0.14MPa pressure, then taken out and put
Enter in 60 DEG C of baking ovens and handle 15min, then naturally cool to room temperature, produce.
4. a kind of preparation technology of the peppermint oil with slow release as claimed in claim 1, it is characterised in that the solvent is
Ethanol presses 1 with glycerine:2 mass ratios mix.
A kind of 5. preparation technology of the peppermint oil with slow release as claimed in claim 1, it is characterised in that the ultrasonic wave
Power is 500W, frequency 30kHz.
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CN113088408A (en) * | 2021-04-07 | 2021-07-09 | 四川兴望源商贸有限公司 | Automobile glass water for cleaning and preparation method thereof |
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