CN108524583A - The preparation method of radix stellariae dichotomae heat-clearing active component - Google Patents
The preparation method of radix stellariae dichotomae heat-clearing active component Download PDFInfo
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- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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Abstract
The preparation method of radix stellariae dichotomae heat-clearing active component is extracted 3 times by by radix stellariae dichotomae pulverizing medicinal materials, being extracted with a concentration of 75% ethyl alcohol, extracts 2h every time, merge extracting solution, be concentrated under reduced pressure into no alcohol taste, be subsequently placed in drying box dry, obtained radix stellariae dichotomae medicinal extract；By radix stellariae dichotomae medicinal extract with hot water dissolving, different solvents petroleum ether, ethyl acetate, extracting n-butyl alcohol is used to obtain butanol extraction liquid, then butanol extraction liquid is concentrated under reduced pressure successively, be subsequently placed in drying box dry, the effective heat-clearing position of radix stellariae dichotomae is made.The constituents extraction of effective heat-clearing in radix stellariae dichotomae is come out, the problem that active ingredient is lost in or goes bad in traditional decoction application method is avoided, improves the utilization rate of radix stellariae dichotomae, so that the heat-clearing of radix stellariae dichotomae is acted on and preferably played.
Description
Technical field
The present invention relates to the preparation method technical fields of effective ingredient in Chinese, and in particular to radix stellariae dichotomae heat-clearing active component
Preparation method.
Background technology
Radix stellariae dichotomae cures mainly clearing heat and cooling blood, consumptive disease hectic fever due to yin, deficiency of Yin chronic malaria, and the lean heat of children is thin thin.It is for oral administration, decoction, 1~3 money；Or
Enter ball, dissipate and match Radix picrorrhizae, removes abnormal heat；With turtle shell, clearing away deficiency-heat；With southern peppermint, pungent relieve heat temperature；With sweet wormwood, it is apt to the saturating network of heat-clearing.Mesh
Before, it is more coarse to the utilization of radix stellariae dichotomae, according only to《Compendium of Materia Medica》、《Sheng Nong's herbal classic》The pharmacopeia of equal Chinese medicines, is placed in Chinese medicine
It is applied by traditional decoction method in formula, although which can play the heat-clearing effect of radix stellariae dichotomae, for a long time
High temperature decoction process in will necessarily make in Chinese medicine the loss of active ingredient or rotten, i.e., utilization rate is relatively low, cannot give full play to
Its drug effect.
Invention content
By in consideration of it, it is necessary to explore a kind of preparation side for the radix stellariae dichotomae heat-clearing active component can make full use of drug effect
Method.
The preparation method of radix stellariae dichotomae heat-clearing active component, includes the following steps：
Step S1：It is 100 mesh by radix stellariae dichotomae pulverizing medicinal materials, is extracted with a concentration of 75% ethanol solution, the solid-liquid ratio of extraction
It is 10：1, it extracts 3 times, extracts 2h every time, merge extracting solution, be concentrated under reduced pressure into no alcohol taste in 60 DEG C, be subsequently placed in 60 DEG C of dryings
It is dry in case, obtain radix stellariae dichotomae medicinal extract；
Step S2：By radix stellariae dichotomae medicinal extract hot water dissolving, obtained radix stellariae dichotomae solution, successively with different solvents petroleum ether, second
Acetoacetic ester, extracting n-butyl alcohol, radix stellariae dichotomae solution are 1 with different solvents extraction volume ratio：1, by obtained butanol extraction liquid in
70 DEG C of reduced pressures are subsequently placed in 60 DEG C of drying boxes dry, obtained radix stellariae dichotomae n-butanol portion medicinal extract, as radix stellariae dichotomae heat-clearing
Active component.
Preferably, in the step S1, ethanol extract uses Rotary Evaporators, and ethyl alcohol is recycled；The step
In rapid S2, butanol extraction liquid uses Rotary Evaporators, and n-butanol is recycled.
The preparation method of radix stellariae dichotomae heat-clearing active component provided by the invention, by being 100 mesh by radix stellariae dichotomae pulverizing medicinal materials,
It is extracted with a concentration of 75% ethyl alcohol, the solid-liquid ratio of extraction is 10：1, it extracts 3 times, extracts 2h every time, merge extracting solution, in 60 DEG C
It is concentrated under reduced pressure into no alcohol taste, is subsequently placed in 60 DEG C of drying boxes dry, obtained radix stellariae dichotomae medicinal extract.Radix stellariae dichotomae medicinal extract hot water is molten
Solution is made radix stellariae dichotomae solution, is extracted successively with different solvents petroleum ether, ethyl acetate, n-butanol successively, radix stellariae dichotomae solution with not
It is 1 with solvent extraction volume ratio：1, butanol extraction liquid is obtained, then by butanol extraction liquid in 70 DEG C of reduced pressures, then
Dry, obtained radix stellariae dichotomae n-butanol portion medicinal extract, as radix stellariae dichotomae heat-clearing active component are placed in 60 DEG C of drying boxes.This method can
Radix stellariae dichotomae heat-clearing active component is prepared, avoids in traditional decoction application method the loss of active ingredient or rotten ask
Topic, improves the utilization rate of radix stellariae dichotomae, the heat-clearing of radix stellariae dichotomae is made to act on having obtained enough performances.
Specific implementation mode
Below in conjunction with specific implementation mode, the present invention will be described in detail, so that those skilled in the art can be more preferable
Understanding advantages of the present invention.
The preparation method of radix stellariae dichotomae heat-clearing active component, includes the following steps：
Step S1：It is 100 mesh by 5kg radix stellariae dichotomae pulverizing medicinal materials, is extracted with a concentration of 75% ethanol solution, solid-liquid ratio is
10：1, it extracts 3 times, extracts 2h every time, merge extracting solution, be concentrated under reduced pressure into no alcohol taste in 60 DEG C, be subsequently placed in 60 DEG C of drying boxes
Middle drying obtains radix stellariae dichotomae medicinal extract 2396.1g.
Step S2：By radix stellariae dichotomae medicinal extract with hot water dissolving, i.e. radix stellariae dichotomae solution, different solvents petroleum ether, acetic acid are used successively
Ethyl ester, extracting n-butyl alcohol, radix stellariae dichotomae solution are 1 with different solvents extraction volume ratio：1, by obtained butanol extraction liquid in 70
It DEG C is concentrated under reduced pressure, is subsequently placed in 60 DEG C of drying boxes dry, radix stellariae dichotomae n-butanol portion medicinal extract is made, i.e. radix stellariae dichotomae heat-clearing is effective
The medicinal extract 229.9g at position.
The verification of radix stellariae dichotomae heat-clearing active component：
1. experiment material
1.1 drugs and reagent
1.1.1 drug
The dry root of radix stellariae dichotomae is purchased from pharmacy, certified products is accredited as through pharmaceutical college of Ningxia Medical University teacher Bai Changcai.Drug
Liuwei Dihuang Wan (condensed pill) is purchased from pharmacy, Beijing Tongrentang Technology Development Co.ltd. Pharmaceutical Factory's production.
1.1.2 reagent
Physiological saline, 75% ethyl alcohol, n-butanol, ethyl acetate, petroleum ether, pure water.
1.2 laboratory apparatus
RWS130 types pulverizer, DC-NSG-100 types extractor, R1002 types rotary evaporator, China of HDM500 types state constant temperature
Regulating temperature electrothermal cover, 5000ml separatory funnels, 100ml graduated cylinders, No. 12 intragastric administration on mice needles, 1ml syringes, A1 typothere electric body-temperatures
Count (35 DEG C~43 DEG C of measurement range) and BWS-3-SN type electronic scales.
1.3 experimental animal
ICR male mices, 19~21g of weight are provided by Ningxia Medical University's Experimental Animal Center.
2. experimental method
2.1 experiment packet
48 ICR male mices are randomly divided into 6 groups, every group 8, respectively blank group, model group, positive group, oil
Ether group, ethyl acetate group, n-butanol group.
It is prepared by 2.2 liquids
2.2.1 prepared by radix stellariae dichotomae liquid
Radix stellariae dichotomae medicinal material 5kg is purchased, is crushed (100 mesh), with 75% ethyl alcohol (solid-liquid ratio 10：1) it extracts, extraction 3 times, every time
2h is extracted, extracting solution is merged, 60 DEG C of heating is concentrated into no alcohol taste, and 60 DEG C of dryings obtain medicinal extract 2396.1g, and medicinal extract hot water is molten
Solution, i.e. radix stellariae dichotomae solution use different solvents petroleum ether, ethyl acetate, extracting n-butyl alcohol, radix stellariae dichotomae solution and different solvents successively
The volume ratio of extraction is 1:1, the extraction of obtain three kinds of different solvents is heated and is concentrated under reduced pressure, the extract liquor of three kinds of different solvents
Heating temperature is respectively 65 DEG C, 65 DEG C, 70 DEG C, is subsequently placed in drying in drying box, and heating temperature is 60 DEG C, obtains oil respectively
Ether position medicinal extract, ethyl acetate extract medicinal extract, n-butanol portion medicinal extract 27.5g, 49.0g, 229.9g.The clinical dosage of people is silver
Radix bupleuri medicine materical crude slice 3~10g/ days, 10~11 times of mouse dose behaviour dosage.Therefore respectively with hot water by petroleum ether and n-butanol
Extraction medicinal extract dissolving is configured to the liquid of a concentration of 0.125g/ml, and ethyl acetate extract is configured to by hot water with solubilizer dense
Degree is the liquid of 0.125g/ml, and the above liquid is set 4 DEG C of refrigerators and is saved backup.
2.2.2 prepared by Liuwei Dihuang Wan (condensed pill) liquid
Liuwei Dihuang Wan (condensed pill) liquid：Liuwei Dihuang Wan weight 1.44g per ball, 8 balls, every 8 ball are equivalent to 3g lifes
Dose.It is configured to the Liuwei Dihuang Wan suspension of 0.2g/ml with purified water, sets 4 DEG C of refrigerators and saves backup.
2.2.3 prepared by hot traditional Chinese medicine liquid
It with tag processed, rhizoma zingiberis and each 200g of Chinese cassia tree, sets in round-bottomed flask, adds 8 times of volume distilled water soaking at room temperature 1h, utilize
Electric jacket heats 135 DEG C and decocts extraction 1h, and filtrate is collected by filtration, and the remaining dregs of a decoction add 6 times of volume distilled water to continue to decoct 0.5h simultaneously
Filtering merges filtrate, 60 DEG C of heating twice and is concentrated into 300ml, obtains the liquid of 2g/ml, set 4 DEG C of refrigerators and preserve, spare.
2.3 experimental program
2.3.1 raising before experiment
48 ICR male mices are randomly divided into 6 groups, every group 8.Enough feeds and drinking water is given once daily, raises one week,
Mouse is set to adapt to experiment room environment.In 7 points of weight, amount of drinking water and anus temperature for measuring and recording each group mouse in the 7th day afternoon, raise
The hair color and active state of observation mouse during supporting.
2.3.2 modeling
Start within 8th day modeling, when daily afternoon seven is administered and Monitoring Indexes.Blank group gives physiological saline
(0.4ml//day), other each groups give hot Chinese medicine (0.4ml//day, 2g/ml), continuously gavage 20d, measure daily
Amount of drinking water, weight is measured every 5d, measures an anus temperature every 1d, and record.Each group mouse hair color and work during observation modeling
Dynamic situation of change.
2.3.3 administration
Physiological saline (0.4ml//day) is gavaged to blank group and model group afterwards for 24 hours in modeling last dose；Positive group fills
Take 2.2.2 lower Liuwei Dihuang Wan suspensions (0.4ml//day, 0.2g/ml)；Petroleum ether group gavages 2.2.1 lower radix stellariae dichotomae
Petroleum ether extraction liquid (0.4ml//day, 0.125g/ml)；Ethyl acetate group gavages 2.2.1 lower radix stellariae dichotomae ethyl acetate extractions
Taking liquid (0.4ml//day, 0.125g/ml)；N-butanol group gavages 2.2.1 lower radix stellariae dichotomae extracting n-butyl alcohol liquids
(0.4ml//day, 0.125g/ml)；Each group continuously gavages 10d, measures each group mouse amount of drinking water daily, every other day measures
Each group mouse anus temperature, and record.Treatment last measures and records each group mouse weight afterwards for 24 hours.Each group mouse during observation treatment
Hair color and activity change situation.
2.4 monitoring index
(1) weight：It is weighed with 1.2 lower electronic scales.Before modeling, after modeling, treatment after stipulated time Weighing body
Weight.1 weight is measured before modeling, measures 1 weight every 5d after modeling, 1 weight is measured after treatment.(2) amount of drinking water：Each group
7 points of mouse every afternoon measures 100ml drinking water with graduated cylinder and is placed in mouse drinking bottle, then the daily drink amount of this group of mouse is
Cylinder scale changing value adds the amount for gavaging liquid or physiological saline after for 24 hours.(3) anus temperature：It is measured 1 time before modeling；After modeling and
It was measured once every 1 day after treatment.(4) overview；Observe modeling before, after modeling and treatment after each group mouse hair color color
Pool, smooth degree and mood whether irritability etc..
2.5 data processing
Data are usedIt indicates, comparison among groups variance analysis, statistical analysis is completed with 18.0 statistical softwares of SPSS.
3. result
3.1 each group mouse modelings it is forward and backward and treatment after changes of weight
As shown in table 1, after modeling, each group mouse weight increases and slows down in addition to blank group, and difference is compared with blank group,
There are significant difference (P<0.05)；After treatment, model group has significant difference (P compared with blank group<0.05)；N-butanol group
Body weight increase is apparent, with significant difference (P compared with model group<0.05), there was no significant difference compared with blank group (P>
0.05)；Positive drug group weight gain value is also more than model group (P<0.05)；Petroleum ether group is with ethyl acetate group compared with model group
There was no significant difference (P>0.05).
Before 1 each group modeling of table, after modeling and treatment after changes of weight (g)
Compared with blank group：①P<0.05,③P>0.05；Compared with model group：④P<0.05,⑤P>0.05
3.2 each group mouse modelings it is forward and backward and treatment after anus temperature change
As shown in table 2, after modeling, each group mouse anus temperature rises in addition to blank group, ascensional range (difference) and blank group
Compare, difference all has conspicuousness (P<0.05)；After treatment, model group has significant difference (P compared with blank group<0.05)；
N-butanol group anus temperature, which declines, is more than model group (P<0.05), compared with blank group
There was no significant difference (P>0.05)；Positive group has significant difference (P compared with model group<0.05), with blank group
Compared to there was no significant difference (P>0.05)；Petroleum ether group, ethyl acetate group there was no significant difference compared with model group (P>0.05).
Before 2 each group mouse modeling of table, after modeling and treatment after anus temperature temperature change (℃)
Compared with blank group：①P<0.05,③P>0.05；Compared with model group：④P<0.05,⑤P>0.05
3.3 each group mouse modelings it is forward and backward and treatment after amount of drinking water change
As shown in table 3, each group mouse amount of drinking water obviously increases in addition to blank group after modeling, difference and blank group phase
Than having significant difference (P<0.05)；After treatment, model group has significant difference (P compared with blank group<0.05)；Positive fourth
Alcohol group amount of drinking water significantly reduces, and has significant difference (P compared with model group<0.05), poor without conspicuousness compared with blank group
Different (P>0.05)；Positive group of there was no significant difference compared with blank group (P>0.05)；Petroleum ether group and ethyl acetate group amount of drinking water
Variation there was no significant difference compared with model group (P>0.05).
Before 3 modeling of table, after modeling and treatment after amount of drinking water variation (ml)
Compared with blank group：①P<0.05,②P>0.05；Compared with model group：③P<0.05,④P>0.05
3.4 overview
Each group mouse hair color is smooth before modeling and neat and tidy, mouse are emotionally stable；It is other in addition to blank group after modeling
Each group mouse shows to become thin, hair color is dull, dirty and messy, mood is irascible and the phenomenon that baiting mutually；After treatment, n-butanol group with
Positive group mouse hair color is without larger difference compared with blank group, and neat and tidy, without irascible phenomenon, appetite increases, and body weight increase adds
Soon；And petroleum ether group and ethyl acetate group mouse hair color are intense darkness without light, the bodily form is become thin, and mood is irascible.
4. conclusion
In summary to the monitoring of the indexs such as amount of drinking water, body temperature, weight and hair color, analysis is understood：The n-butanol of radix stellariae dichotomae
Extraction liquid can be substantially reduced the anus temperature and amount of drinking water of yin asthenia generating intrinsic heat mouse, and the body weight increase of mouse is made to accelerate, and make mouse
Hair color, mood and active state restore normal.Therefore think that the extracting n-butyl alcohol position of radix stellariae dichotomae is the active component of its heat-clearing.
Claims (2)
1. the preparation method of radix stellariae dichotomae heat-clearing active component, which is characterized in that include the following steps：
Step S1：It is 100 mesh by radix stellariae dichotomae pulverizing medicinal materials, is extracted with a concentration of 75% ethanol solution, solid-liquid ratio 10：1, extraction 3
It is secondary, 2h is extracted every time, merges extracting solution, no alcohol taste is concentrated under reduced pressure into 60 DEG C, is subsequently placed in drying in 60 DEG C of drying boxes, is obtained silver-colored
Radix Bupleuri extractum；
Step S2：By radix stellariae dichotomae medicinal extract hot water dissolving, obtained radix stellariae dichotomae solution, then gradually with different solvents petroleum ether, second
The volume ratio of acetoacetic ester, extracting n-butyl alcohol, radix stellariae dichotomae solution and different solvents extraction is 1:1, the butanol extraction liquid that will be obtained
In 70 DEG C of reduced pressures, dry, obtained radix stellariae dichotomae n-butanol portion medicinal extract is subsequently placed in 60 DEG C of drying boxes, and as radix stellariae dichotomae is clear
Hot active component.
2. the preparation method of radix stellariae dichotomae heat-clearing active component as described in claim 1, it is characterised in that：In the step S1,
Ethanol extract uses Rotary Evaporators, and ethyl alcohol is recycled；In the step S2, butanol extraction liquid is steamed using rotation
Instrument is sent out, n-butanol is recycled.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113952372A (en) * | 2021-11-17 | 2022-01-21 | 宁夏大学 | Composition for treating atopic dermatitis and application thereof |
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- 2018-06-28 CN CN201810684998.XA patent/CN108524583A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101628021A (en) * | 2009-03-13 | 2010-01-20 | 江西本草天工科技有限责任公司 | Preparation method of effective part of radix bupleuri and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113952372A (en) * | 2021-11-17 | 2022-01-21 | 宁夏大学 | Composition for treating atopic dermatitis and application thereof |
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Application publication date: 20180914 |