CN108295226A - A kind of preparation method of Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon - Google Patents
A kind of preparation method of Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon Download PDFInfo
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- CN108295226A CN108295226A CN201810149015.2A CN201810149015A CN108295226A CN 108295226 A CN108295226 A CN 108295226A CN 201810149015 A CN201810149015 A CN 201810149015A CN 108295226 A CN108295226 A CN 108295226A
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- volatile oil
- rhizoma zingiberis
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- zingiberis recens
- cyclodextrin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/906—Zingiberaceae (Ginger family)
- A61K36/9068—Zingiber, e.g. garden ginger
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- 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
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/738—Cyclodextrins
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
-
- 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
- A61K2800/10—General cosmetic use
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- 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
Abstract
A kind of preparation method of Rhizoma Zingiberis Recens volatile oil beta cyclodextrin microballoon disclosed by the invention, beta cyclodextrin microballoon is added in distilled water and is dissolved by heating into saturated solution, Rhizoma Zingiberis Recens volatile oil is added after cooling, constant temperature stirs after sealing, it is filtered after cooling, with being drying to obtain after petroleum ether.The Rhizoma Zingiberis Recens volatile oil beta cyclodextrin microballoon that the preparation method of the present invention obtains can obviously increase Rhizoma Zingiberis Recens volatile oil water solubility, it covers its bad stink and mitigates its irritation, make to can be used as raw material and be added in cosmetics and drug, solve the problems, such as that Rhizoma Zingiberis Recens volatile oil poorly water-soluble, irritation are big, greatly improve the scope of application of Rhizoma Zingiberis Recens volatile oil, application idea has been widened in food, medicine and cosmetic field for Rhizoma Zingiberis Recens volatile oil, has been had important practical significance.
Description
Technical field
The invention belongs to method for preparing microsphere technical fields, and in particular to a kind of system of Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon
Preparation Method.
Background technology
Chinese medicine ginger is the fresh rhizome of Zingiber herbaceos perennial ginger (Zingiber officinale Roscoe),
Pungent, tepor, return lung taste warp has inducing sweat and dispelling exogenous evils, warming middle energizer to arrest vomiting, warm lung cough-relieving, solving toxin of fish and crab, the functions such as antidote poison；It is multi-purpose
In deficiency-cold in spleen and stomach, anorexia, nausea and vomiting or phlematic vomiting, the vomiting of disorder of stomach-energy；Chill or cold productive cough are coughed；Flu wind
It is cold, fever with aversion to wind, the illnesss such as nasal obstruction headache.
Rhizoma Zingiberis Recens volatile oil main component is curcumene, zingiberene, zingerone, zingiberol etc..Modern pharmacology shows Rhizoma Zingiberis Recens volatile oil
Have the function of excited cerebral cortex and nerve center, promote blood circulation and boost metabolism；In addition to this, ginger is being eaten
It is widely used as spice in product industry.Since Rhizoma Zingiberis Recens volatile oil is not soluble in water, and it is irritant with mucous membrane to skin, because
This application difficult in terms of preparation process 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 cyclic annular chemical combination for being coupled and generating
Object；By six molecules formed be known as alpha-cyclodextrin (α-CD), be made of seven molecules be beta-cyclodextrin (β-CD), by
That eight molecules are formed is γ cyclodextrin (γ-CD).α-CD cavitys are smaller, and γ-CD prices are more expensive, 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's also positive development microballoon this pharmaceutical formulation techniques, are answered in recent years
Rhizoma Zingiberis Recens volatile oil is prepared into microballoon with beta-cyclodextrin, its stability and bioavailability can be improved, reduces irritation, is expanded
Its application in fields such as biological medicine, food, environmental protection.
Invention content
The object of the present invention is to provide a kind of preparation methods of Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon, solve the prior art
The problem of.
The technical solution adopted in the present invention is a kind of preparation method of Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon, including with
Lower step：
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, kerosene is added while stirring in constant temperature, 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, 20-60 DEG C of heating is to being dissolved into saturated solution；
The volume of the corresponding distilled water of every gram of beta-cyclodextrin microspheres quality is 10-25ml；
Step 3, Rhizoma Zingiberis Recens volatile oil will be added after the saturated solution cooling in step 2, constant temperature stirs after sealing, is taken out after cooling
Filter, obtains filter residue, then uses petroleum ether filter residue, dry to obtain Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon to constant weight.
It is of the invention to be further characterized in that,
The mass concentration of sodium hydrate aqueous solution is 0.1-1.0g/mL, every milliliter of sodium hydrate aqueous solution in step 1.1
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；
The temperature of temperature reaction is 20-60 DEG C, reaction time 6-24h.
It is cleaned in step 1.2 and is specially：Dilute hydrochloric acid, absolute ethyl alcohol, distilled water, acetone is used to clean successively；
Drying temperature is 40-60 DEG C, time 24-48h.
The quality of beta-cyclodextrin microballoon is 4-12g in the saturated solution added in every milliliter of Rhizoma Zingiberis Recens volatile oil in step 3.
The temperature of saturated solution is 20-30 DEG C after cooling down in step 3.
The temperature that constant temperature stirs in step 3 is 30-60 DEG C, time 3-24h.
Saturated solution temperature is 2-10 DEG C after cooling in step 3.
Drying temperature is 40-60 DEG C in step 3.
The beneficial effects of the invention are as follows：A kind of preparation method of Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon of the present invention passes through stirring
Method prepares products therefrom, can get Rhizoma Zingiberis Recens volatile oil microballoon, improves the water solubility of Rhizoma Zingiberis Recens volatile oil, cover bad stink and mitigate it
Irritation solves the problems, such as that Rhizoma Zingiberis Recens volatile oil poorly water-soluble, irritation are big, greatly improves being applicable in for Rhizoma Zingiberis Recens volatile oil
Range has widened application idea in food, medicine and cosmetic field for Rhizoma Zingiberis Recens volatile oil, has had important practical significance；System
Standby obtained Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon can obviously increase Rhizoma Zingiberis Recens volatile oil water solubility, cover its bad stink and mitigate it
Irritation, makes to can be used as raw material and is added in cosmetics and drug.
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；
Fig. 3 is the microscope scanning figure of Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon prepared by the present invention；
Fig. 4 is the infrared spectrum analysis IR spectrograms of five kinds of substances；
In wherein Fig. 4, A is beta-cyclodextrin, and B is the beta-cyclodextrin microballoon that the present invention is prepared, and C is prepared into for the present invention
The Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon arrived, D are Rhizoma Zingiberis Recens volatile oil, and E is that the physics of Rhizoma Zingiberis Recens volatile oil and beta-cyclodextrin microballoon is mixed
Close object；
Fig. 5 is that the differential heating scan analysis DSC of five kinds of substances of the present invention measures spectrogram；
In wherein Fig. 5, A is beta-cyclodextrin, and B is the beta-cyclodextrin microballoon that the present invention is prepared, and C is prepared into for the present invention
The Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon arrived, D are Rhizoma Zingiberis Recens volatile oil, and E is that the physics of Rhizoma Zingiberis Recens volatile oil and beta-cyclodextrin microballoon is mixed
Close object.
Specific implementation mode
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
A kind of preparation method of Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon of the present invention, includes 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
Shi Hengwen is stirred to being completely dissolved；Beta-cyclodextrin quality is 0.1-1.0g in every milliliter of sodium hydrate aqueous solution；
Step 1.2, add epoxychloropropane into the solution of step 1.1,20-60 DEG C, rotating speed 500-1000r/min when
Kerosene is added while stirring 1-5h in constant temperature, is warming up to 20-60 DEG C of reaction 6-24h, is then filtered by vacuum successively, successively using dilute
Hydrochloric acid, absolute ethyl alcohol, distilled water, acetone cleaning, 40-60 DEG C of drying 24-48h, grinding, obtain beta-cyclodextrin microballoon；Epoxy chlorine
Propane and kerosene mass ratio 3:2-2:1；Wherein kerosene is the kerosene containing emulsifier Span-80, Tween-20, wherein emulsifier
The mass ratio of Span-80 and emulsifier Tween-20 are 3:1.
Step 2, the beta-cyclodextrin microballoon of step 1 is added in distilled water, 20-60 DEG C of heating is to being dissolved into saturated solution；
The volume of the corresponding distilled water of every gram of beta-cyclodextrin microspheres quality is 10-25ml；
Step 3, Rhizoma Zingiberis Recens volatile oil is added after the saturated solution in step 2 being cooled to 20-30 DEG C, constant temperature stirs after sealing
It mixes, is filtered after cooling, obtain filter residue, then use petroleum ether filter residue, it is dry that Rhizoma Zingiberis Recens volatile oil β-ring paste is obtained to constant weight
Precise and tiny ball；The quality of beta-cyclodextrin microballoon is 4-12g in the saturated solution added in every milliliter of Rhizoma Zingiberis Recens volatile oil；Constant temperature stirs
Temperature be 30-60 DEG C, time 3-24h；Saturated solution temperature is 2-10 DEG C after cooling；Drying temperature is 40-60 DEG C.
Embodiment 1
(1) beta-cyclodextrin microballoon is prepared
Beta-cyclodextrin is added in the sodium hydrate aqueous solution that mass concentration is 1.0g/mL, constant temperature is stirred to complete at 40 DEG C
Fully dissolved；Beta-cyclodextrin quality is 1g in every milliliter of sodium hydrate aqueous solution；
Add epoxychloropropane into solution, 60 DEG C, rotating speed 500r/min when constant temperature stirring 5h while kerosene is added,
It is warming up to 60 DEG C of reactions for 24 hours, is then filtered by vacuum successively, uses dilute hydrochloric acid, absolute ethyl alcohol, distilled water, acetone cleaning, 50 successively
DEG C drying 48h, grinding, obtain beta-cyclodextrin microballoon；Epoxychloropropane and kerosene mass ratio 3:2；Wherein kerosene is to contain emulsification
The kerosene of agent Span-80, Tween-20, the wherein mass ratio of emulsifier Span-80 and emulsifier Tween-20 are 3:1.
(2) the beta-cyclodextrin microballoon of step 1 is added in distilled water, 60 DEG C of heating is to being dissolved into saturated solution；Every gram of β-
The volume of the corresponding distilled water of cyclodextrin microsphere quality is 25ml；
(3) saturated solution is cooled to after 30 DEG C and Rhizoma Zingiberis Recens volatile oil is added, constant temperature stirs after sealing, filters, obtains after cooling
To filter residue, petroleum ether filter residue is then used, it is dry to obtain Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon to constant weight；Every milliliter of life
The quality of beta-cyclodextrin microballoon is 12g in the saturated solution added in Rhizoma Zingiberis Recens volatile oil；The temperature of constant temperature stirring is 30 DEG C, the time
20h；Saturated solution temperature is 8 DEG C after cooling；Drying temperature is 50 DEG C.
Embodiment 2
(1) beta-cyclodextrin microballoon is prepared
Beta-cyclodextrin is added in the sodium hydrate aqueous solution that mass concentration is 0.1g/mL, constant temperature is stirred to complete at 30 DEG C
Fully dissolved；Beta-cyclodextrin quality is 0.1g in every milliliter of sodium hydrate aqueous solution；
Add epoxychloropropane into solution, 40 DEG C, rotating speed 1000r/min when constant temperature stirring 1h while coal is added
Oil is warming up to 60 DEG C of reaction 12h, is then filtered by vacuum successively, uses dilute hydrochloric acid, absolute ethyl alcohol, distilled water, acetone clear successively
It washes, 40 DEG C of drying 48h, grindings, obtains beta-cyclodextrin microballoon；Epoxychloropropane and kerosene mass ratio 2:1；Wherein kerosene be containing
The kerosene of emulsifier Span-80, Tween-20, the wherein mass ratio of emulsifier Span-80 and emulsifier Tween-20 are 3:1.
(2) beta-cyclodextrin microballoon is added in distilled water, 20 DEG C of heating is to being dissolved into saturated solution；Every gram of beta-cyclodextrin is micro-
The volume of the corresponding distilled water of ball quality is 10ml；
(3) saturated solution is cooled to after 30 DEG C and Rhizoma Zingiberis Recens volatile oil is added, constant temperature stirs after sealing, filters, obtains after cooling
To filter residue, petroleum ether filter residue is then used, it is dry to obtain Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon to constant weight；Every milliliter of life
The quality of beta-cyclodextrin microballoon is 4g in the saturated solution added in Rhizoma Zingiberis Recens volatile oil；The temperature of constant temperature stirring is 30 DEG C, the time
24h；Saturated solution temperature is 10 DEG C after cooling；Drying temperature is 60 DEG C.
Embodiment 3
(1) beta-cyclodextrin microballoon is prepared
Beta-cyclodextrin is added in the sodium hydrate aqueous solution that mass concentration is 0.4g/mL, constant temperature is stirred to complete at 35 DEG C
Fully dissolved；Beta-cyclodextrin quality is 0.6g in every milliliter of sodium hydrate aqueous solution；
Add epoxychloropropane into solution, 30 DEG C, rotating speed 750r/min when constant temperature stirring 1.5h while coal is added
Oil is warming up to 60 DEG C of reaction 6h, be then filtered by vacuum successively, dilute hydrochloric acid, absolute ethyl alcohol, distilled water, acetone is used to clean successively,
60 DEG C drying for 24 hours, grinding, obtain beta-cyclodextrin microballoon；Epoxychloropropane and kerosene mass ratio 3:2；Wherein kerosene is to contain breast
The kerosene of agent Span-80, Tween-20, the wherein mass ratio of emulsifier Span-80 and emulsifier Tween-20 are 3:1.
(2) beta-cyclodextrin microballoon is added in distilled water, 41 DEG C of heating is to being dissolved into saturated solution；Every gram of beta-cyclodextrin is micro-
The volume of the corresponding distilled water of ball quality is 15ml；
(3) saturated solution is cooled to after 30 DEG C and Rhizoma Zingiberis Recens volatile oil is added, constant temperature stirs after sealing, filters, obtains after cooling
To filter residue, petroleum ether filter residue is then used, it is dry to obtain Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon to constant weight；Every milliliter of life
The quality of beta-cyclodextrin microballoon is 10g in the saturated solution added in Rhizoma Zingiberis Recens volatile oil；The temperature of constant temperature stirring is 30 DEG C, the time
24h；Saturated solution temperature is 2 DEG C after cooling；Drying temperature is 40 DEG C.
Beta-cyclodextrin, beta-cyclodextrin microballoon and Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon packet are compared in observation under inverted microscope
Close object shape characteristic, as a result successively as shown in Figure 1, Figure 2 and Figure 3：It was found that Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon includes object
Product obviously increases than β-CD and beta-cyclodextrin microballoon is big, and obviously sees the inner cavity that Rhizoma Zingiberis Recens volatile oil is enclosed in beta-cyclodextrin microballoon
In.
Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon prepared by the present invention volatilizees with beta-cyclodextrin, beta-cyclodextrin microballoon, ginger
Oil, Rhizoma Zingiberis Recens volatile oil and beta-cyclodextrin mixture of microspheres carry out infrared spectrum comparison.By beta-cyclodextrin, beta-cyclodextrin microballoon, life
Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon, Rhizoma Zingiberis Recens volatile oil, Rhizoma Zingiberis Recens volatile oil and beta-cyclodextrin mixture of microspheres make after KBr tablettings respectively
With Fourier Transform Infrared Spectrometer (BRUKER T-27 types, Brooker Germany), 4000~400cm of spectral region- 1, resolution ratio
4.000cm- 1, scanning times 10 times.
Measurement result is as shown in figure 4, the beta-cyclodextrin microballoon of Fig. 4 B is compared with the beta-cyclodextrin of Fig. 4 A, and two lines are in 906cm-1
The absorption peak of left and right epoxy group disappears, and illustrates that crosslinking agent is reacted with beta-cyclodextrin, in 3400cm-1All go out at left and right
The now absorption peak of strong-OH, in 2900cm-1There is-CH at place2Absorption peak, and the peak of beta-cyclodextrin microballoon is stronger, is β-ring
Dextrin and-CH after cross-linking agents2Caused by increasing, 1300~1000cm-1Place is the characteristic peak of ehter bond, and the peak after polymerization is wider
Relatively strong, further demonstrating beta-cyclodextrin and crosslinking agent has apparent crosslinking, beta-cyclodextrin microballoon to be successfully prepared；Fig. 4 C gingers are waved
Hair oil beta-cyclodextrin microballoon is compared with the beta-cyclodextrin microballoon of Fig. 4 B, the spectrum of the characteristic absorption peak of beta-cyclodextrin microballoon in inclusion compound
It is embodied completely in line, and without other different peaks.It is possible thereby to initial guess, Rhizoma Zingiberis Recens volatile oil is micro- by beta-cyclodextrin
Ball includes；Fig. 4 C Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoons are compared with Fig. 4 D Rhizoma Zingiberis Recens volatile oils, the characteristic absorption peak of Rhizoma Zingiberis Recens volatile oil
It has disappeared in inclusion compound；The object of Fig. 4 C Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon and Fig. 4 E Rhizoma Zingiberis Recens volatile oils and beta-cyclodextrin microballoon
Reason mixture is compared, and Fig. 4 E Rhizoma Zingiberis Recens volatile oils are inhaled with there is the feature of apparent volatile oil in the physical mixture of beta-cyclodextrin microballoon
Peak is received, in 1300~1000cm-1Also there is the characteristic absorption peak of beta-cyclodextrin microballoon at place, therefore can further prove that ginger volatilizees
Oil is included by beta-cyclodextrin microballoon.
It is measured using METTLER STAR System type differential thermogravimetric analysis instrument, N2Air-flow protection, empty aluminium crucible is as ginseng
Than object, 30~280 DEG C of scanning range, 10 DEG C/min of heating rate is measured.The results are shown in Figure 5：The beta-cyclodextrin and figure of Fig. 5 A
The beta-cyclodextrin microballoon of 5B has a melting peak at 85 DEG C or so, illustrates that the beta-cyclodextrin microballoon prepared does not contain other impurities,
But the former melting peak is sharp compared with the latter, and the two peak shape is different, illustrates that beta-cyclodextrin microballoon is successfully prepared；With the beta-cyclodextrin of Fig. 5 B
Microballoon is compared, and the beta-cyclodextrin microballoon inclusion compound of Fig. 5 C shows a reinforcement broad peak at 80 DEG C or so, and with volatile oil and Fig. 5 E
Beta-cyclodextrin microballoon the sharp peak that is presented of physical mixture it is different, illustrate Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon inclusion compound
It is successfully prepared.
Claims (10)
1. a kind of preparation method of Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon, which is characterized in that include 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, kerosene is added in constant temperature while stirring, heating is anti-
It answers, 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, 20-60 DEG C of heating is to being dissolved into saturated solution；Every gram
The volume of the corresponding distilled water of beta-cyclodextrin microspheres quality is 10-25ml；
Step 3, Rhizoma Zingiberis Recens volatile oil being added after the saturated solution cooling in step 2, constant temperature stirs after sealing, is filtered after cooling,
Filter residue is obtained, petroleum ether filter residue is then used, it is dry to obtain Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon to constant weight.
2. a kind of preparation method of Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon according to claim 1, which is characterized in that described
The mass concentration of sodium hydrate aqueous solution is 0.1-1.0g/mL in step 1.1, β-ring paste in every milliliter of sodium hydrate aqueous solution
Extract Iuality is 0.1-1.0g；
The whipping temp of the constant temperature stirring is 30-40 DEG C.
3. a kind of preparation method of Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon according to claim 2, which is characterized in that described
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.
4. a kind of preparation method of Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon according to claim 3, which is characterized in that described
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.
5. a kind of preparation method of Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon according to claim 6, which is characterized in that described
It is cleaned in step 1.2 and is specially：Dilute hydrochloric acid, absolute ethyl alcohol, distilled water, acetone is used to clean successively；
The drying temperature is 40-60 DEG C, time 24-48h.
6. according to a kind of preparation method of any Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoons of claim 1-5, feature exists
In the quality of beta-cyclodextrin microballoon is 4-12g in the saturated solution added in every milliliter of Rhizoma Zingiberis Recens volatile oil in the step 3.
7. a kind of preparation method of Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon according to claim 6, which is characterized in that described
The temperature of saturated solution is 20-30 DEG C after cooling down in step 3.
8. a kind of preparation method of Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon according to claim 6, which is characterized in that described
The temperature that constant temperature stirs in step 3 is 30-60 DEG C, time 3-24h.
9. a kind of preparation method of Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon according to claim 6, which is characterized in that described
Saturated solution temperature is 2-10 DEG C after cooling in step 3.
10. a kind of preparation method of Rhizoma Zingiberis Recens volatile oil beta-cyclodextrin microballoon according to claim 6, which is characterized in that institute
It is 40-60 DEG C to state drying temperature in step 3.
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| US20060120967A1 (en) * | 2004-12-07 | 2006-06-08 | Qpharma, Llc | Solution forms of cyclodextrins for nasal or throat delivery of essential oils |
| CN102443198A (en) * | 2010-10-12 | 2012-05-09 | 李沈田 | Ginger volatile oil-beta-cyclodextrin inclusion compound and preparation method thereof |
| CN102703221A (en) * | 2012-05-29 | 2012-10-03 | 商洛学院 | Preparation method of rose essence beta-cyclodextrin polymer microsphere inclusion compound |
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|---|---|---|---|---|
| US20060120967A1 (en) * | 2004-12-07 | 2006-06-08 | Qpharma, Llc | Solution forms of cyclodextrins for nasal or throat delivery of essential oils |
| CN102443198A (en) * | 2010-10-12 | 2012-05-09 | 李沈田 | Ginger volatile oil-beta-cyclodextrin inclusion compound and preparation method thereof |
| CN102703221A (en) * | 2012-05-29 | 2012-10-03 | 商洛学院 | Preparation method of rose essence beta-cyclodextrin polymer microsphere inclusion compound |
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| 杨黎燕等: "薄荷油β-环糊精聚合物的制备及性能研究", 《化工科技》 * |
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