CN108114105A - A kind of preparation method of Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon - Google Patents

A kind of preparation method of Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon Download PDF

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CN108114105A
CN108114105A CN201810149026.0A CN201810149026A CN108114105A CN 108114105 A CN108114105 A CN 108114105A CN 201810149026 A CN201810149026 A CN 201810149026A CN 108114105 A CN108114105 A CN 108114105A
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essential oil
cyclodextrin
acorus tatarinowii
cyclodextrin microballoon
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张彦
张寒
李伟泽
罗国平
唐梅
唐一梅
郑蕾
申旭霁
汪兴军
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Xian Medical University
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    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/11—Encapsulated compositions
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
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    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
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    • A61K8/738—Cyclodextrins
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    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/10—General cosmetic use
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/56—Compounds, absorbed onto or entrapped into a solid carrier, e.g. encapsulated perfumes, inclusion compounds, sustained release forms

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Abstract

A kind of preparation method of Essential Oil of Acorus tatarinowii beta cyclodextrin microballoon disclosed by the invention, first prepare beta cyclodextrin microballoon, then beta cyclodextrin microballoon is added in distilled water and is dissolved by heating into saturated solution, Essential Oil of Acorus tatarinowii is added in after cooling, ultrasonic vibration after sealing, it is filtered after cooling, with being drying to obtain after petroleum ether.The preparation method of the present invention can substantially increase Essential Oil of Acorus tatarinowii water solubility, it covers its bad stink and mitigates its irritation, make as raw material to be added in cosmetics and drug, solves the problems, such as Essential Oil of Acorus tatarinowii poorly water-soluble, there are bad odor, irritation are big, greatly improve the scope of application of Essential Oil of Acorus tatarinowii, application idea has been widened in food, medicine and cosmetic field for Essential Oil of Acorus tatarinowii, has been had important practical significance.

Description

A kind of preparation method of Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon
Technical field
The invention belongs to method for preparing microsphere technical fields, and in particular to a kind of Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon Preparation method.
Background technology
Chinese medicine grass-leaved sweetflag is the rhizome of acorus gramineus araceae plant, there is the effect of inducing resuscitation of having one's ideas straightened out, wherein containing volatility The substances such as ingredient α-asarone (α-asarona), beta-Asarone (β-asarone), methyl eugenol (methy lequens). Modern pharmacological studies have shown that Essential Oil of Acorus tatarinowii has extremely strong sedative-hypnotic effect, clinic is widely used in treatment coma epilepsy, is good for Forget dementia etc..But since Essential Oil of Acorus tatarinowii is not soluble in water, and it is irritant with mucous membrane to skin, therefore in terms of preparation process Application difficult especially prepares the solid pharmaceutical preparations such as piece agent, powder, capsule.
Cyclodextrin (cyclodextrin, CD) is a kind of tubular high-molecular compound, white, by cyclodextrin glucose base One group of ring-type caused by transferase (cyclodextrin glucosyl transferase enzyme, CGT) catalytic starch Oligomer.It is with cavity structure, and external hydrophilic, inner cavity is hydrophobic, and this structure can make insoluble drug group be embedded in its cavity In, not only improve the dispersion degree of drug, and by the hydrophily of itself, improve its solubility and water solubility, make water solubility The drug of difference is fully utilized.The structure of cyclodextrin is that 6-8 D-Glucose molecule carries out the annular chemical combination for being coupled generation Object.It is known as alpha-cyclodextrin (α-CD) by what six molecules were formed, it is beta-cyclodextrin (β-CD) to be made of seven molecules, by That eight molecules are formed is γ cyclodextrin (γ-CD).α-CD cavitys are smaller, γ-CD prices costly, lead to the most commonly used is Beta-cyclodextrin.
Polymer microsphere be at the end of the 20th century the phase start grow up Polymer Technology.The states such as America and Europe are just new by this Type technology is applied in pharmacy and cosmetics industry, and China also actively develops microballoon this pharmaceutical formulation techniques in recent years.It should Essential Oil of Acorus tatarinowii is prepared into microballoon with beta-cyclodextrin, its bad odor can be covered, reduce its irritation and toxic side effect, And its stability and bioavailability are improved, expand its application in fields such as biological medicine, food, environmental protection.
The content of the invention
The object of the present invention is to provide a kind of preparation methods of Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon, solve grass-leaved sweetflag Volatile oil indissoluble solution and has bad odor and irritating problem in hydrophilic solution.
The technical solution adopted in the present invention is a kind of preparation method of Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon, including Following steps：
Step 1, beta-cyclodextrin microballoon is prepared
Step 1.1, beta-cyclodextrin is added in sodium hydrate aqueous solution, constant temperature is stirred to being completely dissolved；
Step 1.2, epoxychloropropane is added into the solution of step 1.1, constant temperature adds in kerosene while stirring, heats up Then reaction is filtered by vacuum, cleans, drying, grinding, obtaining beta-cyclodextrin microballoon successively；
Step 2, the beta-cyclodextrin microballoon of step 1 is added in distilled water, dissolves by heating into saturated solution；
Step 3, Essential Oil of Acorus tatarinowii, ultrasonic vibration after sealing, after cooling will be added in after the saturated solution cooling in step 2 It filters, obtains filter residue, it is dry to obtain Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon to constant weight then with petroleum ether filter residue.
It is of the invention to be further characterized in that,
In step 1.1 mass concentration of sodium hydrate aqueous solution be 0.1-1.0g/mL, every milliliter of sodium hydrate aqueous solution Middle beta-cyclodextrin quality is 0.1-1.0g；
The whipping temp of constant temperature stirring is 30-40 DEG C.
Epoxychloropropane and kerosene mass ratio 3 in step 1.2:2-2:1；
Wherein kerosene is the kerosene containing emulsifier Span-80, Tween-20, wherein emulsifier Span-80 and emulsifier The mass ratio of Tween-20 is 3:1.
In step 1.2 constant temperature whipping temp be 20-60 DEG C, mixing time 1-5h, rotating speed 500-1000r/min；
Wherein the temperature of temperature reaction is 20-60 DEG C, reaction time 6-24h.
It is cleaned in step 1.2 and is specially：It is cleaned successively using dilute hydrochloric acid, absolute ethyl alcohol, distilled water, acetone；
Drying temperature is 40-60 DEG C, time 24-48h.
The volume of the corresponding distilled water of every gram of beta-cyclodextrin microspheres quality is 10-30ml in step 2；Heating temperature is 20- 60℃。
The quality of beta-cyclodextrin microballoon is 4- in the saturated solution added in step 3 in every milliliter of Essential Oil of Acorus tatarinowii 12g。
The temperature of saturated solution is 10-30 DEG C after cooling down in step 3.
The temperature of step 3 ultrasonic vibration is 20-60 DEG C, time 1-5h.
Saturated solution temperature is 2-10 DEG C after being cooled down in step 3；Drying temperature is 40-60 DEG C.
The beneficial effects of the invention are as follows：A kind of preparation method of Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon of the present invention can be apparent It is water-soluble to increase Essential Oil of Acorus tatarinowii, covers its bad stink and mitigates its irritation, make as raw material can be added to cosmetics with In drug, solve the problems, such as Essential Oil of Acorus tatarinowii poorly water-soluble, there are bad odor, irritation are big, greatly improve stone The scope of application of calamus volatile oil has been widened application idea in food, medicine and cosmetic field for Essential Oil of Acorus tatarinowii, has been had There is important realistic meaning.
Description of the drawings
Fig. 1 is the microscope scanning figure of beta-cyclodextrin；
Fig. 2 is the microscope scanning figure of beta-cyclodextrin microballoon prepared by the present invention；
Fig. 3 is the microscope scanning figure of Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon prepared by the present invention；
Fig. 4 is the infrared spectrum analysis spectrogram of beta-cyclodextrin of the present invention and beta-cyclodextrin microballoon, and wherein a represents beta-cyclodextrin Microballoon, b represent beta-cyclodextrin；
Fig. 5 is the infrared spectrum analysis spectrogram of beta-cyclodextrin microballoon of the present invention and Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon, Wherein a represents beta-cyclodextrin microballoon, and c represents Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon；
Fig. 6 is Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon and Essential Oil of Acorus tatarinowii, beta-cyclodextrin, β-ring prepared by the present invention The differential heating scan analysis of five kinds of substances of physical mixture of dextrin microballoon, Essential Oil of Acorus tatarinowii and beta-cyclodextrin measures spectrum Figure.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
A kind of preparation method of Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon of the present invention, comprises the following steps：
Step 1, beta-cyclodextrin microballoon is prepared
Step 1.1, beta-cyclodextrin is added in the sodium hydrate aqueous solution that mass concentration is 0.1-1.0g/mL, 30-40 DEG C Constant temperature is stirred to being completely dissolved, wherein beta-cyclodextrin quality is 0.1-1.0g in every milliliter of sodium hydrate aqueous solution；
Step 1.2, epoxychloropropane, 20-60 DEG C of constant temperature, rotating speed 500-1000r/ are added into the solution of step 1.1 1-5h is stirred during min while adds in kerosene, epoxychloropropane and kerosene mass ratio 3:2-2:1；It is reacted when being warming up to 20-60 DEG C Then 6-24h is filtered by vacuum, cleans, drying, grinding, obtaining beta-cyclodextrin microballoon successively；
Wherein kerosene is the kerosene containing emulsifier Span-80, Tween-20, wherein emulsifier Span-80 and emulsifier The mass ratio of Tween-20 is 3:1；
It is cleaned successively using dilute hydrochloric acid, absolute ethyl alcohol, distilled water, acetone during cleaning；Drying temperature is 40-60 DEG C, time For 24-48h.
Step 2, the beta-cyclodextrin microballoon of step 1 is added in distilled water, dissolves by heating into saturated solution；Wherein every gram of β- The volume of the corresponding distilled water of cyclodextrin microsphere quality is 10-30ml；, heating temperature is 20-60 DEG C.
Step 3, Essential Oil of Acorus tatarinowii is added in after the saturated solution in step 2 being cooled to 10-30 DEG C, in temperature after sealing Ultrasonic vibration 1-5h at 20-60 DEG C filters after being cooled to 2-10 DEG C, obtains filter residue, petroleum ether filter residue is then used, in temperature It is dried at 40-60 DEG C to constant weight and obtains Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon；
The quality of beta-cyclodextrin microballoon is 4-12g in the saturated solution added in wherein every milliliter of Essential Oil of Acorus tatarinowii.
Embodiment 1
(1) beta-cyclodextrin microballoon is prepared
6g beta-cyclodextrins are added in the 10mL sodium hydrate aqueous solutions that mass concentration is 0.4g/mL, 30 DEG C of constant temperature stirrings To being completely dissolved；Then rotating speed control to stir 1.5h at 30 DEG C for 750r/min, add in epoxychloropropane, together while stirring When add in kerosene, epoxychloropropane and kerosene mass ratio 3:2；6h is reacted when being warming up to 60 DEG C, is then filtered by vacuum successively, is clear It washes, dry, grind, obtain beta-cyclodextrin microballoon；
Wherein kerosene is the kerosene containing emulsifier Span-80, Tween-20, wherein emulsifier Span-80 and emulsifier The mass ratio of Tween-20 is 3:1；
It is cleaned successively using dilute hydrochloric acid, absolute ethyl alcohol, distilled water, acetone during cleaning；Drying temperature is 60 DEG C, the time is 24h。
(2) Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon is obtained
Beta-cyclodextrin microballoon is added in distilled water, 40 DEG C is heated to and is dissolved into saturated solution；Every gram of beta-cyclodextrin microballoon The volume of the corresponding distilled water of quality is 20ml.
Saturated solution is cooled to after 10 DEG C and adds in Essential Oil of Acorus tatarinowii, after sealing in 20 DEG C of temperature ultrasonic vibration 3h, It is filtered after being cooled to 2 DEG C, obtains filter residue, then with petroleum ether filter residue, dried in 40 DEG C of temperature to constant weight and obtain stone Calamus volatile oil beta-cyclodextrin microballoon；
The quality of beta-cyclodextrin microballoon is 4 in the saturated solution added in wherein every milliliter of Essential Oil of Acorus tatarinowii.
Embodiment 2
(1) beta-cyclodextrin microballoon is prepared
1g beta-cyclodextrins are added in the 10mL sodium hydrate aqueous solutions that mass concentration is 0.1g/mL, 35 DEG C of constant temperature stirrings To being completely dissolved；Then rotating speed control to stir 3h at 35 DEG C for 700r/min, while stirring addition epoxychloropropane, simultaneously Add in kerosene, epoxychloropropane and kerosene mass ratio 2:1；It is reacted when being warming up to 40 DEG C for 24 hours, be then filtered by vacuum, clean successively, Drying, grinding, obtain beta-cyclodextrin microballoon；
Wherein kerosene is the kerosene containing emulsifier Span-80, Tween-20, wherein emulsifier Span-80 and emulsifier The mass ratio of Tween-20 is 3:1；
It is cleaned successively using dilute hydrochloric acid, absolute ethyl alcohol, distilled water, acetone during cleaning；Drying temperature is 40 DEG C, the time is 48h。
(2) Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon is obtained
Beta-cyclodextrin microballoon is added in distilled water, 20 DEG C is heated to and is dissolved into saturated solution；Every gram of beta-cyclodextrin microballoon The volume of the corresponding distilled water of quality is 10ml.
Saturated solution is cooled to after 10 DEG C and adds in Essential Oil of Acorus tatarinowii, after sealing in 20 DEG C of temperature ultrasonic vibration 1h, It is filtered after being cooled to 2 DEG C, obtains filter residue, then with petroleum ether filter residue, dried in 40 DEG C of temperature to constant weight and obtain stone Calamus volatile oil beta-cyclodextrin microballoon；
The quality of beta-cyclodextrin microballoon is 4g in the saturated solution added in wherein every milliliter of Essential Oil of Acorus tatarinowii.
Embodiment 3
(1) beta-cyclodextrin microballoon is prepared
By 10g beta-cyclodextrins add in mass concentration be 1g/mL 10mL sodium hydrate aqueous solutions in, 40 DEG C of constant temperature stir to It is completely dissolved；Then rotating speed control to stir 1.5h at 40 DEG C for 800r/min, while stirring addition epoxychloropropane, simultaneously Add in kerosene, epoxychloropropane and kerosene mass ratio 3:2；Heating 50 DEG C when react 20h, then successively be filtered by vacuum, clean, dry Dry, grinding, obtains beta-cyclodextrin microballoon；
Wherein kerosene is the kerosene containing emulsifier Span-80, Tween-20, wherein emulsifier Span-80 and emulsifier The mass ratio of Tween-20 is 3:1；
It is cleaned successively using dilute hydrochloric acid, absolute ethyl alcohol, distilled water, acetone during cleaning；Drying temperature is 50 DEG C, the time is 35h。
(2) Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon is obtained
Beta-cyclodextrin microballoon is added in distilled water, 60 DEG C is heated to and is dissolved into saturated solution；Every gram of beta-cyclodextrin microballoon The volume of the corresponding distilled water of quality is 30ml.
Saturated solution is cooled to after 30 DEG C and adds in Essential Oil of Acorus tatarinowii, after sealing in temperature 60 C ultrasonic vibration 5h, It is filtered after being cooled to 10 DEG C, obtains filter residue, then with petroleum ether filter residue, dried in temperature 60 C to constant weight and obtain stone Calamus volatile oil beta-cyclodextrin microballoon；
The quality of beta-cyclodextrin microballoon is 12g in the saturated solution added in wherein every milliliter of Essential Oil of Acorus tatarinowii.
Embodiment 4
(1) beta-cyclodextrin microballoon is prepared
3g beta-cyclodextrins are added in the 10mL sodium hydrate aqueous solutions that mass concentration is 0.3g/mL, 38 DEG C of constant temperature stirrings To being completely dissolved；Then rotating speed control to stir 1.5h at 38 DEG C for 780r/min, add in epoxychloropropane, together while stirring When add in kerosene, epoxychloropropane and kerosene mass ratio 3:2；Heating 60 DEG C when react 10h, then successively be filtered by vacuum, clean, Drying, grinding, obtain beta-cyclodextrin microballoon；
Wherein kerosene is the kerosene containing emulsifier Span-80, Tween-20, wherein emulsifier Span-80 and emulsifier The mass ratio of Tween-20 is 3:1；
It is cleaned successively using dilute hydrochloric acid, absolute ethyl alcohol, distilled water, acetone during cleaning；Drying temperature is 45 DEG C, the time is 40h。
(2) Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon is obtained
Beta-cyclodextrin microballoon is added in distilled water, 30 DEG C is heated to and is dissolved into saturated solution；Every gram of beta-cyclodextrin microballoon The volume of the corresponding distilled water of quality is 15ml.
Saturated solution is cooled to after 15 DEG C and adds in Essential Oil of Acorus tatarinowii, after sealing in 30 DEG C of temperature ultrasonic vibration 2h, It is filtered after being cooled to 4 DEG C, obtains filter residue, then with petroleum ether filter residue, dried in temperature 45 C to constant weight and obtain stone Calamus volatile oil beta-cyclodextrin microballoon；
The quality of beta-cyclodextrin microballoon is 9g in the saturated solution added in wherein every milliliter of Essential Oil of Acorus tatarinowii.
Embodiment 5
(1) beta-cyclodextrin microballoon is prepared
8g beta-cyclodextrins are added in the 10mL sodium hydrate aqueous solutions that mass concentration is 0.8g/mL, 33 DEG C of constant temperature stirrings To being completely dissolved；Then rotating speed control to stir 1.5h at 33 DEG C for 730r/min, add in epoxychloropropane, together while stirring When add in kerosene, epoxychloropropane and kerosene mass ratio 2:1；6h is reacted when being warming up to 60 DEG C, is then filtered by vacuum successively, is clear It washes, dry, grind, obtain beta-cyclodextrin microballoon；
Wherein kerosene is the kerosene containing emulsifier Span-80, Tween-20, wherein emulsifier Span-80 and emulsifier The mass ratio of Tween-20 is 3:1；
It is cleaned successively using dilute hydrochloric acid, absolute ethyl alcohol, distilled water, acetone during cleaning；Drying temperature is 55 DEG C, the time is 30h。
(2) Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon is obtained
Beta-cyclodextrin microballoon is added in distilled water, dissolves by heating into saturated solution；Every gram of beta-cyclodextrin microspheres quality pair The volume for the distilled water answered is 25ml；Heating temperature is 50 DEG C.
Saturated solution is cooled to after 25 DEG C and adds in Essential Oil of Acorus tatarinowii, after sealing in temperature 50 C ultrasonic vibration 4h, It is filtered after being cooled to 8 DEG C, obtains filter residue, then with petroleum ether filter residue, dried in 55 DEG C of temperature to constant weight and obtain stone Calamus volatile oil beta-cyclodextrin microballoon；
The quality of beta-cyclodextrin microballoon is 10g in the saturated solution added in wherein every milliliter of Essential Oil of Acorus tatarinowii.
Beta-cyclodextrin, the beta-cyclodextrin microballoon prepared and Essential Oil of Acorus tatarinowii β-ring paste are compared in observation under inverted microscope As a result successively as shown in Figure 1, Figure 2 and Figure 3 the shape characteristic of precise and tiny ball, shows by comparing：Essential Oil of Acorus tatarinowii beta-cyclodextrin Microsphere volume is substantially bigger than beta-cyclodextrin and beta-cyclodextrin microballoon, and substantially observes that Essential Oil of Acorus tatarinowii is wrapped by figure 3 In the inner cavity of Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon.
Beta-cyclodextrin microballoon, Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon and beta-cyclodextrin prepared by embodiment carries out infrared Spectrum compares.After beta-cyclodextrin, beta-cyclodextrin microballoon and Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon are distinguished KBr tablettings, use Fourier Transform Infrared Spectrometer (BRUKER T-27 types, Brooker Germany), in 4000~400cm of spectral region- 1, resolution ratio 4.000cm- 1Under conditions of scan 10 times.
As shown in figure 4, the infrared spectrum comparison diagram for beta-cyclodextrin and beta-cyclodextrin microballoon；As shown in figure 5, it is β-ring paste The infrared spectrum comparison diagram of precise and tiny ball and Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon.
The results of FT-IR shows：Beta-cyclodextrin and beta-cyclodextrin microballoon are in 3300-3500cm in Fig. 4-l、2900cm-l、 1000-1300cm-lThere is stretching vibration absworption peak in place, it was demonstrated that beta-cyclodextrin has apparent crosslinking with crosslinking agent.β-ring in Fig. 5 The infrared line of dextrin microballoon finds that beta-cyclodextrin microballoon exists compared with Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon infrared line 650~900cm-l, 2100~2400cm-lThere is very strong stretching vibration peak in place, illustrates based on phenols, aromatic compound The Essential Oil of Acorus tatarinowii of ingredient is wanted to be combined with the chemical bond in β-ring paste microballoon.
As shown in fig. 6, Essential Oil of Acorus tatarinowii, beta-cyclodextrin, beta-cyclodextrin microballoon, beta-cyclodextrin microballoon and grass-leaved sweetflag volatilize The differential heating scan of oily physical mixed and Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon is analyzed：Using METTLER STAR System type differential thermogravimetric analysis instrument measures, N2Air-flow protection, empty aluminium crucible rise as reference substance, 30~180 DEG C of scanning range Warm 10 DEG C/min of rate is measured.
DSC measurement results show：Essential Oil of Acorus tatarinowii is without characteristic peak；Beta-cyclodextrin nearby has a sharp melting at 112 DEG C Peak；This solid dispersion system of beta-cyclodextrin microballoon is presented a broad peak, is moved near 100 DEG C without sharp peak；Beta-cyclodextrin with Both beta-cyclodextrin microballoon fusion points are different and peak shape is also different, illustrate that beta-cyclodextrin microballoon is successfully prepared；It is micro- with beta-cyclodextrin Ball peak is compared, and the grass-leaved sweetflag beta-cyclodextrin microballoon of preparation has a reinforcement broad peak at 90 DEG C, the two fusion point is different and peak shape not yet Together, the inclusion Essential Oil of Acorus tatarinowii success of this experiment beta-cyclodextrin microballoon is illustrated.
The inclusion rate and yield of Essential Oil of Acorus tatarinowii β-ring paste microballoon are calculated, is repeated 3 times obtained Essential Oil of Acorus tatarinowii β-ring Dextrin microballoon records volume, according to Y1Formula calculates inclusion rate, 1 is the results are shown in Table, according to Y2Formula calculates yield, the results are shown in Table 2.
1 Essential Oil of Acorus tatarinowii β of table-ring paste microballoon inclusion rate
2 Essential Oil of Acorus tatarinowii β of table-ring paste microballoon yield
The result shows that：The inclusion rate of the Essential Oil of Acorus tatarinowii β that the present invention prepares-ring paste microballoon is carried with yield Height has good practical value.

Claims (10)

1. a kind of preparation method of Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon, which is characterized in that comprise the following steps：
Step 1, beta-cyclodextrin microballoon is prepared
Step 1.1, beta-cyclodextrin is added in sodium hydrate aqueous solution, constant temperature is stirred to being completely dissolved；
Step 1.2, epoxychloropropane is added into the solution of step 1.1, constant temperature adds in kerosene while stirring, heating is anti- Should, it is then filtered by vacuum, cleans successively, drying, grinding, obtaining beta-cyclodextrin microballoon；
Step 2, the beta-cyclodextrin microballoon of step 1 is added in distilled water, dissolves by heating into saturated solution；
Step 3, Essential Oil of Acorus tatarinowii will be added in after the saturated solution cooling in step 2, ultrasonic vibration after sealing is taken out after cooling Filter, obtains filter residue, dry to obtain Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon to constant weight then with petroleum ether filter residue.
A kind of 2. preparation method of Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon according to claim 1, which is characterized in that institute The mass concentration of sodium hydrate aqueous solution in step 1.1 is stated as 0.1-1.0g/mL, β-ring in every milliliter of sodium hydrate aqueous solution Dextrin quality is 0.1-1.0g；
The whipping temp of the constant temperature stirring is 30-40 DEG C.
A kind of 3. preparation method of Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon according to claim 1, which is characterized in that institute State epoxychloropropane and kerosene mass ratio 3 in step 1.2:2-2:1；
Wherein kerosene is the kerosene containing emulsifier Span-80, Tween-20, wherein emulsifier Span-80 and emulsifier The mass ratio of Tween-20 is 3:1.
A kind of 4. preparation method of Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon according to claim 3, which is characterized in that institute State constant temperature whipping temp in step 1.2 be 20-60 DEG C, mixing time 1-5h, rotating speed 500-1000r/min；
Wherein the temperature of temperature reaction is 20-60 DEG C, reaction time 6-24h.
A kind of 5. preparation method of Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon according to claim 4, which is characterized in that institute Stating cleaning in step 1.2 is specially：It is cleaned successively using dilute hydrochloric acid, absolute ethyl alcohol, distilled water, acetone；
The drying temperature is 40-60 DEG C, time 24-48h.
A kind of 6. preparation method of Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon according to claim 1, which is characterized in that institute The volume for stating the corresponding distilled water of every gram of beta-cyclodextrin microspheres quality in step 2 is 10-30ml；Heating temperature is 20-60 DEG C.
A kind of 7. preparation method of Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon according to claim 1, which is characterized in that institute The quality for stating beta-cyclodextrin microballoon in the saturated solution added in step 3 in every milliliter of Essential Oil of Acorus tatarinowii is 4-12g.
A kind of 8. preparation method of Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon according to claim 1, which is characterized in that institute The temperature for stating saturated solution after cooling down in step 3 is 10-30 DEG C.
A kind of 9. preparation method of Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon according to claim 1, which is characterized in that institute The temperature for stating step 3 ultrasonic vibration is 20-60 DEG C, time 1-5h.
10. a kind of preparation method of Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon according to claim 1, which is characterized in that Saturated solution temperature is 2-10 DEG C after being cooled down in the step 3；Drying temperature is 40-60 DEG C.
CN201810149026.0A 2018-02-13 2018-02-13 A kind of preparation method of Essential Oil of Acorus tatarinowii beta-cyclodextrin microballoon Pending CN108114105A (en)

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