CN108404140A - A kind of clathrate process of volatile oil - Google Patents
A kind of clathrate process of volatile oil Download PDFInfo
- Publication number
- CN108404140A CN108404140A CN201810454592.2A CN201810454592A CN108404140A CN 108404140 A CN108404140 A CN 108404140A CN 201810454592 A CN201810454592 A CN 201810454592A CN 108404140 A CN108404140 A CN 108404140A
- Authority
- CN
- China
- Prior art keywords
- volatile oil
- parts
- peppermint
- schizonepeta
- ethyl alcohol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 238000000034 method Methods 0.000 title claims abstract description 23
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 40
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Classifications
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Abstract
The invention discloses a kind of clathrate process of volatile oil, with ethyl alcohol it is dispersant beforehand dilution by the volatile oil of peppermint and schizonepeta extraction gained, is then included with beta cyclodextrin；Wherein the ratio between volume of volatile oil and ethyl alcohol is 1: 3~1: 5, and the mass ratio of volatile oil and beta cyclodextrin is 1: 5~1: 8, includes 1.5~2.5h of time, includes 30~40 DEG C of temperature, 50 DEG C or less dry 3~5h.The clathrate process that the present invention uses is obtainable with higher inclusion rate and medicine stability.
Description
The application is application for a patent for invention (application number：201610378512.0 the applying date：2016.06.01, invention name
Claim：Chuan Xiong Tea particle and preparation method thereof) divisional application.
Technical field
The present invention relates to Chinese medicinal preparation methods, and in particular to a kind of clathrate process of volatile oil.
Background technology
Chuan Xiong Tea granular raw side comes from《The formulary of peaceful benevolent dispensary》Chuanxiong Chatiao San, mainly by Rhizoma Chuanxiong, the root of Dahurain angelica, Qiang
Work, asarum, windproof, peppermint, schizonepeta, Radix Glycyrrhizae composition, have dispelling wind and relieving effect, for ailment said due to cold or exposure headache, or have aversion to cold, fever,
Nasal obstruction, clinical efficacy are definite.
Chinese Pharmacopoeia 2010 editions one has included Chuanxiong Chatiao San Traditional Chinese medicine historical preparation, is formulated as Rhizoma Chuanxiong 120g, the root of Dahurain angelica
60g, Rhizoma Et Radix Notopterygii 60g, asarum 30g, windproof 45g, peppermint 240g, schizonepeta 120g, Radix Glycyrrhizae 60g, preparation method：Ingredients crushes
At direct mixing after fine powder.
Chuanxiong Chatiao San,《Office side》It uploads：" Chuanxiong Chatiao San is controlled husband, is attacked on married woman Zhu Feng, the head's dusk weight, polarization head
Bitterly, stuffy nose and low voice speaking ... but sense general mood, know and all control it." now it is mainly used for ailment said due to cold or exposure headache, it is monarch to select Rhizoma Chuanxiong, and promoting blood circulation and stopping pain is modern
Research is also mostly based on Rhizoma Chuanxiong principle active component ferulic acid.But full side is made a general survey of, only peppermint most significant, the controlled primary symptom of we
Caused by diseases caused by external factors ailment said due to cold or exposure, all YANG-meridians meeting into the head disturbs head in ailment said due to cold or exposure, checks the gas of clear sun, therefore sees headache.First there is ailment said due to cold or exposure criminal's table,
Afterwards just on disturb clear sun.It can be seen that exterior syndrome caused by ailment said due to cold or exposure is it, has a headache and marked for it.Reuse peppermint, not only can dispelling wind pathogens, but also can clear profit
The head, it is all powerful to marking to this.But modern study to the extraction of the effect of peppermint in we and active ingredient (menthol) not
It draws attention.Though extracting volatile oil, under various extracting conditions, the active ingredient type of Mixed chaotic sequences to schizonepeta, peppermint
And proportioning differs widely, and has method and is not thorough to the extraction of menthol, still needs to make peppermint alcohol extracting using more effective way
Rate improves, so that it has more preferable curative effect.
Peppermint, schizonepeta Mixed chaotic sequences in Chuan Xiong Tea particle are lipophilic substance, are played in curative effect of medication important
Effect, not only can dispelling wind pathogens, but also can head clearing.Since content is low in both drugs for volatile oil, and be it is volatile and
Unstable ingredient, the practical efficiency of volatile oil is at a fairly low in preparation.Merely by the theoretical method of incremental dose
It is undesirable, because dosage increases, more other compositions in both medicinal materials can be caused to be extracted, to influence drug
Effect.In addition, the Chuan Xiong Tea particle of the aforementioned prior art using ethyl alcohol dissolving be injected directly by the way of, the stabilization of drug
Property there are problem, simultaneously as the characteristic of granule instructions of taking, need evenly dispersed with water, the dissolubility of active principle becomes
The key point of its bioactivity is played, volatile oil poorly water-soluble, bioavilability is low, and Clinical practice is restricted.
Relative to the present invention, there are following places that have much room for improvement for the prior art：1, the formula of extract, curative effect first have
It waits further increasing.2, the active ingredient peppermint alcohol extracting of the flavour of a drug peppermint of Chuan Xiong Tea particle is not thorough, influences peppermint and dredges
Wind head clearing, the effect for the treatment of both manifestation and root cause of disease, and then influence the advantage of " but the sense general mood, know and all control it " of Chuanxiong Chatiao San.3, river
Peppermint, schizonepeta Mixed chaotic sequences in rhizome of chuanxiong tea tune particle, in such a way that ethyl alcohol dissolving is injected directly into, the stability of drug and molten
Solution property is there are problem, the effect of influencing drug.
Invention content
It is an object of the present invention to provide a kind of best peppermint, the clathrate process of Herba Schizonepetae volatile oil, to improve drug
Inclusion rate and stability.
The technical scheme is that a kind of clathrate process of volatile oil is provided, by waving obtained by peppermint and schizonepeta extraction
Hair oil is dispersant beforehand dilution with ethyl alcohol, is then included with beta-cyclodextrin；Wherein the ratio between the volume of volatile oil and ethyl alcohol
It is 1: 3~1: 5, the mass ratio of volatile oil and beta-cyclodextrin is 1: 5~1: 8, includes 1.5~2.5h of time, includes temperature 30
~40 DEG C, 50 DEG C or less dry 3~5h.
Preferably, the ratio between volume of volatile oil and ethyl alcohol is 1: 4, and the mass ratio of volatile oil and beta-cyclodextrin is 1: 8, packet
Time 2h is closed, 40 DEG C of temperature, 50 DEG C or less dry 3h are included.
Preferably, the temperature of the drying is 40~50 DEG C.
Preferably, the volatile oil is to be used as mixing medicinal material through steam distillation by 2: 1 mass ratio by peppermint and schizonepeta
Extraction obtains.
Preferably, the technique of the steam distillation extraction is：With the water of 3~5 times of quality, distill 3~4 hours.
Another object of the present invention is to improve the preparation method of volatile oil in Chuan Xiong Tea particulate production, to improve
The recovery rate of volatile oil.A further object of the present invention is to propose that a kind of improved Chuan Xiong Tea granular recipe, the formula have
The effect of raising.Further object of the present invention is to improve first to have the auxiliary material of Chuan Xiong Tea particle to design, to reduce its clinical application
It is restricted.
According to the present invention, a kind of Chuan Xiong Tea particle is provided, is mainly made of following ingredients：Dried cream powder 220~270
Part, 16~28 parts of volatile oil clathrate compound, 150~220 parts of excipient, wherein the volatile oil clathrate compound is by peppermint and schizonepeta
Through steam extraction prepare volatile oil with beta-cyclodextrin inclusion compound be made, the dried cream powder be by Rhizoma Chuanxiong, the root of Dahurain angelica, Rhizoma Et Radix Notopterygii, asarum,
Windproof, Radix Glycyrrhizae Aqueous extracts and the peppermint extract volatile oil with schizonepeta after Aqueous extracts merges, concentrate it is obtained.
Further, which includes 6~14 parts of Steviosin.
In a preferred embodiment, the excipient is soluble starch, also, the Chuan Xiong Tea particle is main
It is grouped as by the group of following ratios：10 parts of 245 parts of dried cream powder, 22 parts of volatile oil clathrate compound, 185 parts of soluble starch and Steviosin
Composition.
Further, the Rhizoma Chuanxiong, peppermint, schizonepeta, the root of Dahurain angelica, Rhizoma Et Radix Notopterygii, asarum, windproof and Radix Glycyrrhizae composition be by weight
For：120 parts of Rhizoma Chuanxiong, 220~260 parts of peppermint, 100~140 parts of schizonepeta, 50-70 parts of the root of Dahurain angelica, 50~70 parts of Rhizoma Et Radix Notopterygii, asarum 25~
35 parts, windproof 35~55 parts and 50~70 parts of Radix Glycyrrhizae.
Further, the volatile oil is obtained by steam distillation by 120 parts of 240 parts of peppermint and schizonepeta.
The present invention also provides a kind of Chuan Xiong Tea preparation method of granules, include the following steps：1) by Rhizoma Chuanxiong, the root of Dahurain angelica, Rhizoma Et Radix Notopterygii,
Asarum, windproof, Radix Glycyrrhizae add water to cook, and obtain the first Aqueous extracts；2) peppermint, schizonepeta are mixed with 2 to 1 ratio, carries out water steaming
Steam distillation is extracted, and volatile oil and the second Aqueous extracts are obtained；3) the cyclodextrin encapsulated volatile oil of β-CD is used, inclusion compound is obtained；4)
Merge first Aqueous extracts and second Aqueous extracts, is condensed into medicinal extract, dried cream powder is made；5) by the dried cream powder, inclusion
Object is mixed with excipient, and granulation obtains the Chuan Xiong Tea particle.
Preferably, the inclusion described in step 3) is to use following conditions：The ratio between volatile oil, ethyl alcohol are 1: 3~1: 5,
The ratio between volatile oil and β-CD are 1: 5~1: 8, include 1.5~2.5h of time, include 30~40 DEG C of temperature, and 40~50 DEG C or less dry
It is dry.
Preferably, the mixing ratio of the dried cream powder, the volatile oil clathrate compound and the excipient is：Dried cream powder
220~270 parts, 16~28 parts of volatile oil clathrate compound, 150~220 parts of excipient.
Preferably, Rhizoma Chuanxiong, peppermint, schizonepeta, the root of Dahurain angelica, Rhizoma Et Radix Notopterygii, asarum, windproof and Radix Glycyrrhizae composition are by weight：River
120 parts of rhizome of chuanxiong, 240 parts of peppermint, 120 parts of schizonepeta, 60 parts of the root of Dahurain angelica, 60 parts of Rhizoma Et Radix Notopterygii, 30 parts of asarum, windproof 45 parts and 60 parts of Radix Glycyrrhizae.
Preferably, 245 parts of dried cream powder, 22 parts of volatile oil clathrate compound, 185 parts of soluble starch, 10 parts of Steviosin.
In terms of technique effect, the present invention introduces peppermint oil and the volatile oil clathrate compound of schizonepeta in finished product, improves
The stability and curative effect of drug.The essential oil extraction method and inclusion essential oil method that the present invention uses, to greatest extent land productivity
With volatile oil in raw material so that the volatile oil content highest in finished product.
Specific implementation mode
In the present invention, unless stated otherwise, when referring to proportioning, term " part " refers to parts by weight.
In the present invention, for Rhizoma Chuanxiong, the root of Dahurain angelica, Rhizoma Et Radix Notopterygii, asarum, windproof and Radix Glycyrrhizae extraction, traditional method may be used,
They are merged into extraction, usually using ethyl alcohol or water as Extraction solvent, is preferably extracted with water.Such as measured with 5-8 times
Water decocts twice, is then combined with filtrate, and dried cream powder is made in concentration, drying.
In the present invention, the extraction process of volatile oil is optimized, remarkable effect is achieved.Peppermint in the present invention,
Schizonepeta amount ratio is 2: 1.The prior art is to carry out steam distillation with water more than 6 times of amounts, distillation time usually at 5 hours or
Person is longer.However, it has been found that when being distilled using the water of relatively low amount to peppermint and schizonepeta, more is obtained instead
Volatile oil, moreover, distillation time can shorten.3~5 times of amount (mass ratio) water of the present invention, steam distillation 3~4 hours,
The recovery rate higher of menthol in Mixed chaotic sequences further preferably adds 5 times of amount water, distills 4 hours.It is not intended to by theoretical institute
Constraint, one the possible reason is：The main component of Herba Menthae Haplocalycis volatile oil is monoterpene and its containing oxygen derivative, such as menthol, new thin
Lotus alcohol etc. belongs to low boiling point organic compound.Low boiling point component is distilled off at first during volatile oil extracting, heated time with
And the time contacted with vapor, to compare other compositions longer, if heated for a long time, the lower active ingredient of boiling point is easy to decompose
Loss, influences the property and curative effect of volatile oil component.When amount of water is more simultaneously, since the quantity of steam of generation is big, low boiling point is waved
Hair oil is not easy to be cooled, and is easily taken away by vapor, causes volatile oil production loss.
In the present invention, inclusion essential oil is optimized, is dispersant beforehand dilution volatile oil with ethyl alcohol, then uses
β-CD are included.Determine dispersant (ethyl alcohol) and with the ratio of volatile oil, the ratio of volatile oil and β-CD, inclusion temperature,
Time, drying temperature, drying time etc. are included, it is found that the ratio between oil and ethyl alcohol are 1: 3~1: 5, the ratio between volatile oil and β-CD are 1: 5
~1: 8,1.5~2.5h of time is included, 30~40 DEG C of temperature, 40~50 DEG C or less dry 3~5h, to the inclusion of menthol are included
Rate improves, and further preferably, volatile oil is diluted in 1: 4 ratio with absolute ethyl alcohol, and 8 times of amount β-cdinclusions, the inclusion time is 2 small
When, inclusion temperature is 40 DEG C, and low temperature (50 DEG C or less dryings) is 3 hours dry.It is demonstrated experimentally that using the inclusion compound of the gain of parameter
With highest inclusion rate and medicine stability.
In addition, this patent substitutes the function as sweeteners of sucrose using Steviosin, sugariness it is high (sugariness be sucrose 200~
350 times), institute's heat content is few (being only the 1/300 of sucrose), and dosage is few, there is preferable heat resistance and stability, not by people after eating
Body directly absorbs, and does not generate thermal energy, but is degraded to steviol by enteric microorganism, is excreted with stool, will not cause blood
Sugared concentration increases, therefore is diabetes, the good natural sweetener of bariatric patients.Avoid other Sugarless type Rhizoma Chuanxiong tea simultaneously
Particle is adjusted to improve the safety of product using the adverse reaction of lactose lactose intolerance caused by possible.It is simultaneously improvement
Grain forming and melting, the better soluble starch of dissolubility is added, and (soluble starch is steady without reducing substances, chemical property
Fixed, strong adsorption force, good fluidity can become the clear solution of high degree of dispersion in water).
Another aspect of the present invention further relates to the composition being made of the extract that aforementioned preferred method obtains, the composition
It is preferred that particle can be made.The composition mainly by 220~270 parts of dried cream powder, 16~28 parts of volatile oil clathrate compound and solvable
Property 150~220 parts of starch composition, include preferably further 6~14 parts of Steviosin.Further preferably by 245 parts of dried cream powder, volatilization
22 parts of oily inclusion compound, 10 parts of compositions of 185 parts of soluble starch and Steviosin.Rhizoma Chuanxiong, schizonepeta, the root of Dahurain angelica, Rhizoma Et Radix Notopterygii, asarum, is prevented peppermint
Wind and the composition of Radix Glycyrrhizae preferably 120 parts of Rhizoma Chuanxiong, 220~260 parts of peppermint, 100~140 parts of schizonepeta, root of Dahurain angelica 50-70 by weight
Part, 50-70 parts of Rhizoma Et Radix Notopterygii, 25-35 parts of asarum, windproof 35-55 parts and 50-70 parts of Radix Glycyrrhizae, it is more excellent for 120 parts of Rhizoma Chuanxiong, peppermint 240
Part, 120 parts of schizonepeta, 60 parts of the root of Dahurain angelica, 60 parts of Rhizoma Et Radix Notopterygii, 30 parts of asarum, windproof 45 parts and 60 parts of Radix Glycyrrhizae are made.It is demonstrated experimentally that having
The composition of this proportioning shows advantageous curative effect.
Embodiment 1：Medicine preparation
It is raw materials used：299.8 parts of Rhizoma Chuanxiong, 149.9 parts of the root of Dahurain angelica, 149.9 parts of Rhizoma Et Radix Notopterygii, 75.05 parts of asarum, it is 112.5 parts windproof,
299.8 parts of schizonepeta, 599.8 parts of peppermint, 149.9 parts of Radix Glycyrrhizae.
Above eight taste, Rhizoma Chuanxiong, the root of Dahurain angelica, Rhizoma Et Radix Notopterygii, asarum, windproof, Radix Glycyrrhizae add water to cook secondary, first time plus 6 times of amount water, pan-fried
It boils 1.5 hours, second plus 5 times of amount water decoct 1 hour, collecting decoction, filtration；Peppermint, schizonepeta add 5 times of amount water, vapor to steam
Evaporate extraction volatile oil 4 hours, volatile oil is diluted with 1: 4 ratio with absolute ethyl alcohol, and 8 times of amount β-cdinclusions, the inclusion time is 2 small
When, inclusion temperature is 40 DEG C, and filtration, low temperature (50 DEG C or less dryings) is 3 hours dry, obtains volatile oil clathrate compound, spare；Extraction is waved
Aqueous solution filtration after hair oil, filtrate merge with above-mentioned decocting liquid, and it is the clear of 1.05~1.10 (80 DEG C) to be concentrated into relative density
Cream, spray drying, the powder that gets dry extract are spare.Dried cream powder adds soluble starch, appropriate Steviosin, mixing to pelletize, dry, whole grain, etc.
Amount is incrementally added above-mentioned beta-CD inclusion, mixing, be made 1000g to get.
Comparative example：Medicine preparation
In the ratio of embodiment 1 by Rhizoma Chuanxiong, the root of Dahurain angelica, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae, windproof, the medicinal water extract of asarum Six-element, that is, add water
It decocts secondary, for the first time plus 8 times of amount water, decocts 1.5 hours, second plus 6 times of amount water, it decocts 1 hour, decocting liquid filtration, filtrate
Merge, obtains aqueous extract；8 times of amount water, steam distillation are added to extract volatile oil 2.5 hours, waved both peppermint, schizonepeta
Hair oil and aqueous extract (filtration) two parts；Each Aqueous extracts of gained are merged, it is 1.12-1.16 (80 DEG C) to be concentrated into relative density
Medicinal extract, be spray-dried (230 DEG C of intake air temperature, 110 DEG C of air outlet temperature), obtain extract powder；Gained volatile oil and suitable
Lactose, the dextrin (the two is with 1: 1 ratio use of weight ratio) of amount are added in gained extract powder, prepare particle, per 4g particle phases
When in 1.2g Ligusticum chuanxiong Horts.
The parameters and medicinal effects of 1 product of embodiment and comparative product are investigated below.
(1) recovery rate of menthol
Peppermint and schizonepeta will be mixed with 2 to 1, is that 3kg feeds intake with total medicinal material amount, input volatile oil extractor (Wuhan
Pharmaceutical machine Co., Ltd, 200L) in carry out volatile oil extraction, collect, statistics volatile oil extracting amount, gas chromatography is used in combination
Assay is carried out to the menthol of gained each time, calculates menthol recovery rate.The recovery rate calculation formula of menthol is as follows：
Menthol content * peppermint medicinal materials in menthol content * volatilizations oil yield/peppermint in menthol recovery rate=volatile oil
Inventory * 100%
It is 201.4330mg/100g that experiment, which measures menthol content in peppermint,.Test result is as shown in table 1.
| Serial number | Amount of water (again) B | Extraction time (h) C | Menthol recovery rate |
| 1 | 4 | 6 | 55.7% |
| 2 | 5 | 4 | 67.9% |
| 3 | 6 | 5 | 61.3% |
As it can be seen from table 1 amount of water and extraction time have a significant impact the recovery rate of peppermint oil.When add 5 times amount
When water is with extracting 4 hours, obtained recovery rate is highest.This extraction time is short, obtains higher yield instead, is imaginary
Less than.
(2) inclusion rate of menthol
By the parameter in table 2, β-CD is taken to be dissolved in the water, and stir, heat in magnetic stirring apparatus, and set temperature.
(or being added without) absolute ethyl alcohol (a certain amount of) is added in appropriate volatile oil, when β-CD are completely dissolved temperature and reach control temperature, delays
It is slow to be added in magnetic stirring apparatus, it persistently stirs and keeps temperature parameter.After including a period of time, stop heating, stirring, it is cooling,
Filtering.It will filtering gained inclusion compound low temperature drying.
Peppermint schizonepeta extraction gained volatile oil is taken, the content for first measuring menthol in volatile oil is 381.66mg/ml, is carried out
After inclusion, the content of menthol in inclusion compound is detected with gas chromatography, inclusion rate calculation formula is as follows：
Menthol contains in menthol content * inclusion compounds total weight/volatile oil total weight * volatile oil in inclusion rate=inclusion compound
Amount * 100%
2 inclusion essential oil test result data of table
It can be seen from the above result that clathrate process used by serial number 1 respectively compares the inclusion rate of menthol far above other
Example.
(3) stability of menthol
Reference《Provisions for new drugs approval》Requirement under Chinese medicine stability test item, by Chuan Xiong Tea particle in commercially available back item
Under part, using accelerated test and long term test method, menthol study on the stability comparative study is carried out.
1, test method
Accelerated test：With reference to the requirement under stability test item, using reserved sample observing method, take using Key works Drug packing use of aluminizing
The Chuan Xiong Tea particle or inclusion compound (embodiment 1 and comparative example) of composite film packaging in right amount, in 40 DEG C ± 2 of temperature
DEG C, place 6 months under conditions of relative humidity 75% ± 5%, monthly investigate in 1,2,3,6 primary, carried out with 0 month testing result
Compare, the results are shown in Table 3.
Long term test：The river packed using aluminizer is taken using reserved sample observing method with reference to the requirement under stability test item
Rhizome of chuanxiong tea tune particle or appropriate inclusion compound, in 18 DEG C ± 2 DEG C of temperature (because in room temperature preserving item in view of menthol thin-layer chromatography spot
Variation under part selects the shady and cool condition preserved to carry out stability test), place 24 under conditions of relative humidity 60%+10%
A month, at the 3rd, 6,9,12,18,24 month, monthly examination was primary；It is compared with 0 month testing result.
2, assay method
This product particle 4g (or inclusion compound takes 0.1g) is taken, it is finely ground, it sets in conical flask with cover, add diethyl ether 20ml, and close plug shakes
It shakes, is ultrasonically treated 20 minutes in ice bath, filtered, filtrate is waved to about 1ml, as test solution.Separately take menthol (i.e. peppermint
Alcohol) appropriate reference substance, add ethyl alcohol that solution of every 1ml containing 0.5mg is made, as a contrast product solution.According to thin-layered chromatography (middle traditional Chinese medicines
One annex VI B of allusion quotation version in 2010) experiment, each 10 μ l of above two solution are drawn, are put respectively on same silica gel g thin-layer plate,
With toluene-ethyl acetate (17: 3) for solvent, it is unfolded, takes out, dry, spray is dried with 5% vanillin-sulfuric acid solution, at 105 DEG C
It is clear to spot development.In test sample chromatography, on position corresponding with reference substance chromatography, the spot of same color is shown.
3, test result
Accelerated test：Embodiment 1 places 6 months under conditions of 40 DEG C+2 DEG C of temperature, relative humidity 75% ± 5%, 0,
1,2,3,6 months on position corresponding with reference substance chromatography, detect same color spot, show said preparation stablize.Than
Compared with the spot that example product can detect same color at 0,1 month, 2 months whens, are not detected.Concrete outcome see the table below 3.
Long term test：Embodiment 1 is placed 24 months under conditions of 18 DEG C ± 2 DEG C of temperature, relative humidity 60%+10%,
0,3,6,9,12,18,24 months on position corresponding with reference substance chromatography, detect same color spot, show the system
Agent is stablized.Comparative example product was not detected at 6 months.
(4) antipyretic-antalgic anti-inflammatory effect compares
1, test method
Influence (colouring) to mouse vola pedis sweat secretion：
Kunming mice 40,18~22g of weight is taken, female is randomly divided into five groups, i.e. blank group, embodiment 1, comparative example,
Every group 10.6d is administered in continuous gavage, one time a day.Administered volume is 10mL/kg, and blank group gives isometric physiological saline,
Other groups of dosages are shown in Table 4.It after the last administration by mouse chloral hydrate anesthesia, faces upward position with rubber band and fixes, after exposure is double
Limb.Absolute ethyl alcohol is dipped after to administration with cotton swab when 30min lightly to wipe foot plantar dirt and original sweat away, then with dry cotton
Label are dried.Then skin of sole of foot coat with the high Yuan Shi reagent As liquid in field-, after abundant drying, then it is very thin coat B liquid, then
It with the dense degree of 1 mouse left footpad portion darkviolet colored spots (i.e. sweat point) of stereoscopic sem observation and is commented every 10min
Point, observe 3 times altogether, respectively 10,20, sweat point dense degree in 30min (start to observe timing).Standards of grading：Lossless point
Occurs 1 point；There is fragmentary sparse sweat point 1 minute；Sweat point occurs more and is distributed more close 5 minutes；Sweat point pole is more and is linked to be piece 10
Point, it the results are shown in Table 4.
The influence of Dichlorodiphenyl Acetate induced mice writhing response：
Kunming mice 40,18~22g of weight is taken, female is randomly divided into 4 groups, i.e. blank group, embodiment 1, comparative example,
Every group 10.Continuous gavage is to 6d, one time a day.Administered volume is 10mL/kg, and blank group gives isometric physiological saline,
He organizes dosage and is shown in Table 5.Fasting 12h before last dose, after 3min is administered, every mouse peritoneal injects Fresh
0.8% acetum (is calculated) by 0.1mL/10g, and the time for starting writhing occur after record mouse injection acetum is (latent
Phase) and 15min in there is writhing response number (there is abdomen indent in "S" shape with mouse, trunk and hind leg uphold crawling
Deng hips up is writhing response), it the results are shown in Table 5.
Anti-inflammatory effect：
With Freund's complete adjuvant (FCA) induced rat arthritis model, Wista rats 40 are taken, are randomly divided into 4 groups, point
Group and administration are shown in Table 6.Model control group fills normal saline, and experiment each group distinguishes gastric infusion, 1 time a day, continuous 7 days.
It is in 60min after the last administration, plantar intracutaneous injection FCA0.05ml causes after each group Rat Right is scorching, 6h, 2d, 4d, 8d points after Yu Zhiyan
The right metapedes ankle-joint perimeter for not measuring every rat with tape observes and records the difference of right metapedes ankle-joint perimeter before and after causing inflammation
As swelling, and carry out statistical procedures.It the results are shown in Table 6.
2, statistical method：
Each group experimental data uses 17.0 statistical softwares of SPSS, and measurement data data are with mean ± standard deviationIt indicates,
Using one-way analysis of variance (ANOVA), compares examined using t two-by-two.It is that difference is statistically significant with P ＜ 0.05.
3 results
The influence of 3.1 pairs of mouse vola pedis sweat secretions
Table 4 the results show that compared with blank group, embodiment 1 be painted with 10 after the high Yuan Shi reagents in field-, 20,30min it is each
Time point can dramatically increase mouse toes portion sweat dot density (P ＜ 0.01).Compared with blank group, comparative example, which has, increases sweat
The trend of secretory volume, but no significant difference (P ＞ 0.05).
4 Chuan Xiong Tea Granules on Mouse vola pedis sweat secretion of table effect scoring (N=10)
Note：Compared with blank group,*P ＜ 0.05,**P ＜ 0.01
The influence of 3.2 Dichlorodiphenyl Acetate induced mice writhing responses
For table 5 the results show that compared with blank group, embodiment 1 can significantly extend the latent of acetic acid induced mice writhing response
Phase (P ＜ 0.01), and substantially reduce the writhing number in mouse 15min (P ＜ 0.01).In terms of incubation period influence, with blank
Group compares, and comparative example difference is not statistically significant (P ＞ 0.05).In 15min in terms of writhing number, comparative example mouse writhing
Number has reduction (P ＜ 0.05) to a certain extent.
5 Chuan Xiong Tea particle Dichlorodiphenyl Acetate induced mice writhing response of table influence (N=12)
Note：Compared with blank group,*P ＜ 0.05,**P ＜ 0.01
3.3 anti-inflammatory effect：
Table 6 is the results show that each group causes 6h no significant differences compared with blank control group after inflammation, embodiment 1, aspirin group
There is obvious inhibiting effect to paw swelling in 2d, 4d, 8d.Embodiment 1 and aspirin group no significant difference (P ＞
0.05).Comparative example antiphlogistic effects are markedly less than aspirin group, and difference is statistically significant (P ＜ 0.05).
The lesion of 6 Chuan Xiong Tea granules in rats adjuvant-induced arthritis of table influence (N=10)
Note：Compared with blank group,*P ＜ 0.05,**P ＜ 0.01, compared with aspirin group, Δ P ＜ 0.05
In summary it is found that the antipyretic-antalgic antiphlogistic effects of 1 produced product of embodiment are substantially better than comparative example.
Claims (5)
1. a kind of clathrate process of volatile oil, which is characterized in that the volatile oil ethyl alcohol by peppermint and schizonepeta extraction gained is point
Powder beforehand dilution, is then included with beta-cyclodextrin；Wherein the ratio between volume of volatile oil and ethyl alcohol is 1: 3~1: 5, volatilization
The mass ratio of oil and beta-cyclodextrin is 1: 5~1: 8, includes 1.5~2.5h of time, includes 30~40 DEG C, 50 DEG C or less of temperature
Dry 3~5h.
2. clathrate process as described in claim 1, which is characterized in that the ratio between volume of volatile oil and ethyl alcohol is 1: 4, volatile oil
Mass ratio with beta-cyclodextrin is 1: 8, includes time 2h, includes 40 DEG C of temperature, 50 DEG C or less dry 3h.
3. clathrate process as described in claim 1, which is characterized in that the temperature of the drying is 40~50 DEG C.
4. clathrate process as described in claim 1, which is characterized in that the volatile oil be by peppermint and schizonepeta by 2: 1 matter
Amount through steam distillation as mixing medicinal material than extracting to obtain.
5. clathrate process as claimed in claim 4, which is characterized in that the technique of steam distillation extraction is：With 3~5
The water of times quality distills 3~4 hours.
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| CN107811081A (en) * | 2017-10-20 | 2018-03-20 | 刘青亚 | A kind of production method of peppermint tea chewable tablet |
| CN116173092A (en) * | 2022-11-28 | 2023-05-30 | 黑龙江森工药业有限责任公司 | Rhododendron dauricum oil clathrate compound, and preparation method and application thereof |
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| CN108478626A (en) | 2018-09-04 |
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