CN109568378A - A method of Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granule are prepared using continuous dynamic countercurrent extraction process - Google Patents
A method of Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granule are prepared using continuous dynamic countercurrent extraction process Download PDFInfo
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- CN109568378A CN109568378A CN201811373566.3A CN201811373566A CN109568378A CN 109568378 A CN109568378 A CN 109568378A CN 201811373566 A CN201811373566 A CN 201811373566A CN 109568378 A CN109568378 A CN 109568378A
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- cortex eucommiae
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Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/46—Eucommiaceae (Eucommia family), e.g. hardy rubber tree
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1605—Excipients; Inactive ingredients
- A61K9/1611—Inorganic compounds
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1605—Excipients; Inactive ingredients
- A61K9/1617—Organic compounds, e.g. phospholipids, fats
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1605—Excipients; Inactive ingredients
- A61K9/1629—Organic macromolecular compounds
- A61K9/1652—Polysaccharides, e.g. alginate, cellulose derivatives; Cyclodextrin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Natural Medicines & Medicinal Plants (AREA)
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- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses a kind of methods for preparing Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granule using continuous dynamic countercurrent extraction process, comprising steps of a, Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution be broken into coarse granule, coarse granule is continuously inputted to the extraction pipe of Continuous Countercurrent Extraction machine, in the end of extraction pipes at different levels continue that hot water inversely is added, continuous dynamic countercurrent extracts, extracting solution is collected, the dregs of a decoction are discharged；B, extracting solution filters, and ultra high temperature short time sterilization, filtrate decompression is condensed into clear cream；C, auxiliary material dissolution is added in clear cream, is spray-dried to obtain dry extract；D, pharmaceutical adjunct is added in dry extract, dry granulation to obtain the final product.The present invention uses Continuous Countercurrent Extraction, high-temperature short-time sterilization, reduced pressure, spray drying, dry granulation production technology, and various process parameters are studied, to enable active constituent content in granule sustainedly and stably to reach higher level, the product quality of Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granule is improved.
Description
Technical field
The invention belongs to Chinese medicinal granule technical fields, and in particular to a kind of to utilize continuous dynamic countercurrent extraction process system
The method of standby Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granule.
Background technique
Cortex Eucommiae is the dry bark of Eucommiaceae plant Cortex Eucommiae Eucommia ulmoides Oliv., is recorded in version in 2015
" Chinese Pharmacopoeia " has nourishing liver and kidney, strengthening the bones and muscles, and miscarriage prevention effect is used for kidney deficiency and liver, and soreness of waist and knee joint, muscles and bones is powerless, dizzy mesh
It is dizzy, blood leaking in gestation, threatened abortion.Cortex Eucommiae and stir-baked CORTEX EUCOMMIAE with salt solution main pharmacodynamics ingredient are Pinoresinol diglucoside, Geniposidic acid, capital
The flat glycosides of Buddhist nun, aucubin, chlorogenic acid etc., wherein Pinoresinol diglucoside is main antihypertensive compositions, is version " China in 2015
Pharmacopeia " quality control reference compound.According in relation to studies have shown that the glucosides constituents such as Pinoresinol diglucoside in Cortex Eucommiae
Stability is poor, and glycosidic bond is easily broken when heated, and temperature is higher or heated time is longer, and fracture is more obvious.
Chinese medicinal granule is to be mentioned, be concentrated through water by single medicinal material medicine materical crude slice, dried, pelletized, by tcm clinical practice formula
Afterwards, it takes after mixing it with water use for patient.The quality level of Chinese medicinal granule is with paste-forming rate, finger-print or characteristic spectrum, main work
Property the ingredient rate of transform (or content) three norms and standard decoction (being prepared with the preparation method of traditional Chinese medicine decoction) consistency
It is evaluated.
Chinese medicinal granule is prepared as a kind of industrialization product, production equipment, technique, process control and standard decoction
There are huge differences for process, low temperature concentration, dry preparation process such as standard decoction for the short time, and mass production Chinese medicine preparation
Particle has to pass through the concentration of long period under the conditions of certain temperature, dry could form used for medical institutions' adjustment
Grain, different equipment, technique and process control make the quality of the two generate difference, while different kinds is because of its ingredient
Physics, differing chemical properties, different tendency of changes or rule are presented in process of production.How equipment and technology hand passed through
Section makes industrialized product acquirement and the consistent clinical effectiveness of traditional Chinese medicine decoction, is that Chinese medicinal granule research is most important
Purpose.
Cortex Eucommiae or the existing production technology of stir-baked CORTEX EUCOMMIAE with salt solution Chinese medicinal granule are quiet mainly using the static extracting method decocted twice
State, which decocts to exist, decocts the defects of temperature is high, decocting time is long, production efficiency is low, energy consumption is at high cost, active ingredient loss is more.
Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution main active are Pinoresinol diglucoside, propose decoction, the sterilizing of clear cream ingredient, wet granulation baking in water
Do is influenced easily to degrade during waiting by long-time high temperature, thus causes the ingredient rate of transform low, and content deviates standard decoction
Technical requirements range, so that the Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granular mass of production be not up to standard, other than causing the huge wasting of resources, batch
Between quality level inconsistency, clinical application but will be influenced safely, effectively.
Continuous dynamic countercurrent extraction is novel extraction process in recent years, it collects extraction, weight diacolation, dynamic and adverse current skill
Art is integrated, and has many advantages, such as that simple process, saving solvent, low energy consumption, extraction time is short, extraction efficiency is high.Currently, there is not yet
The report of Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granule is prepared using continuous dynamic countercurrent extraction process.
Summary of the invention
In order to overcome above-mentioned problem of the prior art, mentioned the purpose of the present invention is to provide a kind of using continuous dynamic countercurrent
The method that taking technique prepares Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granule, this method contain effective component in Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granule
Amount can sustainedly and stably reach higher level, improve the product quality of Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granule.
The present invention is achieved through the following technical solutions；
A method of Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granule being prepared using continuous dynamic countercurrent extraction process, including is walked as follows
It is rapid:
A, continuous dynamic countercurrent extracts
Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution are broken into coarse granule, broken coarse granule is continuously inputted into continuous flow upstream by feed inlet and is mentioned
Material is continuously pushed to forward extraction pipe slag-drip opening by a set of helical structure in extraction pipe and slagged tap by the extraction pipe for taking machine,
Continue the hot water that 10~25 times of amounts are inversely added, preferably 13~20 times amounts, continuous dynamic countercurrent in the end of extraction pipes at different levels
1~3h, preferably 1.5~2.5h are extracted, extracting solution is collected, the dregs of a decoction are discharged；
B, high-temperature short-time sterilization
Extracting solution cooling after refilter, filtrate through ultra high temperature short time sterilization, then under the conditions of 50~80 DEG C be concentrated under reduced pressure at
The clear cream that relative density is 1.01~1.20；
C, it is spray-dried
Auxiliary material dissolution is added in qinghuo reagent, is spray-dried to obtain dry extract；
D, dry granulation
Pharmaceutical adjunct will be added in dry extract, dry granulation obtains Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granule.
The present invention carries out the extraction process of Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution using continuous dynamic countercurrent extractor, extracts principle are as follows:
Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution medicine materical crude slice are continuously added to the extraction pipe of Continuous Countercurrent Extraction machine by feed inlet (front end), passed through in extraction pipe
Material is continuously pushed to forward extraction pipe slag-drip opening (end) and slagged tap by a set of helical structure, and water-soluble matchmaker then manages in extractions at different levels
End be continuously added into, with material in liquid is brought out before reverse flow to feed inlet end or extraction pipe at different levels, material and extraction are molten
Agent comes into full contact with, and the concentration gradient of solute is made to remain at higher level, so as to greatly improve mentioning for effective component
The rate of transform, while the Extracting temperature by controlling extraction pipes at different levels are taken, the degradation of heat-sensitive ingredients at high temperature is reduced and destroys.
The size of the broken partial size of raw material will affect whether effective component can be fully dissolved out, while influence extraction process object
Whether push movement is smooth forward for material, is unfavorable for solute if partial size is excessive and quickly transmits into solvent, while existing to material
Smooth retard motion in Continuous Countercurrent Extraction is easy to miss from spiral plate hole and can not be successfully transmission if partial size is too small
To slag-drip opening, it is preferred that in step a, the broken coarse grained partial size is 0.3~0.8cm.
Dry coarse granule is easy to appear in blanking process to get stuck, and the medicine materical crude slice after water soaks is easier blanking, to protect
Card can be such that material comes into full contact with Extraction solvent with the blanking of continuous and quantitative, while be conducive in material after effective component blanking
Quickly extract transfer, it is preferred that in step a, broken coarse granule is first added to after the water wetting of 1~5 times of amount the company of input again
In continuous dynamic countercurrent extractor.
Preferably, in step a, the Continuous Countercurrent Extraction machine is spiral Continuous Countercurrent Extraction machine, is 10 section of stage type
Pipe structure.Compared to pot group type countercurrent extraction machine group, horizontal spiral Continuous Countercurrent Extraction machine has agglomerated dynamic countercurrent extraction, continuous
The features such as slag charge extruding, continuous automatic slag-liquid separation and filtering, realize whole serialization, automatic control, fast low temperature extraction.
Preferably, in step a, the temperature of the hot water is 60~95 DEG C, preferably 70~95 DEG C.
For the rate of transform for further increasing effective component, it is preferred that in step a, by Cortex Eucommiae or the stir-baked CORTEX EUCOMMIAE with salt solution dregs of a decoction through squeezing
It is then exhausted from after recovery section medical fluid, the part medical fluid of recycling merges with extracting solution, so as to further increase Cortex Eucommiae or salt Du
The rate of recovery of secondary extracting solution increases the rate of transform of effective component.
Preferably, in step a, the Cortex Eucommiae or the coarse grained input speed of stir-baked CORTEX EUCOMMIAE with salt solution are 100~250kg/h, reverse to add
The flow velocity for entering hot water is 1000~6250kg/h.The present invention is fed by continuous and quantitative, comes into full contact with material with Extraction solvent,
The solvent that extracts of equipment is added with certain flow velocity, is constantly updated, thus make material be constantly in throughout the extraction process compared with
Big concentration gradient is poor, is conducive to being fully dissolved out for effective component, so can greatly improve in Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution effectively at
The rate of transform divided.
Preferably, it in step b, is refiltered after extracting solution is first cooled to 40~55 DEG C.
The present invention uses Continuous Countercurrent Extraction, and Extracting temperature is lower, and product microorganism risk of exceeding criterion is big, and it is further right to need
Extracting solution carries out ultra high temperature short time sterilization, to prevent Pinoresinol diglucoside from chemical degradation occurring in sterilization process, preferably
, in step b, the ultra high temperature short time sterilization be by filtrate in supper high temperature instant sterilizer at 100~150 DEG C sterilizing 2~
30 seconds.
Ingredient is easily degraded in active constituent material wet granulation drying course, is preferably suitable for dry granulation.To improve
The viscosity of material, mobility meet granule melting requirement to be adapted to dry granulation, in clear cream spray drying ingredient
Relevant auxiliary materials are added, and takes a step forward in dry granulation and proper auxiliary materials are added adjust its mobility, compressibility.Preferably, step c
In, the auxiliary material is one or more of maltodextrin, dextrin, starch, lactose or beta-cyclodextrin；The work of the spray drying
Skill parameter are as follows: 160 DEG C~190 DEG C of inlet air temperature, 80 DEG C~100 DEG C of leaving air temp of control.
Preferably, in step d, the pharmaceutical adjunct is maltodextrin, dextrin, starch, lactose, beta-cyclodextrin, titanium dioxide
One or more of silicon or magnesium stearate.
Compared with prior art, the present invention having the following beneficial effects:
(1) present invention can keep concentration difference between solute and solvent using continuous flow upstream for a long time, and can be lower
At a temperature of the characteristics of extracting, improve the physics of Pinoresinol diglucoside during the extraction process and dissolve out the rate of transform, while can be with
Lower temperature carries out the continuous extraction of temperature leaching, reduces its chemical degradation.
(2) present invention makes microorganism be inactivated and produce under superhigh temperature in short-term using ultra high temperature short time sterilization technology (UHT)
The characteristics of product ingredient does not change prevents degradation of the Pinoresinol diglucoside in spray drying blending process, and preferably
Various granulation auxiliary materials carry out dry granulation, prevent active constituent from crossing in kind in preparation and change.
(3) present invention combines Continuous Countercurrent Extraction, ultra high temperature short time sterilization, reduced pressure, spray drying, dry granulation raw
Production. art, and various process parameters are studied, to make Cortex Eucommiae and its processed product stir-baked CORTEX EUCOMMIAE with salt solution Chinese medicinal granule rosin spirit
Diglucoside content can sustainedly and stably reach higher level, improve the product quality of Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granule.
Specific embodiment
Further illustrate that the present invention, following embodiment are the specific embodiment party of the present invention below by specific embodiment
Formula, but embodiments of the present invention are not limited by following embodiments.
Stir-baked CORTEX EUCOMMIAE with salt solution used by the embodiment of the present invention is according to stir-baked CORTEX EUCOMMIAE with salt solution under version " Chinese Pharmacopoeia " Cortex Eucommiae item in 2015
Processing regulation and four 0213 process general rule items under method of stir-baking medicine with salt solu-tion process.
The present invention passes through the study found that in continuous dynamic countercurrent extraction process, the temperature of hot water, solvent amount, when extracting
Between, the factors such as temperature of cooling have bigger influence to extraction effect.For this purpose, the present invention has been carried out for these factors into one
The optimization of step, specific as follows:
The present invention is to extract solvent with hot water, is fed intake using hot water, and water temperature height directly affects extraction effect.Water temperature is too low
Then solvent warm-up movement is unfavorable for solute slowly and transmits into solvent water in extraction process, water temperature over-high then effective component in solvent water
Easy thermal degradation, to further illustrate influence of the water temperature height to extraction effect, water temperature is optimized in the present invention, concrete outcome
It is as follows:
| Water temperature | 50℃ | 60℃ | 70℃ | 85℃ | 95℃ | 100℃ |
| The Cortex Eucommiae Pinoresinol diglucoside rate of transform (%) | 50.5 | 70.0 | 75.8 | 81.0 | 77.5 | 69.4 |
| The stir-baked CORTEX EUCOMMIAE with salt solution Pinoresinol diglucoside rate of transform (%) | 55.8 | 76.5 | 82.6 | 86.0 | 83.2 | 73.5 |
If the temperature of water is lower it can be seen from the above results, it may cause effective component and extract not exclusively, if water
Temperature it is excessively high, the Pinoresinol diglucoside rate of transform be easy to happen in aqueous solution chemical degradation loss, it is preferred, therefore, that
In step a, the temperature of the hot water is 60~95 DEG C, more preferably 70~95 DEG C.
Solvent amount also directly influences the extraction and degradation of active constituent, and the present invention has further carried out solvent amount excellent
Change, concrete outcome is as follows:
| Solvent amount | 10 times of amounts | 13 times of amounts | 16 times of amounts | 20 times of amounts | 25 times of amounts | 30 times of amounts |
| The Cortex Eucommiae Pinoresinol diglucoside rate of transform (%) | 65.5 | 76.0 | 80.2 | 76.5 | 71.4 | 62.3 |
| The stir-baked CORTEX EUCOMMIAE with salt solution Pinoresinol diglucoside rate of transform (%) | 72.5 | 82.3 | 87.0 | 84.8 | 79.6 | 69.1 |
If solvent amount is very few it can be seen from the above results, active constituent each extraction pipeline section cannot reach compared with
High concentration difference, physical transfer is incomplete, and when solvent amount reaches 16 times of amounts, the Pinoresinol diglucoside rate of transform is basically reached
Peak value, if solvent amount is excessive, not only energy consumption is improved, but also extracting solution also accordingly extends in concentration time, and ingredient is being concentrated
Duan Fasheng degradation, so that the rate of transform of Pinoresinol diglucoside can be reduced.It is preferred, therefore, that the additional amount of the hot water is
10~25 times of amounts, more preferably 13~20 times amounts.
Extraction time of the material in extraction pipe is also related to the physical transfer rate and chemical degradation of active constituent, the present invention
Further extraction time is optimized, concrete outcome is as follows:
| Extraction time | 0.5h | 1h | 1.5h | 2.5h | 3h | 4h |
| The Cortex Eucommiae Pinoresinol diglucoside rate of transform (%) | 60.5 | 72.0 | 80.5 | 74.2 | 70.3 | 58.6 |
| The stir-baked CORTEX EUCOMMIAE with salt solution Pinoresinol diglucoside rate of transform (%) | 70.1 | 79.6 | 87.3 | 81.5 | 76.0 | 63.5 |
If extraction time is short it can be seen from the above results, active constituent physical transfer is incomplete, if extraction time
Too long, Pinoresinol diglucoside chemical degradation rate is high, while reducing production efficiency.Preferably, in step a, Cortex Eucommiae or salt Du
Secondary coarse granule extraction time in continuous dynamic countercurrent extraction is 1~3h, more preferably 1.5~2.5h.
In order to avoid Pinoresinol diglucoside ingredient breakdown in Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution medicine materical crude slice, the rate of transform is further increased,
The present invention will first refilter after the extracting solution cooling in step a, and the present invention is further optimized cooling temperature, specific to tie
Fruit is as follows:
| Cool down temperature | 25℃ | 40℃ | 55℃ | 70℃ | 80℃ |
| The Cortex Eucommiae Pinoresinol diglucoside rate of transform (%) | 81.0 | 80.9 | 80.5 | 76.4 | 74.2 |
| The stir-baked CORTEX EUCOMMIAE with salt solution Pinoresinol diglucoside rate of transform (%) | 86.8 | 86.5 | 85.7 | 82.4 | 78.0 |
The thermal degradation that can effectively avoid Pinoresinol diglucoside after extracting solution cooling it can be seen from the above results, has
Retain conducive to its content and improves the rate of transform.When being cooled to 25~55 DEG C of temperature ranges, Pinoresinol diglucoside thermal degradation
Less and tend towards stability, the temperature being concentrated in combination with extracting solution after cooling is mentioned in 50~80 DEG C of temperature ranges to reduce
Heating energy consumption when liquid being taken to be concentrated, it is preferred that in step b, refiltered after extracting solution is first cooled to 40~55 DEG C.
Embodiment 1:
A method of Cortex Eucommiae granule being prepared using continuous dynamic countercurrent extraction process, is included the following steps:
A, continuous dynamic countercurrent extracts
Eucommia ulmoides are scraped off into residual rough bark, vibration is weeded out except impurity, is broken into 0.5cm particle；By broken coarse granule
It is soaked with 2 times of amount water, the extraction pipe of spiral Continuous Countercurrent Extraction machine (10 section pipe structure of stage type) is continuously inputted by feed inlet,
Material is continuously pushed to forward extraction pipe slag-drip opening by a set of helical structure in extraction pipe to slag tap, in extraction pipes at different levels
End continues 95 DEG C of hot water Continuous Countercurrent Extraction 1.5h that 16 times of amounts are inversely added, and hot water and material are in reverse flow to leachings at different levels
Liquid is brought out before mentioning pipe, extracting solution is collected, the Cortex Eucommiae dregs of a decoction is then exhausted from after squeezing recovery section medical fluid, the part medical fluid of recycling
Merge with extracting solution；The input speed of the Cortex Eucommiae medicine materical crude slice is 100kg/h, and the reverse flow velocity that hot water is added is 1600L/h；
B, high-temperature short-time sterilization
Extracting solution after merging filters after being cooled to 80 DEG C, and filtered fluid is in supper high temperature instant sterilizer (UHT) at 150 DEG C
Sterilizing 10 seconds, after at 60 DEG C be concentrated under reduced pressure at relative density be 1.05 clear cream；
C, it is spray-dried
Qinghuo reagent is added maltodextrin and dissolves and stir evenly, and is spray-dried, obtains dry extract, the spray drying
Technological parameter are as follows: control 175 DEG C~190 DEG C of inlet air temperature, 80 DEG C~90 DEG C of leaving air temp；
D, dry granulation
Maltodextrin is added in dry extract and silica, dry granulation obtain Cortex Eucommiae granule.
Embodiment 2:
A method of Cortex Eucommiae granule being prepared using continuous dynamic countercurrent extraction process, is included the following steps:
A, continuous dynamic countercurrent extracts
Eucommia ulmoides are scraped off into residual rough bark, vibration is weeded out except impurity, is broken into 0.5cm particle；By broken coarse granule
It is soaked with 2 times of amount water, the extraction pipe of spiral Continuous Countercurrent Extraction machine (10 section pipe structure of stage type) is continuously inputted by feed inlet,
Material is continuously pushed to forward extraction pipe slag-drip opening by a set of helical structure in extraction pipe to slag tap, in extraction pipes at different levels
End continues 95 DEG C of hot water Continuous Countercurrent Extraction 1.5h that 16 times of amounts are inversely added, and hot water and material are in reverse flow to leachings at different levels
Liquid is brought out before mentioning pipe, extracting solution is collected, the Cortex Eucommiae dregs of a decoction is then exhausted from after squeezing recovery section medical fluid, the part medical fluid of recycling
Merge with extracting solution；The input speed of the Cortex Eucommiae medicine materical crude slice is 100kg/h, and the reverse flow velocity that hot water is added is 1600L/h；
B, high-temperature short-time sterilization
Extracting solution after merging filters after being cooled to 50 DEG C, and filtered fluid is in supper high temperature instant sterilizer (UHT) at 150 DEG C
Sterilizing 10 seconds, after at 60 DEG C be concentrated under reduced pressure at relative density be 1.05 clear cream；
C, it is spray-dried
Qinghuo reagent is added maltodextrin and dissolves and stir evenly, and is spray-dried, obtains dry extract, the spray drying
Technological parameter are as follows: control 175 DEG C~190 DEG C of inlet air temperature, 80 DEG C~90 DEG C of leaving air temp；
D, dry granulation
Maltodextrin and silica is added in dry extract, is uniformly mixed, dry granulation obtains Cortex Eucommiae granule.
Embodiment 3:
A method of Cortex Eucommiae granule being prepared using continuous dynamic countercurrent extraction process, is included the following steps:
A, continuous dynamic countercurrent extracts
Eucommia ulmoides are scraped off into residual rough bark, vibration is weeded out except impurity, is broken into 0.5cm particle；By broken coarse granule
It is soaked with 2 times of amount water, the extraction pipe of spiral Continuous Countercurrent Extraction machine (10 section pipe structure of stage type) is continuously inputted by feed inlet,
Material is continuously pushed to forward extraction pipe slag-drip opening by a set of helical structure in extraction pipe to slag tap, in extraction pipes at different levels
End continues 85 DEG C of hot water Continuous Countercurrent Extraction 1.5h that 16 times of amounts are inversely added, and hot water and material are in reverse flow to leachings at different levels
Liquid is brought out before mentioning pipe, extracting solution is collected, the Cortex Eucommiae dregs of a decoction is then exhausted from after squeezing recovery section medical fluid, the part medical fluid of recycling
Merge with extracting solution；The input speed of the Cortex Eucommiae medicine materical crude slice is 100kg/h, and the reverse flow velocity that hot water is added is 1600L/h；
B, high-temperature short-time sterilization
Extracting solution after merging filters after being cooled to 50 DEG C, and filtered fluid is in supper high temperature instant sterilizer (UHT) at 150 DEG C
Sterilizing 10 seconds, after at 60 DEG C be concentrated under reduced pressure at relative density be 1.05 clear cream；
C, it is spray-dried
Qinghuo reagent is added maltodextrin and dissolves and stir evenly, and is spray-dried, obtains dry extract, the spray drying
Technological parameter are as follows: control 175 DEG C~190 DEG C of inlet air temperature, 80 DEG C~90 DEG C of leaving air temp；
D, dry granulation
Maltodextrin and silica is added in dry extract, is uniformly mixed, dry granulation obtains Cortex Eucommiae granule.
Embodiment 4:
A method of Cortex Eucommiae granule being prepared using continuous dynamic countercurrent extraction process, is included the following steps:
A, continuous dynamic countercurrent extracts
Eucommia ulmoides are scraped off into residual rough bark, vibration is weeded out except impurity, is broken into 0.5cm particle；By broken coarse granule
The extraction pipe that spiral Continuous Countercurrent Extraction machine (10 section pipe structure of stage type) is continuously inputted by feed inlet passes through in extraction pipe
Material is continuously pushed to forward extraction pipe slag-drip opening and slagged tap by a set of helical structure, continues inversely to add in the end of extraction pipes at different levels
Enter 85 DEG C of hot water Continuous Countercurrent Extraction 1.5h of 16 times of amounts, hot water and material are in bring out before reverse flow to extraction pipes at different levels
Liquid collects extracting solution, the Cortex Eucommiae dregs of a decoction is discharged；The input speed of the Cortex Eucommiae medicine materical crude slice is 100kg/h, the reverse stream that hot water is added
Speed is 1600L/h；
B, high-temperature short-time sterilization
Extracting solution after merging filters after being cooled to 50 DEG C, and filtered fluid is in supper high temperature instant sterilizer (UHT) at 150 DEG C
Sterilizing 10 seconds, after at 60 DEG C be concentrated under reduced pressure at relative density be 1.05 clear cream；
C, it is spray-dried
Qinghuo reagent is added maltodextrin and dissolves and stir evenly, and is spray-dried, obtains dry extract, the spray drying
Technological parameter are as follows: control 160 DEG C~175 DEG C of inlet air temperature, 90 DEG C~100 DEG C of leaving air temp；
D, dry granulation
Maltodextrin is added in dry extract, is uniformly mixed, dry granulation obtains Cortex Eucommiae granule.
Embodiment 5:
A method of Cortex Eucommiae granule being prepared using continuous dynamic countercurrent extraction process, is included the following steps:
A, continuous dynamic countercurrent extracts
Eucommia ulmoides are scraped off into residual rough bark, vibration is weeded out except impurity, is broken into 0.5cm particle；By broken coarse granule
It is soaked with 2 times of amount water, the extraction pipe of spiral Continuous Countercurrent Extraction machine (10 section pipe structure of stage type) is continuously inputted by feed inlet,
Material is continuously pushed to forward extraction pipe slag-drip opening by a set of helical structure in extraction pipe to slag tap, in extraction pipes at different levels
End continues 75 DEG C of hot water Continuous Countercurrent Extraction 2h that 14 times of amounts are inversely added, and hot water and material are in reverse flow to extractions at different levels
Bring out liquid before pipe, collect extracting solution, the Cortex Eucommiae dregs of a decoction are then exhausted from after squeezing recovery section medical fluid, the part medical fluid of recycling and
Extracting solution merges；The input speed of the Cortex Eucommiae medicine materical crude slice is 50kg/h, and the reverse flow velocity that hot water is added is 700L/h；
B, high-temperature short-time sterilization
Extracting solution after merging filters after being cooled to 45 DEG C, and filtered fluid is in supper high temperature instant sterilizer (UHT) at 105 DEG C
Sterilizing 30 seconds, after at 75 DEG C be concentrated under reduced pressure at relative density be 1.05 clear cream；
C, it is spray-dried
Qinghuo reagent is added maltodextrin and dissolves and stir evenly, and is spray-dried, obtains dry extract, the spray drying
Technological parameter are as follows: control 160 DEG C~175 DEG C of inlet air temperature, 90 DEG C~100 DEG C of leaving air temp；
D, dry granulation
Lactose, silica and magnesium stearate is added in dry extract, is uniformly mixed, dry granulation obtains Cortex Eucommiae granule.
Comparative example 1: Chinese medicine extracting tank is used
A kind of preparation method of Cortex Eucommiae granule, includes the following steps:
A, Eucommia ulmoides are scraped off into residual rough bark, vibration is weeded out except impurity, is broken into 0.5cm particle；
B, Cortex Eucommiae coarse granule is added in Chinese medicine extracting tank, with water boiling and extraction 2 times, for the first time plus 9 times of amount water heating are decocted
1h is boiled, second plus 7 times of amount water heating decoction 0.5h, extracting solution filtration；
C, the clear cream that relative density is 1.05 when filtrate decompression is condensed into 60 DEG C；
D, qinghuo reagent is added maltodextrin and dissolves and stir evenly, and is spray-dried, and dry extract is obtained, described spraying dry
Dry technological parameter are as follows: 175 DEG C~190 DEG C of inlet air temperature, 80 DEG C~90 DEG C of leaving air temp of control；
E, dry extract adds maltodextrin and magnesium stearate, is uniformly mixed, dry granulation obtains Cortex Eucommiae granule.
Comparative example 2: pot group type countercurrent extraction machine is used
A kind of preparation method of Cortex Eucommiae granule, includes the following steps:
A, Eucommia ulmoides are scraped off into residual rough bark, vibration is weeded out except impurity, is broken into 0.5cm particle；
B, medicine materical crude slice is put into the series connection extractor group formed with 5 end to end extractors by the following arrangement mode that feeds intake
In, fresh solvent is added with material-water ratio 1:16 ratio in tail tank, is mentioned with 95 DEG C of each tank Extracting temperature, extraction time 1.5h
Take: the material in 5 tanks is successively new medicine materical crude slice, the dregs of a decoction after 1 time is extracted, the dregs of a decoction extracted through 2 times, the medicine extracted through 3 times
Fresh solvent is added in (dregs of a decoction after extracting equipped with the 4th) tank of most end by slag, the dregs of a decoction extracted through 4 times, other each
Tank is sequentially arranged with from the extracting solution that next stage tank transfer moves past and extracts, and final extracting solution is discharged from the tank of foremost,
The last extractor discharge dregs of a decoction are simultaneously packed into new medicine materical crude slice, become most preceding extractor, and so circulation is reverse extracts, and collect extracting solution
Filtration merges；
C, the extracting solution after merging filters after being cooled to 50 DEG C, and filtered fluid is 150 DEG C in supper high temperature instant sterilizer (UHT)
It is lower sterilizing 10 seconds, after at 60 DEG C be concentrated under reduced pressure at relative density be 1.05 clear cream；
D, qinghuo reagent is added maltodextrin and dissolves and stir evenly, and is spray-dried, and dry extract is obtained, described spraying dry
Dry technological parameter are as follows: 175 DEG C~190 DEG C of inlet air temperature, 80 DEG C~90 DEG C of leaving air temp of control；
E, maltodextrin and magnesium stearate is added in dry extract, is uniformly mixed, dry granulation obtains Cortex Eucommiae granule.
The Cortex Eucommiae granule that embodiment and comparative example is prepared measures Pinoresinol diglucoside content, calculates
Paste-forming rate, rate of transform situation, the results are shown in Table 1:
1 Cortex Eucommiae granule embodiment of table is compared with comparative example result
By embodiment 1 it is found that the present invention uses Continuous Countercurrent Extraction technology, with traditional extraction compared with 1 result of comparative example
Tank extractive technique is compared, and not only solvent consumption amount is few, and can continuous slag charge squeeze, continuous automatic slag-liquid separation, realize complete
Journey serialization, automatic control, fast low temperature extract, and remain heat-sensitive ingredients Pinoresinol diglucoside content, hence it is evident that improve
The rate of transform shows that the present invention is substantially better than common extractor currently on the market using Continuous Countercurrent Extraction technology and extracts skill
Art.
By embodiment 1 compared with 2 result of comparative example it is found that compared with pot group type countercurrent extraction machine, the continuous flow upstream of use
The content and the rate of transform of extractive technique either paste-forming rate or Pinoresinol diglucoside increase, i.e., the present invention adopts
It is better than pot group type countercurrent extraction machine with Continuous Countercurrent Extraction technology.
By embodiment 1, it is found that the present invention is used, by extracting solution, cooling is handled rapidly compared with 2 result of embodiment, can be kept away
Exempt from the degradation loss of Pinoresinol diglucoside, hence it is evident that improve the rate of transform of the ingredient.
By 2~5 result of embodiment it is found that the present invention, which carries out low-temperature dynamic adverse current using Continuous Countercurrent Extraction technology, extracts energy
Pinoresinol diglucoside content and the rate of transform are significantly improved, and then improves the quality of product.Meanwhile continuous dynamic countercurrent technology
In the case where guaranteeing paste-forming rate, component content and the rate of transform, it can be further reduced the consumption of solvent, be one kind of economical and energy saving
Novel extracting mode.
By Examples 1 to 5 compared with comparative example 1 it is found that the present invention using ultra high temperature short time sterilization technology to extracting solution into
Row sterilizing preferably can control microorganism from source, guarantee that the microorganism of finished product is qualified.
Embodiment 6:
A method of stir-baked CORTEX EUCOMMIAE with salt solution granule being prepared using continuous dynamic countercurrent extraction process, is included the following steps:
A, continuous dynamic countercurrent extracts
Stir-baked CORTEX EUCOMMIAE with salt solution medicine materical crude slice is taken, 0.5cm particle is broken into；2 times of amount water of broken coarse granule are soaked, are connected by feed inlet
The extraction pipe of the continuous spiral Continuous Countercurrent Extraction machine (10 section pipe structure of stage type) of input, passes through a set of spiral knot in extraction pipe
Material is continuously pushed to forward extraction pipe slag-drip opening and slagged tap by structure, in the end of extraction pipes at different levels continues that 16 times of amounts are inversely added
95 DEG C of hot water Continuous Countercurrent Extraction 1.5h, hot water and material are collected and are extracted in liquid is brought out before reverse flow to extraction pipes at different levels
The stir-baked CORTEX EUCOMMIAE with salt solution dregs of a decoction are then exhausted from by liquid after squeezing recovery section medical fluid, and the part medical fluid of recycling merges with extracting solution；Salt Du
The input speed of secondary medicine materical crude slice is 100kg/h, and the reverse flow velocity that hot water is added is 1600L/h；
B, high-temperature short-time sterilization
Extracting solution after merging filters after being cooled to 80 DEG C, and filtered fluid is in supper high temperature instant sterilizer (UHT) at 150 DEG C
Sterilizing 10 seconds, after at 60 DEG C be concentrated under reduced pressure at relative density be 1.05 clear cream；
C, it is spray-dried
Qinghuo reagent is added maltodextrin and dissolves and stir evenly, and is spray-dried, obtains dry extract, the spray drying
Technological parameter are as follows: control 175 DEG C~190 DEG C of inlet air temperature, 80 DEG C~90 DEG C of leaving air temp；
D, dry granulation
Maltodextrin is added in dry extract and silica, dry granulation obtain stir-baked CORTEX EUCOMMIAE with salt solution granule.
Embodiment 7:
A method of stir-baked CORTEX EUCOMMIAE with salt solution granule being prepared using continuous dynamic countercurrent extraction process, is included the following steps:
A, continuous dynamic countercurrent mentions
Stir-baked CORTEX EUCOMMIAE with salt solution medicine materical crude slice is taken, 0.5cm particle is broken into；2 times of amount water of broken coarse granule are soaked, are connected by feed inlet
The extraction pipe of the continuous spiral Continuous Countercurrent Extraction machine (10 section pipe structure of stage type) of input, passes through a set of spiral knot in extraction pipe
Material is continuously pushed to forward extraction pipe slag-drip opening and slagged tap by structure, in the end of extraction pipes at different levels continues that 16 times of amounts are inversely added
95 DEG C of hot water Continuous Countercurrent Extraction 1.5h, hot water and material are collected and are extracted in liquid is brought out before reverse flow to extraction pipes at different levels
The stir-baked CORTEX EUCOMMIAE with salt solution dregs of a decoction are then exhausted from by liquid after squeezing recovery section medical fluid, and the part medical fluid of recycling merges with extracting solution；Salt Du
The input speed of secondary medicine materical crude slice is 100kg/h, and the reverse flow velocity that hot water is added is 1600L/h；
B, high-temperature short-time sterilization
Extracting solution after merging filters after being cooled to 50 DEG C, and filtered fluid is in supper high temperature instant sterilizer (UHT) at 150 DEG C
Sterilizing 10 seconds, after at 60 DEG C be concentrated under reduced pressure at relative density be 1.05 clear cream；
C, it is spray-dried
Qinghuo reagent is added maltodextrin and dissolves and stir evenly, and is spray-dried, obtains dry extract, the spray drying
Technological parameter are as follows: control 175 DEG C~190 DEG C of inlet air temperature, 80 DEG C~90 DEG C of leaving air temp；
D, dry granulation
Maltodextrin and silica is added in dry extract, is uniformly mixed, dry granulation obtains stir-baked CORTEX EUCOMMIAE with salt solution granule.
Embodiment 8:
A method of stir-baked CORTEX EUCOMMIAE with salt solution granule being prepared using continuous dynamic countercurrent extraction process, is included the following steps:
A, continuous dynamic countercurrent extracts
Stir-baked CORTEX EUCOMMIAE with salt solution medicine materical crude slice is taken, 0.5cm particle is broken into；2 times of amount water of broken coarse granule are soaked, are connected by feed inlet
The extraction pipe of the continuous spiral Continuous Countercurrent Extraction machine (10 section pipe structure of stage type) of input, passes through a set of spiral knot in extraction pipe
Material is continuously pushed to forward extraction pipe slag-drip opening and slagged tap by structure, in the end of extraction pipes at different levels continues that 16 times of amounts are inversely added
85 DEG C of hot water Continuous Countercurrent Extraction 1.5h, hot water and material are collected and are extracted in liquid is brought out before reverse flow to extraction pipes at different levels
The stir-baked CORTEX EUCOMMIAE with salt solution dregs of a decoction are then exhausted from by liquid after squeezing recovery section medical fluid, and the part medical fluid of recycling merges with extracting solution；Salt Du
The input speed of secondary medicine materical crude slice is 100kg/h, and the reverse flow velocity that hot water is added is 1600L/h；
B, high-temperature short-time sterilization
Extracting solution after merging filters after being cooled to 50 DEG C, and filtered fluid is in supper high temperature instant sterilizer (UHT) at 150 DEG C
Sterilizing 10 seconds, after at 60 DEG C be concentrated under reduced pressure at relative density be 1.05 clear cream；
C, it is spray-dried
Qinghuo reagent is added maltodextrin and dissolves and stir evenly, and is spray-dried, obtains dry extract, the spray drying
Technological parameter are as follows: control 160 DEG C~175 DEG C of inlet air temperature, 90 DEG C~100 DEG C of leaving air temp；
D, dry granulation
Maltodextrin and silica is added in dry extract, is uniformly mixed, dry granulation obtains stir-baked CORTEX EUCOMMIAE with salt solution granule.
Embodiment 9:
A method of stir-baked CORTEX EUCOMMIAE with salt solution granule being prepared using continuous dynamic countercurrent extraction process, is included the following steps:
A, continuous dynamic countercurrent extracts
Stir-baked CORTEX EUCOMMIAE with salt solution medicine materical crude slice is taken, 0.5cm particle is broken into；Broken coarse granule is continuously inputted by feed inlet and is spirally connected
The extraction pipe of continuous countercurrent extraction machine (10 section pipe structure of stage type), in extraction pipe by a set of helical structure by material continuously to
Before push to extraction pipe slag-drip opening slag tap, it is at different levels extraction pipes ends continue inversely be added 16 times amount 85 DEG C of hot water it is continuously inverse
Stream extracts 1.5h, hot water and material in liquid is brought out before reverse flow to extraction pipes at different levels, extracting solution is collected, by the stir-baked CORTEX EUCOMMIAE with salt solution dregs of a decoction
Discharge；The input speed of the stir-baked CORTEX EUCOMMIAE with salt solution medicine materical crude slice is 100kg/h, and the reverse flow velocity that hot water is added is 1600L/h；
B, high-temperature short-time sterilization
Extracting solution after merging filters after being cooled to 50 DEG C, and filtered fluid is in supper high temperature instant sterilizer (UHT) at 150 DEG C
Sterilizing 10 seconds, after at 60 DEG C be concentrated under reduced pressure at relative density be 1.05 clear cream；
C, it is spray-dried
Qinghuo reagent is added maltodextrin and dissolves and stir evenly, and is spray-dried, obtains dry extract, the spray drying
Technological parameter are as follows: control 160 DEG C~175 DEG C of inlet air temperature, 90 DEG C~100 DEG C of leaving air temp；
D, dry granulation
Maltodextrin is added in dry extract, is uniformly mixed, dry granulation obtains stir-baked CORTEX EUCOMMIAE with salt solution granule.
Embodiment 10:
A method of stir-baked CORTEX EUCOMMIAE with salt solution granule being prepared using continuous dynamic countercurrent extraction process, is included the following steps:
A, continuous dynamic countercurrent extracts
Stir-baked CORTEX EUCOMMIAE with salt solution medicine materical crude slice is taken, 0.5cm particle is broken into；2 times of amount water of broken coarse granule are soaked, are connected by feed inlet
The extraction pipe of the continuous spiral Continuous Countercurrent Extraction machine (10 section pipe structure of stage type) of input, passes through a set of spiral knot in extraction pipe
Material is continuously pushed to forward extraction pipe slag-drip opening and slagged tap by structure, in the end of extraction pipes at different levels continues that 14 times of amounts are inversely added
75 DEG C of hot water Continuous Countercurrent Extraction 2h, hot water and material collect extracting solution in liquid is brought out before reverse flow to extraction pipes at different levels,
The stir-baked CORTEX EUCOMMIAE with salt solution dregs of a decoction are then exhausted from after squeezing recovery section medical fluid, the part medical fluid of recycling merges with extracting solution；The stir-baked CORTEX EUCOMMIAE with salt solution
The input speed of medicine materical crude slice is 50kg/h, and the reverse flow velocity that hot water is added is 700L/h；
B, high-temperature short-time sterilization
Extracting solution after merging filters after being cooled to 45 DEG C, and filtered fluid is in supper high temperature instant sterilizer (UHT) at 105 DEG C
Sterilizing 30 seconds, after at 75 DEG C be concentrated under reduced pressure at relative density be 1.05 clear cream；
C, it is spray-dried
Qinghuo reagent is added maltodextrin and dissolves and stir evenly, and is spray-dried, obtains dry extract, the spray drying
Technological parameter are as follows: control 160 DEG C~175 DEG C of inlet air temperature, 90 DEG C~100 DEG C of leaving air temp；
D, dry granulation
Lactose, silica and magnesium stearate is added in dry extract, is uniformly mixed, and dry granulation obtains stir-baked CORTEX EUCOMMIAE with salt solution formula
Grain.
Comparative example 3: Chinese medicine extracting tank is used
A kind of preparation method of stir-baked CORTEX EUCOMMIAE with salt solution granule, includes the following steps:
A, stir-baked CORTEX EUCOMMIAE with salt solution medicine materical crude slice is taken, 0.5cm particle is broken into；
B, stir-baked CORTEX EUCOMMIAE with salt solution coarse granule is added in Chinese medicine extracting tank, with water boiling and extraction 2 times, for the first time plus 9 times of amount water are heated
1h is decocted, second plus 7 times of amount water heating decoct 0.5h, extracting solution filtration；
C, the clear cream that relative density is 1.05 when filtrate decompression is condensed into 60 DEG C；
D, qinghuo reagent is added maltodextrin and dissolves and stir evenly, and is spray-dried, and dry extract is obtained, described spraying dry
Dry technological parameter are as follows: 175 DEG C~190 DEG C of inlet air temperature, 80 DEG C~90 DEG C of leaving air temp of control；
E, dry extract adds maltodextrin and magnesium stearate, is uniformly mixed, dry granulation obtains stir-baked CORTEX EUCOMMIAE with salt solution granule.
Comparative example 4: pot group type countercurrent extraction machine is used
A kind of preparation method of stir-baked CORTEX EUCOMMIAE with salt solution granule, includes the following steps:
A, stir-baked CORTEX EUCOMMIAE with salt solution medicine materical crude slice is taken, 0.5cm particle is broken into；
B, medicine materical crude slice is put into the series connection extractor group formed with 5 end to end extractors by the following arrangement mode that feeds intake
In, fresh solvent is added with material-water ratio 1:16 ratio in tail tank, is mentioned with 95 DEG C of each tank Extracting temperature, extraction time 1.5h
Take: the material in 5 tanks is successively new medicine materical crude slice, the dregs of a decoction after 1 time is extracted, the dregs of a decoction extracted through 2 times, the medicine extracted through 3 times
Fresh solvent is added in (dregs of a decoction after extracting equipped with the 4th) tank of most end by slag, the dregs of a decoction extracted through 4 times, other each
Tank is sequentially arranged with from the extracting solution that next stage tank transfer moves past and extracts, and final extracting solution is discharged from the tank of foremost,
The last extractor discharge dregs of a decoction are simultaneously packed into new medicine materical crude slice, become most preceding extractor, and so circulation is reverse extracts, and collect extracting solution
Filtration merges；
C, the extracting solution after merging filters after being cooled to 50 DEG C, and filtered fluid is 150 DEG C in supper high temperature instant sterilizer (UHT)
It is lower sterilizing 10 seconds, after at 60 DEG C be concentrated under reduced pressure at relative density be 1.05 clear cream；
D, qinghuo reagent is added maltodextrin and dissolves and stir evenly, and is spray-dried, and dry extract is obtained, described spraying dry
Dry technological parameter are as follows: 175 DEG C~190 DEG C of inlet air temperature, 80 DEG C~90 DEG C of leaving air temp of control；
E, maltodextrin and magnesium stearate is added in dry extract, is uniformly mixed, dry granulation obtains stir-baked CORTEX EUCOMMIAE with salt solution granule.
The stir-baked CORTEX EUCOMMIAE with salt solution granule that embodiment and comparative example is prepared measures Pinoresinol diglucoside content, meter
Paste-forming rate, rate of transform situation are calculated, the results are shown in Table 2:
2 stir-baked CORTEX EUCOMMIAE with salt solution granule embodiment of table is compared with comparative example result
Claims (10)
1. a kind of method for preparing Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granule using continuous dynamic countercurrent extraction process, which is characterized in that
Include the following steps:
A, continuous dynamic countercurrent extracts
Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution are broken into coarse granule, broken coarse granule is continuously inputted into Continuous Countercurrent Extraction machine by feed inlet
Extraction pipe, extraction pipe in by a set of helical structure by material continuously forward push to extraction pipe slag-drip opening slag tap, each
The end that grade extracts pipe continues that 10 ~ 25 times of hot water measured inversely are added, preferably 13 ~ 20 times amounts, and continuous dynamic countercurrent extraction 1 ~
3h, preferably 1.5 ~ 2.5h collect extracting solution, and the dregs of a decoction are discharged；
B, high-temperature short-time sterilization
It is refiltered after extracting solution cooling, filtrate is concentrated under reduced pressure through ultra high temperature short time sterilization, then under the conditions of 50 ~ 80 DEG C at relatively close
The clear cream that degree is 1.01 ~ 1.20；
C, it is spray-dried
Auxiliary material dissolution is added in qinghuo reagent, is spray-dried to obtain dry extract；
D, dry granulation
Pharmaceutical adjunct will be added in dry extract, dry granulation obtains Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granule.
2. the side according to claim 1 for preparing Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granule using continuous dynamic countercurrent extraction process
Method, which is characterized in that in step a, the broken coarse grained partial size is 0.3 ~ 0.8cm.
3. the side according to claim 1 for preparing Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granule using continuous dynamic countercurrent extraction process
Method, which is characterized in that in step a, input continuous dynamic countercurrent again after broken coarse granule to be first added to the water wetting of 1 ~ 5 times of amount
In extractor.
4. the side according to claim 1 for preparing Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granule using continuous dynamic countercurrent extraction process
Method, which is characterized in that in step a, the Continuous Countercurrent Extraction machine is spiral Continuous Countercurrent Extraction machine, is 10 section pipe of stage type
Structure.
5. the side according to claim 1 for preparing Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granule using continuous dynamic countercurrent extraction process
Method, which is characterized in that in step a, the temperature of the hot water is 60 ~ 95 DEG C, preferably 70 ~ 95 DEG C.
6. the side according to claim 1 for preparing Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granule using continuous dynamic countercurrent extraction process
Method, which is characterized in that in step a, the dregs of a decoction are then exhausted from after squeezing recovery section medical fluid, the part medical fluid and extracting solution of recycling
Merge.
7. the side according to claim 1 for preparing Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granule using continuous dynamic countercurrent extraction process
Method, which is characterized in that in step a, the Cortex Eucommiae or the coarse grained input speed of stir-baked CORTEX EUCOMMIAE with salt solution are 100 ~ 250kg/h, reverse to be added
The flow velocity of hot water is 1000 ~ 6250kg/h.
8. the side according to claim 1 for preparing Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granule using continuous dynamic countercurrent extraction process
Method, which is characterized in that in step b, refiltered after extracting solution is first cooled to 40 ~ 55 DEG C；The ultra high temperature short time sterilization be
It sterilizes 2~30 seconds at 100 ~ 150 DEG C in supper high temperature instant sterilizer.
9. the side according to claim 1 for preparing Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granule using continuous dynamic countercurrent extraction process
Method, which is characterized in that in step c, the auxiliary material is one of maltodextrin, dextrin, starch, lactose or beta-cyclodextrin or several
Kind；The technological parameter of the spray drying are as follows: 160 DEG C ~ 190 DEG C of inlet air temperature, 80 DEG C ~ 100 DEG C of leaving air temp of control.
10. according to claim 1 prepare Cortex Eucommiae or stir-baked CORTEX EUCOMMIAE with salt solution granule using continuous dynamic countercurrent extraction process
Method, which is characterized in that in step d, the pharmaceutical adjunct is maltodextrin, dextrin, starch, lactose, beta-cyclodextrin, titanium dioxide
One or more of silicon or magnesium stearate.
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