CN104127463B - A kind of Echinacea Purpurea Herb P.E and its preparation method and application - Google Patents
A kind of Echinacea Purpurea Herb P.E and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to a kind of Echinacea Purpurea Herb P.E and its preparation method and application, the extract contains the ingredient of following weight percent：Phenolic Compounds content is higher than 12%, and Echinacea polyoses content is higher than 20%, and the content of Cichoric acid is higher than 4%.Extract provided by the invention, which generates mouse hemolytic antibody to have, is obviously promoted effect, illustrates that the medicine can enhance humoral immunity, and effect is better than the prior art.
Description
Technical field
The present invention relates to Chinese medical extracts, and in particular to a kind of Echinacea Purpurea Herb P.E and its preparation method and application.
Background technology
Echinacea (Echinacea) is a kind of Echinacea purpurea number plant for originating in North America and southern Canada, the platymiscium
8 kinds and several mutation are shared, there are three kind, purple coneflower (Echinacea currently as drug development main
Purpurea, i.e., usually said Echinacea), narrow leaf Echinacea (Echinacea augustifolia) and white Echinacea
(Echinacea pallida)。
Echinacea is a kind of immunopotentiating agent and immunomodulator for being now subjected to international most attention, is world-famous
" immune " herbal medicine, have the function of outstanding anti-infective with promoting immunity, its extract and the U.S. formulations sold E Ju herbal medicine
5 before market sale ranking, by very big concern both domestic and external.
And currently, the extraction of Echinacea has following method, such as：
CN03134457.7 (Publication No. CN1473602) includes alcohol reflux extraction, removal of impurities, concentration, is dried in vacuo, on
Column and etc..It has the following disadvantages：1. extracting solution directly carries out micro-filtration processing, it is be easy to cause microfiltration membranes blocking, and raw
It is low to produce efficiency, is not suitable for producing greatly.2. concentration gained medicinal extract, is dried under reduced pressure, since the polyphenol components such as Cichoric acid are heat-resisting
Property it is bad, it is prolonged heated to cause Cichoric acid loss more, cause witloof acid content in finally obtained extract not high.
The preparation method of CN200610031845.2 (Publication No. CN1957961A) Echinacea Purpurea Herb P.E, what raw material used
It is the Echinacea herb of fresh state, it is extracted, it is concentrated to give Echinacea Purpurea Herb P.E.This method has the following disadvantages：1. making
Standby technique is using Echinacea fresh medicine material as research object, although Echinacea fresh goods witloof acid content is higher, Echinacea Purpurea Herb P.E
Production is subject to seasonal restrictions, and the medicine source problem of Echinacea Purpurea Herb P.E limits its industrialized production.2. its technique productions is mainly
Using witloof acid content as index, and in medicinal material play immunization polysaccharide component its do not consider, cause medicinal material to a certain degree
The waste of resource.3. preparation process Chinese medicine timber-used high concentration ethanol extracts 2 times, it is adsorbed with a large amount of ethyl alcohol in the dregs of a decoction, and has no place
The Echinacea Purpurea Herb P.E cost of reason, production is higher.
CN200610061847.6 (Publication No. CN101032541A) discloses a kind of Echinacea Purpurea Herb P.E and its preparation
Method and content assaying method, this method have the following disadvantages：1. extraction amount of alcohol is larger, ethyl alcohol consumption is big, at
This is higher.Through experimental study, its technique witloof acid transfer rate is relatively low, in 40-50% or so.2. Echinacea prepared by its technique carries
It takes witloof acid content in object relatively low, and index is single, does not embody total polyphenols and total starches constituents content transfer case.
The Echinacea Purpurea Herb P.E that CN201210216720.2 (Publication No. CN102716164A) is provided is using alkaline second
Alcoholic solution and lysozyme carry out extraction twice to Echinacea medicinal material and obtain；In product：Polyoses content >=21.50%, polyphenol content
>=8.10%, witloof acid content >=5.00%.It has the following disadvantages：It is extracted and is held with pH=12 calcium hydroxide ethanol solutions
The polyphenol components such as calcium ion and Cichoric acid chelating is easily caused, forms precipitation insoluble matter, and chrysanthemum is easily caused in high-temperature alkaline environment
The fracture of ester bond contained by lettuce acid, causes the destruction of the ingredients such as Cichoric acid, and actually by the alkali alcohol extracting method of the document, in
The tolerant content that document restriction is not achieved.
At present, it is considered that the active constituent of Echinacea is mainly Caffeic acids derivative and phenolic acid compound, more
Sugar and glycoprotein, alkylamide constituents, flavonoids etc..Polyphenol components be it is all the time putative have Immune-enhancing effect,
Anti-inflammatory, antivirus action substance, wherein Cichoric acid are used to evaluate the quality of Echinacea medicinal material as a kind of index ingredient.And
Echinacea polysaccharide and sugar-protein compound also can stimulating expression of macrophage phagocytic function, stimulate T lymphopoiesis, hemolysis plaque
Experiments have shown that plaque number can be obviously increased, thus humoral immune function can be significantly increased, function can be more with astragalus polyose, mushroom
A variety of polysaccharide constituents such as sugar compare favourably.
Therefore, polyphenol and polysaccharide two major classes active constituent should be retained for Echinacea Purpurea Herb P.E, is rationally provided using medicinal material
Source, the effect of giving full play to anti-inflammatory Echinacea, promoting immunity.
Presently commercially available Echinacea Purpurea Herb P.E is mostly using total phenol and witloof acid content as index, mostly yellow greenish powder, price compared with
Height, its contained polysaccharide constituents is relatively low after measured, is less than 5%, while the commercially available Echinacea for having no mark Echinacea polyoses content
Extract.
Invention content
The object of the present invention is to provide a kind of Echinacea Purpurea Herb P.Es.
A kind of Echinacea Purpurea Herb P.E provided by the invention, extract contain the ingredient of following weight percent：Echinacea
Polyphenol content is higher than 12%, and Echinacea polyoses content is higher than 20%, and the content of Cichoric acid is higher than 4%.
Specifically, the extract contains the ingredient of following weight percent：Phenolic Compounds 12.1-14.4%, purple cone
Chrysanthemum polysaccharide 21.1-25.8%, Cichoric acid 4.11-5.12%.
Preferably, the ingredient of following weight percent is contained in the extract：Phenolic Compounds 12.1-12.8% is purple
Bore chrysanthemum polysaccharide 21.5-25.8%, Cichoric acid 4.11-4.72%.
Further preferably, the ingredient of following weight percent is contained in the extract：Phenolic Compounds 12.8%, purple cone
Chrysanthemum polysaccharide 25.8%, Cichoric acid 4.11%.
The present invention also provides the preparation methods of above-mentioned Echinacea Purpurea Herb P.E, and this approach includes the following steps：
1) Echinacea crushes, and sieves for subsequent use；
2) ethanol solution refluxing extraction of the Echinacea powder for obtaining step 1) containing acid, wherein concentration of alcohol are 60-
95%, the dregs of a decoction and filtrate are collected in filtration, and filtrate is concentrated to give medicinal extract, spare；
3) aqueous solution temperature extraction of the dregs of a decoction containing alkali that step 2) obtains is taken, filters, obtains filtrate and the dregs of a decoction, filtrate concentration
Medicinal extract is obtained, it is spare；
4) merge the medicinal extract of step 2) and step 3) concentration, clear liquid is collected in separation, dry, obtains Echinacea Purpurea Herb P.E.
Preferably, it the described method comprises the following steps：
1) Echinacea crushes, and crosses -24 mesh of 10 mesh sieve, spare；
2) step 1) Chinese drugs powder is taken, 7-10 times of Echinacea powder weight is added to measure the acid containing 0.1%-0.5% of volume
60%-85% ethanol solutions, refluxing extraction 1.5-3.0 hours, filtration obtain filtrate and the dregs of a decoction, filtrate decompression is concentrated into 60 DEG C of surveys
Determine the medicinal extract that relative density is 1.06-1.12, it is spare；
3) by the gained dregs of a decoction in step 2), add the water of 5-7 times of alkali containing 0.05%-0.15% for measuring volume of Echinacea powder weight
Solution, 60-90 DEG C of temperature extraction take 0.5-2.0 hours, filter, obtain filtrate and the dregs of a decoction, the dregs of a decoction discard, and filtrate decompression is concentrated into 60 DEG C
The medicinal extract that relative density is 1.06-1.08 is measured, it is spare；
4) merge gained medicinal extract in step 2) and step 3), carry out centrifugal treating, clear liquid is dried, obtain Echinacea extraction
Object.
Further preferably, it the described method comprises the following steps：
1) Echinacea crushes, and crosses 15 mesh sieve, spare；
2) step 1) Chinese drugs powder is taken, 70% ethyl alcohol containing 0.2% citric acid of 8 times of amount volumes of Echinacea powder weight is added
Solution, refluxing extraction 2.0 hours, filtration obtain filtrate and the dregs of a decoction, and it is 1.06- that filtrate decompression, which is concentrated into 60 DEG C and measures relative density,
1.12 medicinal extract, it is spare；
3) by the gained dregs of a decoction in step 2), add 0.1% sodium carbonate liquor of 6 times of amount volumes of Echinacea powder weight, 75 DEG C of temperature
Extraction takes 1.0 hours, filters, obtains filtrate and the dregs of a decoction, and the dregs of a decoction discard, and relative density is measured when filtrate decompression is concentrated into 60 DEG C and is
1.06-1.08 medicinal extract, it is spare；
4) merge gained medicinal extract in step 2) and step 3), carry out high speed tubular type centrifugal treating, clear liquid and precipitation are obtained, by institute
Clear liquid spray drying is obtained, Echinacea Purpurea Herb P.E is obtained.
In the above method：
The Echinacea is the herb of Echinacea or one or more of mixtures of stem, leaf, flower, root.
Acid in the step 2) is the one or more of concentrated hydrochloric acid, phosphoric acid, glacial acetic acid, citric acid；
Alkali in the step 3) is one kind or several of sodium carbonate, sodium bicarbonate, sodium hydroxide, potassium hydroxide, concentrated ammonia liquor
Kind；
The ethyl alcohol of the 60-85% containing sour 0.1-0.5% is that the acid of 0.1-0.5g is dissolved in a concentration of 60- of 100ml
In 85% ethyl alcohol.
It is separately made or by extract and pharmacy by said extracted object the present invention also provides the preparation of the object containing said extracted
Upper acceptable carrier is made.
The preparation is micropill preparation, powder, syrup, oral solution, tincture, tablet, granule, capsule or ointment.
The auxiliary material is selected from sucrose, dextrin, ethyl alcohol, microcrystalline cellulose, starch, superfine silica gel powder, potassium sorbate, bisulfite
One or more mixing in sodium, magnesium stearate, stearic acid, glycerin monostearate, potassium carbonate, triethanolamine or glycerine
Object.
The present invention also provides said extracted objects or its preparation to prepare for common infection or wound, flu, tonsillotome
Application in the drug of inflammation, the infection of the upper respiratory tract, abscess of throat etc. and enhancing function of immune system.
Echinacea Purpurea Herb P.E provided by the invention has the following advantages：
1, compared with prior art, the present invention will add the acidic ethanol of appropriate concentration to carry out first after Echinacea pulverizing medicinal materials
Extraction, primarily directed to polyphenol components contained in medicinal material, polyphenol components are usually and exist with its esters in crude drug, add
After entering appropriate amount of acid, polyphenol components are in free state, and lipophilicity enhancing is soluble in high concentration ethanol, than individually using a certain concentration
Ethyl alcohol extraction recovery rate wants high, and after filtration, the dregs of a decoction add the buck temperature extraction of appropriate concentration to take, contained in medicinal material
Polysaccharide constituents add certain density alkali in aqueous, plant cell wall broken wall, polysaccharide constituents can be made to be more easy to leach, carry
It takes effect more preferable, while controlling Extracting temperature, it is ensured that avoid temperature is excessively high to cause the disconnected of polysaccharide sugar chain in extraction process
It splits, ensure that the space structure of polysaccharide constituents, and then ensure that the validity of extract, while the second pan-fried plus buck extraction,
The ethanol solution that first boils medicine material absorption can be covered and be washed out, and then recycle ethyl alcohol, save cost.Summarizing advantage is：
1. rational technology, the active ingredient rate of transform is high, is convenient for quality control.After Echinacea pulverizing medicinal materials, the first pan-fried acid adding
Property ethanol solution extract polyphenol components, recovery rate is high, and second decocts plus the extraction of alkali temperature takes polysaccharide constituents, breaking-wall cell, polysaccharide
Ingredient leaches complete.
2. polyphenol, polysaccharide and witloof acid content are high in extract, at low cost, good drug efficacy.Polyphenol contains in extract of the present invention
Amount is higher than 12%, and polyoses content is higher than 20%, and the content of Cichoric acid is higher than 4%.
2, compared with prior art, in method provided by the invention：
1) pH value of ethanol solution：Ethanol solution containing sour 0.1-0.5%, pH value is indefinite because variety classes it is sour,
The ethanol solution of its 0.1-.05% of various concentration its pH value is different, in the prior art pH value be less than or equal to 3, experiment proves that
Witloof acid content highest in the ethanol solution extraction Echinacea of pH=3.
2) difference of concentration of alcohol：A concentration of the 50% of ethyl alcohol in the prior art, the present invention in ethyl alcohol a concentration of 60-
85%, the big impurity of polarity obtained by the too low extraction of concentration of alcohol is excessively unfavorable for later-period purification；
3) ethanol extract concentrates：Alcohol extracting twice is used in the prior art, then concentrates filtrate, first by alcohol in the present invention
Carry filtrate concentration, and the present invention first with solution containing acid alcohol extraction, after extracted with aqueous alkali, therefore, cannot merge carry twice
Liquid is taken to concentrate again, it is necessary to first carry out concentration and remerge；
4) processing of the dregs of a decoction：The prior art by the dregs of a decoction again use pH value be 3 ethanol solution extract, and the present invention be then by
The dregs of a decoction are extracted with buck, the reason is that：In medicinal material, Cichoric acid is existed in the form of sodium salt, water-soluble good, is carried using acid
Cichoric acid is free before this extracts, and changes buck extraction for the second time, makes not extract complete Cichoric acid and is extracted in water at salt
Out and polysaccharide constituents can be also extracted in this step；
5) it extracts：The prior art also extracts the alcohol extract after concentration, and dehydration, the present invention does not have, the reason is that：This
Invention directly obtains extract using spray drying, need not be carried out dehydrating.Dehydration is in laboratory lab scale application
Shi Changyong；Extraction process is unrealistic in big production and is not suitable for.
In finally obtained extract, Phenolic Compounds, Echinacea polysaccharide and witloof in the extract that the prior art provides
The content of acid is less than the present invention.
3, extract provided by the invention, which generates mouse hemolytic antibody to have, is obviously promoted effect, illustrates that the medicine can increase
Strong humoral immunity, and effect is better than the prior art.
Specific implementation mode
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
The ethanol solution of the acid containing a few percent, is w/v, such as with 70% second containing 0.2% citric acid
Alcoholic solution is dissolved in 0.2g citric acids in the ethyl alcohol of 100ml a concentration of 70%.
The aqueous slkali of a concentration of 0.05%-0.15%, be by 0.05-0.15g alkali solubles in 100ml water.
Embodiment 1：The extracting method of Echinacea
1, Echinacea crushes, and crosses 15 mesh sieve, spare；
2, step 1 Chinese drugs powder is taken, 70% ethyl alcohol containing 0.2% citric acid of 8 times of amount volumes of Echinacea powder weight is added
Solution, refluxing extraction 2.0 hours, filtration obtain filtrate and the dregs of a decoction, and it is 1.12 that filtrate decompression, which is concentrated into 60 DEG C and measures relative density,
Medicinal extract, it is spare；
3, by the step 2 gained dregs of a decoction, add 0.1% sodium carbonate liquor of 6 times of amount volumes of Echinacea powder weight, 75 DEG C of temperature extractions
It takes 1.0 hours, filters, obtain filtrate and the dregs of a decoction, the dregs of a decoction discard, and filtrate decompression measures relative density when being concentrated into 60 DEG C be 1.08
Medicinal extract, it is spare；
4, merge gained medicinal extract in step 2 and step 3, carry out high speed tubular type centrifugal treating, clear liquid and precipitation are obtained, by gained
Clear liquid is spray-dried, and obtains Echinacea Purpurea Herb P.E.
Embodiment 2：The extracting method of Echinacea
1, echinacea root 10kg is taken, is crushed, 15 mesh sieve is crossed, it is spare；
2, step 1 Chinese drugs powder is taken, adds 75% ethyl alcohol containing 0.3% hydrochloric acid of 7 times of amount volumes of Echinacea powder weight molten
Liquid, refluxing extraction 1.5 hours, filtration obtain filtrate and the dregs of a decoction, and filtrate decompression is concentrated into 60 DEG C and measures the leaching that relative density is 1.07
Cream, it is spare；
3, by the gained dregs of a decoction in step 2, add 0.15% sodium bicarbonate solutions of 6 times of Echinacea powder weight amount volume, 80 DEG C
Temperature extraction takes 40 minutes, filters, obtains filtrate and the dregs of a decoction, and the dregs of a decoction discard, and filtrate decompression is concentrated into 60 DEG C of measurement relative densities and is
1.08 medicinal extract, it is spare；
4, merge gained medicinal extract in step 2 and step 3, carry out high speed tubular type centrifugal treating, obtain clear liquid and precipitation, precipitation is abandoned
It goes, the another device harvesting of clear liquid is spare；
5, centrifugation gained clear liquid is spray-dried, obtains Echinacea Purpurea Herb P.E 1.95kg (yield 19.5%).
Embodiment 3：The extracting method of Echinacea
1, Echinacea herb 10kg is taken, is crushed, 24 mesh sieve is crossed, it is spare；
2, take step 1 Chinese drugs powder, add 8 times amount containing 0.3% acetic acid 60% ethanol solutions, refluxing extraction 2.0 hours,
Filtration obtains filtrate and the dregs of a decoction, and filtrate decompression is concentrated into 60 DEG C and measures the medicinal extract that relative density is 1.08, spare；
3, by the gained dregs of a decoction in step 2,7 times of 0.05% sodium hydroxide solutions of amount, 70 DEG C of temperature extractions is added to take 1.0 hours, filter
It crosses, obtains filtrate and the dregs of a decoction, the dregs of a decoction discard, and filtrate decompression is concentrated into 60 DEG C and measures the medicinal extract that relative density is 1.08, spare；
4, merge gained medicinal extract in step 2 and step 3, carry out high speed tubular type centrifugal treating, obtain clear liquid and precipitation, precipitation is abandoned
It goes, the another device harvesting of clear liquid is spare；
5, centrifugation gained clear liquid is spray-dried, obtains Echinacea Purpurea Herb P.E 2.2kg (yield 22%).
Embodiment 4：The extracting method of Echinacea
1, Echinacea leaf, flower mixture 10kg are taken, is crushed, 15 mesh sieve is crossed, it is spare；
2, take step 1 Chinese drugs powder, add 8 times amount containing 0.2% hydrochloric acid 70% ethanol solutions, refluxing extraction 1.5 hours,
Filtration obtains filtrate and the dregs of a decoction, and filtrate decompression is concentrated into 60 DEG C and measures the medicinal extract that relative density is 1.08, spare；
3, by the gained dregs of a decoction in step 2,7 times of 0.05% sodium hydroxide solutions of amount, 70 DEG C of temperature extractions is added to take 1.0 hours, filter
It crosses, obtains filtrate and the dregs of a decoction, the dregs of a decoction discard, and filtrate decompression is concentrated into 60 DEG C and measures the medicinal extract that relative density is 1.08, spare；
4, merge gained medicinal extract in step 2 and step 3, carry out high speed tubular type centrifugal treating, obtain clear liquid and precipitation, precipitation is abandoned
It goes, the another device harvesting of clear liquid is spare；
5, centrifugation gained clear liquid is spray-dried, obtains Echinacea Purpurea Herb P.E 1.75kg (yield 17.5%).
Comparative example 1：The preparation of Cichoric acid powder
With reference to the method for the embodiment 1 of CN201210470455.0 (Publication No. CN102911056A) patent, specific side
Method is：
1) Echinacea was smashed to pieces 20 mesh sieve, the pH that the ethanol solution that mass concentration is 50% is adjusted with HCl solution is 3,
It is first 8 according to mass ratio by deployed solution and Echinacea powder：1 ratio boils extraction at being 100 DEG C in temperature
Deployed solution and Echinacea powder according to mass ratio are again 6 after filtering by 1.5h：1 ratio is boiled at being 100 DEG C in temperature
Boiling 1.5 hours, it is 1.1g/cm to mix concentration densities with first time filtrate after filtering3Solution；
2) it is 1.1g/cm by density3Concentrate and ethyl acetate according to mass ratio be 1：1.2 hybrid extractions, acetic acid second
Ester merges after extraction extract liquor respectively is added in three times, and the deionization that the pH that the extract liquor hydrochloric acid after merging is adjusted is 3 is washed
It washs primary；
3) it is 1 according to mass ratio with anhydrous sodium sulfate by the solution after washing：1.2 ratio mixed dehydration 8h, concentrates back
It receives solution and obtains Cichoric acid powder.
Experimental example 1：The detection of active ingredient in extract
Embodiment 1-4 and comparative example 1 extract provided are detected, specific detection method is：
1, Cichoric acid assay
Chromatographic condition is with system suitability using octadecylsilane chemically bonded silica as filler；Using acetonitrile as mobile phase
A, 0.1% phosphoric acid solution are Mobile phase B, and gradient elution is carried out by table 1；Detection wavelength 330nm.Number of theoretical plate is based on Cichoric acid peak
1500 should be not less than by calculating.
Table 1：Cichoric acid assay gradient elution
| Time (minute) | Mobile phase A (%) | Mobile phase B (%) |
| 0-20 | 15 | 85 |
| 20-22 | 15→40 | 85→60 |
| 22-25 | 40→15 | 60→85 |
The preparation precision of reference substance solution weighs that Cichoric acid reference substance is appropriate, adds 70% methanol that every 1ml is made containing 40 μ g
Solution to get.
The preparation of test solution takes extract fine powder about 0.1g, accurately weighed, sets in conical flask with cover, and precision is added
70% methanol 50ml, weighed weight, ultrasonic (power 250W, frequency 35kHz) are handled 30 minutes, are let cool, then weighed weight, are used
70% methanol supplies the weight of less loss, shakes up, filtration to get.
Measuring method is accurate respectively to draw reference substance solution and each 10 μ l of test solution, injects liquid chromatograph, measures, i.e.,
.
2, in extract polyphenol content assaying method
The preparation precision of reference substance solution weighs chlorogenic acid reference substance 10mg, and 40% ethanol solution is added and is diluted to 100ml.
The preparation precision of test solution weighs extract 250mg, and 40% ethanol solution water bath sonicator is added and dissolves (water-bath
Temperature is controlled at 15 DEG C or less), at room temperature 100ml is settled to the dilution of 40% ethanol solution.
Measuring method is accurate respectively to measure in 1ml reference substances and test solution to 50ml volumetric flasks, is separately added into 15ml F-
D test solutions and 7ml30%Na2CO3For test solution in the volumetric flask, edged shaking in side adds water constant volume mixing, after placing 90min, according to purple
Outside-visible spectrophotometry makees blank with blank sample solution, and absorbance is measured at 700nm wavelength.Using standard control
Method calculates polyphenol content.
3, in extract polysaccharide content assaying method：
The preparation of test solution takes extract fine powder about 20.0mg, and accurately weighed, adding water 50ml to heat makes dissolving, lets cool
After be settled in 100ml measuring bottles, mixing to get.
Glucose control product are produced in matching for standard solution, accurately weighed, add water to be configured to the solution of 0.1mg/ml, i.e.,
.
The foundation of standard curve is accurate to measure 0,0.05,0.1,0.15,0.20,0.25, the standard glucose of 0.30ml it is molten
Liquid (0.1mg/ml), adds water to mend to 0.5ml, adds 6% phenol 0.3ml, then enriching sulfuric acid 1.5ml, shakes up, and boiling water bath heats 10 points
Clock, cooling, 490nm detects absorbance, and using glucose quality as abscissa, corresponding absorbance is that ordinate draws standard song
Line obtains calibration curve equation.
Measuring method precision measures test solution 0.15ml, adds water to supply 0.5ml, 6% phenol of addition parallel with standard items
0.3ml, concentrated sulfuric acid 1.5ml, shakes up, and boiling water bath heats 10 minutes, cooling, and 490nm detects absorbance.By the extinction number of degrees of sample
Value substitutes into calibration curve equation, calculates polyoses content.
4, testing result：It is shown in Table 2
Table 2：Ingredient (weight percent %) in embodiment 1-3 extracts
| Phenolic Compounds | Echinacea polysaccharide | Cichoric acid | |
| Embodiment 1 | 12.8 | 25.8 | 4.11 |
| Embodiment 2 | 14.4 | 21.1 | 4.89 |
| Embodiment 3 | 12.1 | 21.5 | 4.72 |
| Embodiment 4 | 14.4 | 22.7 | 5.12 |
| Comparative example | 10.5 | 2.58 | 3.46 |
2 result of table is shown：The present invention is finally in Echinacea Purpurea Herb P.E obtained, and Phenolic Compounds content is higher than 12%, purple
It bores chrysanthemum polyoses content and is higher than 21%, the content of Cichoric acid is higher than 4%；Preferably, following weight percent is contained in extract
Ingredient：Phenolic Compounds 12.1-14.4%, Echinacea polysaccharide 21.1-25.8%, Cichoric acid 4.72-5.12%.
Embodiment 5：Echinacea granule
Sucrose 1200g, dextrin 40 0g, mixing, with 85% second is added in the Echinacea Purpurea Herb P.E 400g that Example 1 obtains
Alcohol is wetting agent, softwood processed, wet granulation, and drying, whole grain obtains Echinacea particle 1890g.
Embodiment 6：Echinacea pellet
Microcrystalline cellulose 100g, starch 300g, dextrin 200g is added in the Echinacea Purpurea Herb P.E 300g that Example 3 obtains,
Sucrose 100g, mixing are wetting agent with 85% ethyl alcohol, softwood processed, extrusion-spheronization pill, and drying selects ball, it is micro- to obtain Echinacea
Ball 920g.
Embodiment 7：Echinacea powder
The Echinacea Purpurea Herb P.E 800g that Example 2 obtains, be added microcrystalline cellulose 100g, superfine silica gel powder 100g, mixing,
Obtain Echinacea powder 980g.
Embodiment 8：Echinacea syrup
Sucrose 650g is taken, water 800ml heating is added to make dissolving, the Echinacea Purpurea Herb P.E 200g that embodiment 1 obtains, sorb is added
Sour potassium 3g, stirs evenly, and stands 24 hours, and filtration, filtrate adds water to 1000ml to get Echinacea syrup.
Embodiment 9：Echinacea oral liquid
The Echinacea Purpurea Herb P.E 200g that Example 2 obtains adds water 800ml, heating to make dissolving, potassium sorbate 3g is added,
Sodium hydrogensulfite 1g, stirs evenly, and stands 24 hours, and filtration, filtrate adds water to 1000ml mixings, obtains Echinacea oral liquid.
Embodiment 10：Echinacea tincture
The Echinacea Purpurea Herb P.E 100g that Example 1,2 or 3 obtains adds 50% ethanol solution 800ml, stirs evenly, quiet
It sets 24 hours, filters, filtrate adds 50% ethanol solution to 1000ml, obtains Echinacea tincture.
Embodiment 11：Echinacea piece
Echinacea particle 350g made from Example 4, is added magnesium stearate 1g, mixing, and tabletting obtains Echinacea piece 957
Piece.
Embodiment 12：Echinacea capsule
Echinacea particle 330g, encapsulated made from Example 5, obtains Echinacea capsule 982.
Embodiment 13：Echinacea capsule
Echinacea powder 330g, encapsulated made from Example 6, obtains Echinacea capsule 974.
Embodiment 14：Echinacea capsule
Echinacea pellet 330g, encapsulated made from Example 7, obtains Echinacea capsule 989.
Embodiment 15：Echinacea ointment
Stearic acid 120g, glycerin monostearate 25g, potassium carbonate 9g is taken to set in container, heating water bath continues to add to melting
Heat is to 70-80 DEG C；Separately triethanolamine 3ml, glycerine 100g, distilled water 550ml is taken to set in another container, be heated to 70-80 DEG C, delayed
It is slow to import in the oil phases such as stearic acid, it is stirring while adding, until emulsification is complete；The Echinacea Purpurea Herb P.E 200g that Example 1 obtains is taken,
It is added in the matrix of above-mentioned preparation, stirs evenly to get Echinacea ointment.
Experimental example 2：The comparison of extracting method
Contrast test 1, water carry：Echinacea is ground into coarse powder, 15 mesh sieve is crossed, weighs two parts respectively, respectively about 500g, mark
For A, B group, respectively plus water 5000g, 4000g, refluxing extraction 2 times 1.5 hours every time, extracting solution are merged, is concentrated under reduced pressure into 60
DEG C measure relative density be 1.08 medicinal extract, medicinal extract spray drying, obtain Echinacea Purpurea Herb P.E.Measure Cichoric acid, more in extract
The content of phenol and polysaccharide.
Contrast test 2, the extraction of 70% ethyl alcohol
Echinacea is ground into coarse powder, 15 mesh sieve is crossed, weighs two parts respectively, respectively about 500g, be labeled as A, B group, add respectively
70% ethyl alcohol 5000g, 4000g, refluxing extraction 2 times 1.5 hours every time, extracting solution are merged, and are concentrated under reduced pressure into 60 DEG C of measurement phases
The medicinal extract for being 1.08 to density, medicinal extract spray drying, obtains Echinacea Purpurea Herb P.E.Measure Cichoric acid, polyphenol and polysaccharide in extract
Content.
Contrast test 3,70% ethyl alcohol of 0.2% citric acid and the extraction experiment of 0.1% sodium carbonate liquor
Echinacea is ground into coarse powder, 15 mesh sieve is crossed, weighs two parts respectively, respectively about 500g, is labeled as A, B group, first decocts
70% ethanol solution 5000g of 0.2% citric acid, refluxing extraction 1.5 hours is added to filter, the dregs of a decoction add 0.1% sodium carbonate liquor
4000g80 DEG C of temperature extraction takes 1.5 hours, filters, and filtrate merges with a pan-fried extracting solution, is concentrated under reduced pressure into 60 DEG C of measurement relative densities
For 1.08 medicinal extract, medicinal extract spray drying obtains Echinacea Purpurea Herb P.E.Measure the content of Cichoric acid, polyphenol and polysaccharide in extract.
Contrast test 4,50% ethyl alcohol (adjusting pH=12 with calcium hydroxide) and the extraction experiment (reference of 1% lysozyme soln
The method of CN201210216720.2 (Publication No. CN102716164A))
Echinacea is ground into coarse powder, 15 mesh sieve is crossed, weighs two parts respectively, respectively about 500g, is labeled as A, B group, first decocts
The 50% ethanol solution 5000g with calcium hydroxide pH=12, refluxing extraction 1.5 hours is added to filter, the dregs of a decoction add 1% lysozyme molten
Liquid 4000g refluxing extractions 1.5 hours, filtration, filtrate merge with a pan-fried extracting solution, are concentrated under reduced pressure into 60 DEG C of measurement relative densities and are
1.07 medicinal extract, medicinal extract spray drying, obtains Echinacea Purpurea Herb P.E.
The content that Cichoric acid, polyphenol and polysaccharide in extract are measured according to the method that experimental example 1 provides, the results are shown in Table 3.
Table 3：Cichoric acid, polyphenol and polysaccharide component content results in Different Preparation Echinacea Purpurea Herb P.E
3 result of table is shown：In contrast test 1-4,70% ethyl alcohol and 0.1% sodium carbonate of 0.2% citric acid are only used
Each active component content highest in the extract that solution extracts.
Experimental example 3：Mouse hemolysin is tested
Further to verify the immunologic enhancement of Echinacea Purpurea Herb P.E prepared by the present invention, inventor has investigated it to small
The influence of mouse hemolysin.
1, materials and methods
1.1 experimental drug
Test medicine：Echinacea Purpurea Herb P.E is prepared according to embodiment 1-4 and comparative example 1, the Qingdao health ground limited public affairs of grace medicine company
Department provides.
Control drug：Levamisole hydrochloride-astragalus polyose soluble powder, lot number 20121013, Guangzhou and raw hall animal
Pharmaceutcal corporation, Ltd's production.
1.2 laboratory apparatus：UV-1100 types ultraviolet specrophotometer (Japanese Shimadzu).
1.3 experimental animal
Kunming mouse, male, weight 18-20g are provided by Shanghai Si Laike experimental animal responsibilities Co., Ltd.It is qualified
Card number：SCXK (Shanghai) 2007-0005
1.4 experimental method
1.4.1 the preparation of sheep red blood cell (SRBC) suspension
Sheep anticoagulation 30ml is taken, is put into centrifuge tube, with brine 3 times, each 2000rpm centrifugations,
Preceding 2 centrifugations 5min, last 1 centrifugation 10min, 10 discard supernatant liquid.Two parts of sheep red blood cell (SRBC) 3ml is taken respectively, uses physiology salt
Water is configured to 20%, 10% sheep red blood cell (SRBC) suspension respectively.
1.4.2 prepared by complement
It is derived from the serum obtained by guinea pig heart blood, by serum：20% sheep red blood cell=1：0.2 mixing, in 4 DEG C of refrigerators
30min is placed, 2000rpm centrifuges 10min, and Aspirate supernatant is spare.
1.4.3 experimental animal grouping and processing
Kunming mouse totally 90 is randomly divided into 9 groups, every group 10.Respectively 1 high, medium and low 3 dosage group of embodiment,
Embodiment 2,3,4 groups, 1 group of comparative example, positive controls and blank group.
Start to be administered within the 2nd day after grouping, 1 high, medium and low dosage group of embodiment is respectively with 2.7g/kg, 0.9g/kg, 0.3g/
The dosage of kg, by Echinacea Purpurea Herb P.E physiological saline solution, prepare containing the molten of 0.012g/ml, 0.036g/ml, 0.108g/ml
Liquid, every mouse administered volume is 250ul/10g, and administering mode is gastric infusion；1 group of embodiment 2-4 groups and comparative example are pressed
Echinacea Purpurea Herb P.E physiological saline solution is prepared into the solution containing 0.036g/ml according to the dosage administration of 0.9g/kg, it is every small
Mouse administered volume is 250ul/10g, and administering mode is gastric infusion；Positive control medicine dosage is 0.1g/kg, and method is same
On, daily timed drug administrations are primary, all equal successive administrations of administration group 2 weeks.
1.4.4 the measurement of the preparation of serum and hemolytic antibody
Terminate first 4 days in mouse administration, by a concentration of 20% sheep red blood cell (SRBC) suspension, with the dosage of 0.2ml/ only to institute
There is the injection of group mouse peritoneal.
Eyeball takes blood after 4 days, centrifuges serum, by gained serum by 500 times of dilutions, is added in 1ml dilute serums
10%0.5ml sheep red blood cell (SRBC)s add 1ml pretreated 1：10 guinea pig serums, merging ice water is whole after 37 DEG C of water-bath 10min
Only react.2000r/min centrifugations 10min takes supernatant 1ml to add 3ml Dou Shi reagents, places after 10min in 722s spectrophotometers
OD values are measured at 540nm wavelength.
Sheep red blood cell (SRBC) half hemolysis OD values measure：It takes 10% sheep red blood cell (SRBC) 0.25ml to add 3ml Dou Shi reagents, places 10
OD values are measured after minute.Hemolysin value (the HC of each sample is calculated according to the following formula50)。
HC50=(OD values when sample OD values/sheep red blood cell half hemolysis) × extension rate
2, experimental result and analysis：It is shown in Table 4
Table 4：Influence of the Echinacea to mouse hemolysin
| Group | Dosage (g/kg) | Number of animals (only) | OD values | HC50 |
| 1 low dose group of embodiment | 0.3 | 10 | 0.17±0.07 | 108.9±47.4 |
| 1 middle dose group of embodiment | 0.9 | 10 | 0.22±0.10* | 139.0±58.3* |
| 1 high dose group of embodiment | 2.7 | 10 | 0.24±0.04** | 149.2±29.1** |
| 2 groups of embodiment | 0.9 | 10 | 0.21±0.04 | 101.2±31.7 |
| 3 groups of embodiment | 0.9 | 10 | 0.17±0.05** | 158.3±10.9** |
| 4 groups of embodiment | 0.9 | 10 | 0.15±0.01* | 121.8±20.6* |
| 1 group of comparative example | 0.9 | 10 | 0.12±0.02 | 109.2±42.4* |
| Positive controls | 0.1 | 10 | 0.26±0.09** | 148.2±46.4** |
| Blank control group | - | 10 | 0.14±0.06 | 91.6±24.3 |
Note：Each group is compared with blank control group：* significant difference (P is indicated<0.05)；* indicates pole significant difference (P<
0.01)。
4 result of table is shown：
Compared with blank control group, 1 middle and high dosage group of embodiment has the effect of improving the hemolysin value of mouse, has
Notable or pole conspicuousness difference；
Compared with 1 group of comparative example, embodiment 1 is i.e. two groups middle and high, embodiment 2-4 each groups also improve the hemolysin of mouse
Value has significant difference；
The result shows that：Extract provided by the invention, which generates mouse hemolytic antibody to have, is obviously promoted effect, explanation
The medicine can enhance humoral immunity, and effect is better than the prior art.
Although above having used general explanation, specific implementation mode and experiment, the present invention is made to retouch in detail
It states, but on the basis of the present invention, it can be made some modifications or improvements, this is apparent to those skilled in the art
's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed
Range.
Claims (12)
1. a kind of Echinacea Purpurea Herb P.E, extract contains the ingredient of following weight percent：Phenolic Compounds content is higher than
12%, Echinacea polyoses content is higher than 20%, and the content of Cichoric acid is higher than 4%；
The method for preparing the Echinacea Purpurea Herb P.E includes the following steps：
1) Echinacea crushes, sieving, crosses -24 mesh of 10 mesh sieve, spare；
2) step 1) Chinese drugs powder is taken, 7-10 times of Echinacea powder weight is added to measure the 60%- of the acid containing 0.1%-0.5% of volume
85% ethanol solution, refluxing extraction 1.5-3.0 hours, filtration obtain filtrate and the dregs of a decoction, and filtrate decompression is concentrated into 60 DEG C and measures relatively
Density is the medicinal extract of 1.06-1.12, spare；
3) dregs of a decoction for obtaining step 2) add the water-soluble of 5-7 times of alkali containing 0.05%-0.15% for measuring volume of Echinacea powder weight
Liquid, 60-90 DEG C of temperature extraction take 0.5-2.0 hours, filter, obtain filtrate and the dregs of a decoction, the dregs of a decoction discard, and filtrate decompression is concentrated into 60 DEG C of surveys
Determine the medicinal extract that relative density is 1.06-1.08, it is spare；
4) merge gained medicinal extract in step 2) and step 3), carry out centrifugal treating, clear liquid is dried, Echinacea Purpurea Herb P.E is obtained.
2. extract according to claim 1, which is characterized in that the extract contain following weight percent at
Point：Phenolic Compounds 12.1-14.4%, Echinacea polysaccharide 21.1-25.8%, Cichoric acid 4.11-5.12%.
3. extract according to claim 1, which is characterized in that in the extract containing following weight percent at
Point：Phenolic Compounds 12.1-12.8%, Echinacea polysaccharide 21.5-25.8%, Cichoric acid 4.11-4.72%.
4. extract according to claim 1, which is characterized in that in the extract containing following weight percent at
Point：Phenolic Compounds 12.8%, Echinacea polysaccharide 25.8%, Cichoric acid 4.11%.
5. extract according to claim 1, which is characterized in that the described method comprises the following steps：
1) Echinacea crushes, and crosses 15 mesh sieve, spare；
2) step 1) Chinese drugs powder is taken, adds 70% ethanol solution containing 0.2% acid of 8 times of amount volumes of Echinacea powder weight, returns
Stream extraction 2.0 hours, filtration obtain filtrate and the dregs of a decoction, and filtrate decompression is concentrated into 60 DEG C and measures the leaching that relative density is 1.06-1.12
Cream, it is spare；
3) by the gained dregs of a decoction in step 2), 0.1% aqueous slkali of 6 times of amount volumes of Echinacea powder weight, 75 DEG C of temperature extractions is added to take 1.0
Hour, filtration obtains filtrate and the dregs of a decoction, and the dregs of a decoction discard, and filtrate decompression measures relative density when being concentrated into 60 DEG C be 1.06-1.08's
Medicinal extract, it is spare；
4) merge gained medicinal extract in step 2) and step 3), carry out high speed tubular type centrifugal treating, obtain clear liquid and precipitation, gained is clear
Liquid is spray-dried, and obtains Echinacea Purpurea Herb P.E.
6. extract according to claim 1 or 5, which is characterized in that the Echinacea be Echinacea herb or stem,
One or more of mixtures of leaf, flower, root.
7. extract according to claim 1 or 5, which is characterized in that acid in the step 2) be concentrated hydrochloric acid, phosphoric acid,
The one or more of glacial acetic acid, citric acid；
Alkali in the step 3) is the one or more of sodium carbonate, sodium bicarbonate, sodium hydroxide, potassium hydroxide, concentrated ammonia liquor.
8. a kind of method preparing claim 1-4 any one of them extracts, which is characterized in that this method includes following step
Suddenly：
1) Echinacea crushes, and crosses -24 mesh of 10 mesh sieve, spare；
2) step 1) Chinese drugs powder is taken, 7-10 times of Echinacea powder weight is added to measure the 60%- of the acid containing 0.1%-0.5% of volume
85% ethanol solution, refluxing extraction 1.5-3.0 hours, filtration obtain filtrate and the dregs of a decoction, and filtrate decompression is concentrated into 60 DEG C and measures relatively
Density is the medicinal extract of 1.06-1.12, spare；
3) by the gained dregs of a decoction in step 2), add the water-soluble of 5-7 times of alkali containing 0.05%-0.15% for measuring volume of Echinacea powder weight
Liquid, 60-90 DEG C of temperature extraction take 0.5-2.0 hours, filter, obtain filtrate and the dregs of a decoction, the dregs of a decoction discard, and filtrate decompression is concentrated into 60 DEG C of surveys
Determine the medicinal extract that relative density is 1.06-1.08, it is spare；
4) merge gained medicinal extract in step 2) and step 3), carry out centrifugal treating, clear liquid is dried, Echinacea Purpurea Herb P.E is obtained.
9. according to the method described in claim 8, it is characterized in that, the described method comprises the following steps：
1) Echinacea crushes, and crosses 15 mesh sieve, spare；
2) step 1) Chinese drugs powder is taken, adds 70% ethanol solution containing 0.2% acid of 8 times of amount volumes of Echinacea powder weight, returns
Stream extraction 2.0 hours, filtration obtain filtrate and the dregs of a decoction, and filtrate decompression is concentrated into 60 DEG C and measures the leaching that relative density is 1.06-1.12
Cream, it is spare；
3) by the gained dregs of a decoction in step 2), 0.1% aqueous slkali of 6 times of amount volumes of Echinacea powder weight, 75 DEG C of temperature extractions is added to take 1.0
Hour, filtration obtains filtrate and the dregs of a decoction, and the dregs of a decoction discard, and filtrate decompression measures relative density when being concentrated into 60 DEG C be 1.06-1.08's
Medicinal extract, it is spare；
4) merge gained medicinal extract in step 2) and step 3), carry out high speed tubular type centrifugal treating, obtain clear liquid and precipitation, gained is clear
Liquid is spray-dried, and obtains Echinacea Purpurea Herb P.E.
10. method according to claim 8 or claim 9, which is characterized in that the Echinacea be Echinacea herb or stem, leaf,
One or more of mixtures of flower, root.
11. method according to claim 8 or claim 9, which is characterized in that the acid in the step 2) is concentrated hydrochloric acid, phosphoric acid, ice
The one or more of acetic acid, citric acid；
Alkali in the step 3) is the one or more of sodium carbonate, sodium bicarbonate, sodium hydroxide, potassium hydroxide, concentrated ammonia liquor.
12. any one of claim 1-7 any one of them extract or claim 8-11 the methods are preparation-obtained
Application of the extract in the drug for preparing enhancing function of immune system.
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| CN106666032A (en) * | 2015-11-10 | 2017-05-17 | 桂龙药业(安徽)有限公司 | Coneflower composition |
| CN107261104A (en) * | 2017-06-16 | 2017-10-20 | 张新成 | Promote alimentation composition of autologous stem cells regeneration and preparation method thereof |
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| EA039488B1 (en) * | 2019-12-04 | 2022-02-02 | Общество с ограниченной ответственностью "ФАРМАЦЕЛЬ" | Echinacea tincture |
| CN113069481A (en) * | 2021-05-11 | 2021-07-06 | 华南农业大学 | Application of echinacea purpurea extract in preparation of drugs for preventing and/or treating damp-heat diarrhea |
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| CN101032541A (en) * | 2006-07-28 | 2007-09-12 | 成都地奥九泓制药厂 | Echinacea purpurea extractive and the preparing method and the content measuring method |
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| CN102716164A (en) * | 2012-06-28 | 2012-10-10 | 齐鲁动物保健品有限公司 | Echinacea extract and preparation method of echinacea extract |
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| CA2307614A1 (en) * | 1997-10-23 | 1999-04-29 | Elliot P. Friedman | Pharmaceutical grade echinacea |
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| CN101032541A (en) * | 2006-07-28 | 2007-09-12 | 成都地奥九泓制药厂 | Echinacea purpurea extractive and the preparing method and the content measuring method |
| CN102060706A (en) * | 2010-12-24 | 2011-05-18 | 南京泽朗医药科技有限公司 | Method for extracting and purifying cichoric acid from Echinacea purpurea |
| CN102716164A (en) * | 2012-06-28 | 2012-10-10 | 齐鲁动物保健品有限公司 | Echinacea extract and preparation method of echinacea extract |
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