CN109432817A - A kind of the automation extraction separation method and granule preparation method of the Chinese medicine of the effective component containing thermal sensitivity - Google Patents
A kind of the automation extraction separation method and granule preparation method of the Chinese medicine of the effective component containing thermal sensitivity Download PDFInfo
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61J—CONTAINERS SPECIALLY ADAPTED FOR MEDICAL OR PHARMACEUTICAL PURPOSES; DEVICES OR METHODS SPECIALLY ADAPTED FOR BRINGING PHARMACEUTICAL PRODUCTS INTO PARTICULAR PHYSICAL OR ADMINISTERING FORMS; DEVICES FOR ADMINISTERING FOOD OR MEDICINES ORALLY; BABY COMFORTERS; DEVICES FOR RECEIVING SPITTLE
- A61J3/00—Devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Veterinary Medicine (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The present invention relates to a kind of automation extraction separation method of the Chinese medicine of effective component containing thermal sensitivity and granule preparation methods.The three-level separation of solid and liquid for automating extraction separation method and including Dynamic Extraction and being arranged in after Dynamic Extraction.The present invention can utmostly retain thermal sensitivity effective component, ensure that product quality indicator and economic indicator, improve extraction efficiency, improve separating effect, reduce production cost and energy consumption, ensure that each process equipment and pipeline meet the online site requirement of GMP.
Description
Technical field
The present invention relates to Chinese medicine production technical field more particularly to a kind of automation extraction process technologies of Chinese medicine.
Background technique
Extraction is the primary link and important operation unit of Chinese medicine production, and the superiority and inferiority of technique directly influences the matter of product
Amount.Traditional Chinese medicine extracting method includes decocting method, infusion process, circumfluence method, percolation, Gelatin improving method etc., but conventional method is deposited
In more disadvantage: 1) decocting method loss of effective components is more, especially water insoluble active ingredient;2) organic solvent in extraction process
It is possible that acting on effective component, it is made to lose original effectiveness;3) extract yield is low, extraction time is long, technique is cumbersome;4) Chinese medicine
Manufacturing enterprise is often used multi-function extractor at present and carries out boiling extraction, and temperature raising during the extraction process be easy to cause thermal sensitivity
Effective component changes.Chinese medicine thermal sensitivity effective component refers to the active constituent of case of thermal instability contained by Chinese medicine, these work
Property ingredient heat be easy decompose destroy, to influence drug effect.
Ultrasonic wave, microwave, supercritical CO are applied with the development of science and technology, gradually rising in recent years2The method of extraction carries out
It extracts, ultrasonic wave, multistage microwave amplifier can be obviously shortened extraction time, reduce energy consumption, but be not easy to realize commercial scale, and influence people
Health;Microwave has fuel factor, and heating is obvious under microwave action for the traditional Chinese medicine extractions such as water, ethyl alcohol common solvent, so
Microwave-assisted extraction technique is unsuitable for thermal sensitivity effective component;Supercritical CO2Suitable for extracting liposoluble substance, application range is relatively narrow,
And the thermal sensitivity effective component in drug is also vulnerable to destruction.
How to reduce the loss of thermal sensitivity effective component and improve its finished product transfer efficiency, is the key that promote traditional Chinese medicine quality
Subject under discussion.CN105147618A discloses a kind of preparation method of the free decoction of effective component containing thermal sensitivity agent, uses super-pressure
Extractive technique extracts the Chinese medicine containing thermal sensitivity effective component, is then filtered to extracting solution using micro-filter technology,
By filtrate concentration, dry, ultramicro grinding, medicinal extract fine powder is made to the free decoction preparation of the effective component containing thermal sensitivity.However, super
High pressure extraction technology high, high production cost for equipment requirement, is not suitable for being mass produced.
CN1339307A, which is disclosed, at low temperature leaches its Chinese herbal medicine with the charged extractor of dynamic, and using centrifugation point
Separation drying is carried out from effective component of the technique with freeze concentration and freeze-drying to Chinese herbal medicine.The entirety of the technique produced
Journey be all carried out under low-temperature condition, therefore do not destroy the effective component in medical fluid, and to its effective component especially thermal sensitivity at
Divide and plays maximum protection.However use low temperature extracting mode, the rate of transform of the paste-forming rate of product or other constituents
It is difficult to reach requirement.
CN102258883A discloses the dynamic circulation extracting method of a Plant Extracts, and plant material is in extraction process
It is middle that multiple dynamic circulation extraction is carried out using Extraction solvent, and use and force solvent circulation.Extraction solvent used is every time
1.5-3 times of material quality, solvent cycle-index are 2-5 times;Extracting total degree is 2-5 times.Work is extracted with conventional dynamic countercurrent
Skill is compared, and is had many advantages, such as that the raising of unit extract equipment utilization rate, apparatus adaptability are wide, simple for process, be can be applied to plant
The production of object extract is particularly suitable for the extraction of the plants active princlple such as thermal sensitivity, perishable.But the document is not specific
Provide the extraction example and extraction effect of thermal sensitivity effective component.
Traditional Chinese medicine extraction subsequent process is to be separated by solid-liquid separation, and dregs of a decoction physical features caused by different extraction processes are such as
The equal different froms such as viscosity, water content, solid granularity, and the form of the different Chinese medicine dregs of a decoction after extraction is also different, there is matter
Light floating material, also has sediment at suspended matter, and for the Chinese medicine of the effective component containing thermal sensitivity, the single separation of solid and liquid of tradition is
Make to be to configure advanced solid-liquid separating equipment and be also difficult to realize utmostly retain thermal sensitivity effective component, ensure that production
Quality figureofmerit and economic indicator.
CN102552400A, which is disclosed, to be filtered for Chinese medicine extract using plate and frame filter press, and disk plate centrifuge is then carried out
The second-order separation, be concentrated later using sub-prime, it is effective to retain thermal sensitivity, oxidisability, volatile ingredient in Chinese medical extract;
The advantage being concentrated using film, target component is retained, liquid is will transmit through and is concentrated, passes through the collection of membrane technology and concentration technique
At can both solve the problems, such as thermal sensitivity, oxidisability, the rate of transform of volatility pharmacodynamics index ingredient.But this method is at high cost, in
Medicine composition particle or general Chinese medicine solid orally ingestible such as use film concentration to will appear effective component instead and shut off and big, film are lost
The problems such as prevention and cure of pollution are not thorough, production efficiency is low.
Therefore, it is necessary to be improved to the traditional Chinese medicine extraction separate mode for the effective component containing thermal sensitivity, improves and extract
Efficiency and quality reduce production energy consumption, improve separating effect.
Summary of the invention
Problems to be solved by the invention
It is a kind of effective containing thermal sensitivity it is an object of the invention to design in order to solve the above-mentioned technical problem of the prior art
The automation extraction separation method of the Chinese medicine of ingredient and granule preparation method with utmostly retain thermal sensitivity effective component,
It ensures that product quality indicator and economic indicator, improves extraction efficiency, improve separating effect, reduce production cost and energy consumption,
Ensure that each process equipment and pipeline meet the online site requirement of GMP.
The solution to the problem
The present invention provides a kind of automation extraction separation method of the Chinese medicine of effective component containing thermal sensitivity, this method includes
Following steps,
(1) it feeds intake:
The raw material to be extracted of solvent and the effective component containing thermal sensitivity is sequentially added by metering into dynamic extraction pot body;
(2) Dynamic Extraction:
After the completion of feeding intake, open in tank raw material and solvent heat, heating rate be 0.5 DEG C/min~4 DEG C/min,
It is preferred that heating rate is 2 DEG C~3 DEG C/min, Extracting temperature is set as 60 DEG C~80 DEG C, 65~75 DEG C of preferable temperature;
Open stirring in the forced circulation and tank of dynamic extraction pot;
While dynamic extraction pot heating, program automatically begins to record and extracts the setting time decocted, decocts when extracting
After setting time reaches, extractor heating is closed, extracts end and out liquid;
(3) combined solid-liquid separates:
Successively using first-stage centrifugal machine or slag remover, filtering type solid-liquid separating machine and the second-order separation machine to from dynamic extraction pot
The extracting solution and the dregs of a decoction of interior outflow are combined formula separation of solid and liquid.
Further, decocting time (i.e. decoction soaking time) is set as 15~150 minutes, preferably decocting time 30~90
Minute.
Further, the first-stage centrifugal machine or slag remover are sedimentation-type centrifuge or slag remover, and preferably horizontal helical type removes
Slag machine;The filtering type solid-liquid separating machine is wet type shaking screen;The second-order separation machine is sedimentation-type centrifuge, preferably disk
Formula seperator.
Further, the first-stage centrifugal machine or slag remover liquid inlet volume are set as 4-6T/ hours, first-stage centrifugal machine or slagging-off
Owner's motor speed is 2300-2600 revs/min, and auxiliary-motor revolving speed is 1500-1900 revs/min.
Further, the vibration grit number of the wet type shaking screen is 100 mesh~250 mesh;The second-order separation machine into
Liquid measure is set as 3-4T/ hours, the deslagging period: 150-300 seconds, the deslagging time 0.1-1 seconds.
Further, the Dynamic Extraction step is normal pressure decoction.
Further, after the completion of the Dynamic Extraction step, software judges whether to need automatically according to the instruction sheet assigned
Execute program of clearing out a gathering place automatically: the alkali cleaning heating water cleaning after cleaning and whether needing replacing batch, kind including hot water;When
Into after program of clearing out a gathering place automatically, the control parameter that setting has been subjected to verifying in CIP on-line cleaning program is completed to equipment, pipeline
Automatic cleaning.
Further, the control parameter includes the washing time of dynamic extraction pot, cleaning feed liquor time, clean cycle
Delay time is completed in time, cleaning discharge;Delay time is completed in pipeline-cleaning feed liquor time, pipeline-cleaning discharge;First-stage centrifugal
Machine or slag remover, the washing time of filtering type solid-liquid separating machine and sedimentation-type centrifuge, pipeline-cleaning feed liquor time;Extracting solution storage
Delay time is completed in the washing time of tank, cleaning feed liquor time, cleaning discharge.
Further, the raw material to be extracted of the effective component of the present invention containing thermal sensitivity be selected from honeysuckle, chrysanthemum, Radix Angelicae Sinensis,
One of rheum officinale, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong, glutinous rehmannia, polygonum cuspidate, caulis lonicerae, pyrrosia lingua, paniculate swallowwort or stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice are a variety of, the solvent
For water.
Further, the raw material to be extracted for the effective component containing thermal sensitivity that the additive amount of the solvent is 10~25 times
Inventory;Particle size range < 1.0cm of the raw material to be extracted for the effective component containing thermal sensitivity that rate-determining steps (1) are added,
It is preferred that < 0.8cm.
The present invention also provides a kind of Chinese medicinal granule preparation methods of effective component containing thermal sensitivity, it is characterised in that:
This method includes such as present invention automation extraction separation method above-mentioned and concentration, drying and granulation step.
Further, the vacuum pressure of the concentration is -0.09~-0.08MPa, and thickening temperature is 60 DEG C ± 5 DEG C, described
It is dry dry selected from spray drying or vacuum bag, wherein in spray drying step material in spray drying tower body hot environment
Residence time is 15-20 seconds, and the control of dry materials temperature is in 30~70 DEG C when vacuum bag is dry.
The effect of invention
Compared with the prior art, the advantages of the present invention are as follows:
1) specific dynamic extraction pot is used, by select the medicinal material of specified particle size as extraction raw material, using dynamically mentioning
It takes the circulating pump T-M2 high frequency of tank stirring motor T-M1 and dynamic extraction pot to control, reaches technique and require forced circulation number, fill
Divide and utilize diffusion principle, be quickly dissolved in medicinal material effective component in solvent, improve and extract production efficiency, pressure makes medicinal material surface
Effective component reaches certain concentration difference, and extraction required temperature can be reduced by soaking dynamic process by temperature, reaches and boils extraction
Effect, and then heat-sensitive ingredients less loss rate is reduced, improve the rate of transform of heat-sensitive ingredients;
2) extracting solution in dynamic extraction pot and the dregs of a decoction combined solid-liquid separation assembly is imported together after extracting to carry out
Be separated by solid-liquid separation, thoroughly solves the problems, such as filter screen be easy blocking and clean it is unsuitable, the present invention creatively use three-level solid-liquid divide
From equipment, can continuous production, high production efficiency, at low cost and good separating effect, clarity are high, melting is good;
3) by being adjusted to heating rate, Extracting temperature, decocting time and spin-on filter device corresponding process parameters
Control, so that the indexs such as the paste-forming rate of product, the index components rate of transform, finished product clarity, melting relatively use Multifunction tank to divide 1-2
The technique of secondary extraction is enhanced, and the economic indicators such as amount of water and the daily output also have more than 20% compared with original process and change
It is kind;
4) automation Dynamic Extraction mode successfully realize the effective component containing thermal sensitivity Chinese Traditional Medicine it is each important
The computer auto-detection of technological parameter, control, monitoring are, it can be achieved that Automatic Control, standardized production, ensure that different batches
Stable product quality, well solved extraction process interference from human factor is more, production efficiency is lower, influence product quality
Etc. problems, realize standardization, scale, the automation of the traditional Chinese medicine extraction of the effective component containing thermal sensitivity;
5) present invention can be used single-effect concentrator and be concentrated, and thickening temperature can be effectively reduced, and protect effective component not
By high temperature, in spray drying step, material enters spray drying tower body to dry extract is dried to, in the high temperature environment
Residence time is of short duration, greatly reduces a possibility that destroying to heat-sensitive ingredients.
Detailed description of the invention
Fig. 1 is the structural representation that separator is extracted in Chinese medicine automation used in present invention automation extraction separation method
Figure.
Fig. 2 is the structural schematic diagram of Horizontal helical type centrifuge used in the present invention.
Description of symbols
T-1-dynamic extraction pot
T-2-horizontal helical type slag remover
T-3-wet type shaking screen
T-4-intermediate storage tank 1
T-5-intermediate storage tank 2
T-6-disc separator
T-7-extraction liquid storage tank
T-M1-dynamic extraction pot stirring motor
T-M2-dynamic extraction pot circulating pump
T-N1-dynamic extraction pot agitating paddle
T-N2-dynamic extraction pot circulation line
T-N3-extractor heating jacket
T-N4-extracting solution liquid control valve
TQRV-1-extractor jacket steam regulating valve
TQPT-1-extractor jacket steam pressure gauge
Steam pressure gauge in TQPT-2-extractor tank
Thermometer in TQTT-1-extractor tank
TQPV-1-extractor feed liquid control valve
TQLS-1-dynamic extraction pot liquid-level switch
1-auxiliary motor
2-main motors
3-differential mechanisms
4-rotary drums
5-discharge with endless screw devices
Specific embodiment
The present invention will be described in further detail below with reference to the embodiments of the drawings.
The present invention provides a kind of automation extraction separation methods of the Chinese medicine of effective component containing thermal sensitivity, and which employs spies
Separator is extracted in fixed Chinese medicine automation.
<separator is extracted in Chinese medicine automation>
As shown in Figure 1, separator is extracted in the automation of Chinese medicine used in the present invention comprising dynamic extraction pot T-1, combination
Formula is separated by solid-liquid separation component.
The tank body of the dynamic extraction pot T-1 is equipped with during the extraction process that recycle stock circulation extraction introducing tank is intracorporal
Circulation line T-N2, recycle stock include the Chinese medicine of the i.e. effective component containing thermal sensitivity of solvent and extract, and circulation line is equipped with
The design of circulating pump T-M2, circulation line and circulating pump will meet solvent and extract recycles together, and in cyclic process not
The character for destroying material, can enable whole tank material quickly be uniformly mixed, extractor feed liquid can be equipped on circulation line T-N2
Control valve TQPV-1, dynamic extraction pot liquid-level switch TQLS-1 are also provided with the row for slag liquid discharge on circulation line
Dirty branch pipe.The dynamic extraction pot inner cavity is equipped with multiple impellers T-N1, and agitating paddle is driven by dynamic extraction pot stirring motor T-M1
Dynamic, agitating paddle is preferably provided with not in tank body axial centerline, and agitating paddle is preferably three layers of agitating paddle, and top layer is press-down type,
The material of some floatings can be made to sink by stirring, middle layer is horizontal, can promote diffusion horizontally outward, promotes material
Dynamic exchange, lowest level are upper-turn-type, by promoting rolling material upwards, material are avoided to be deposited on tank bottom.The above agitating paddle
Design can make to reach better mixing effect in tank.The present invention utilizes dynamic extraction pot stirring motor T-M1 and dynamic extraction pot
The control of circulating pump T-M2 high frequency reaches technique and requires forced circulation number, makes full use of diffusion principle, make thermal sensitivity effective component
It is quickly dissolved in solvent, pressure makes the effective component on medicinal material surface reach certain concentration difference.
Dynamic extraction pot is additionally provided with feed intake unit and heating unit.The throwing of the unit that feeds intake completion solvent and raw material to be extracted
It puts, and delivering opportunity, injected volume is carried out and controlled, and open circulation and stirring launching terminal.Heating unit is to extraction body
System's heating makes temperature in extractor tank reach the temperature of technique initialization and be maintained at the temperature value of the technique initialization, is recorded in the work
Extraction time under the temperature value of skill setting.Heating unit includes extractor heating jacket T-N3, temperature in Detection and Extraction tank tank
Extractor tank in thermometer TQTT-1, be connected to extractor heating jacket steam pipe, the extraction on steam pipe pipeline is set
Tank jacket steam regulating valve TQRV-1, steam pressure gauge TQPT-2 in the extractor tank of steam pressure, inspection in Detection and Extraction tank tank
Survey the extractor jacket steam pressure gauge TQPT-1 of extractor jacket steam pressure.The present invention adjusts extractor collet by PID
Steam control valve TQRV-1 opening size, steadily reaches decoction temperature, effectively solves medicinal material after manual adjustment manual steam valve
The too fast, material that heats up when decoction runs material phenomenon.Preferably, each valve of dynamic extraction pot is controlled by PLC controller.Extraction terminates
Afterwards, by dynamic extraction pot extracting solution and the dregs of a decoction import combined type gas-liquid-solid together under the control of extracting solution liquid control valve T-N4
Liquid separation assembly is separated by solid-liquid separation.The dispensing unit of dynamic extraction pot includes the outlet tube with extracting solution liquid control valve T-N4
One end branch on road, the outlet tube road connects on circulation line, and the other end connects combined solid-liquid separation assembly.Of the invention one
In a possible embodiment, the bottom cover of dynamic extraction pot is not provided with filter plant.
Combined solid-liquid separation assembly of the present invention includes three solid-liquid separating equipments, is disposed with first-stage centrifugal machine
Or slag remover, filtering type solid-liquid separating machine and the second-order separation machine, the first-stage centrifugal machine or slag remover, filtering type solid-liquid separating machine
Feed lines connection is passed sequentially through between the second-order separation machine three.
Further, the first-stage centrifugal machine or slag remover are sedimentation-type centrifuge or slag remover, and effect is to by slag liquid
Carry out initial gross separation, with the difference of specific gravity separating most solid dregs of a decoction, in the specific embodiment of the present invention level-one from
Scheming or slag remover are preferably horizontal helical type slag remover T-2.Horizontal helical type slag remover is generally used for the fields such as water process, the invention
Property the biggish horizontal helical type slag remover for the treatment of capacity is used for traditional Chinese medicine extraction separation process, the traditional Chinese medicine extraction that compares separation is conventional to be used
The biggish link-suspended basket centrifuge for the treatment of capacity or flat centrifuge, horizontal helical type slag remover allow continuous production and inside it
Be conducive to the cleaning of the dregs of a decoction with screw machine structure.In the specific embodiment of the present invention, as shown in Fig. 2, sleeping spiral shell
Formula centrifuge includes rotary drum (4), discharge with endless screw device (5), motor, differential mechanism (3), and the discharge with endless screw device (5) is arranged in rotary drum
(4) in, walking feeding tube is inserted in discharge with endless screw device (5), one end of walking feeding tube is feed inlet, and the other end is as discharge port, rotary drum
(4) it close to one end of feed inlet as purified liquor outlet, is exported close to one end of discharge port as sediment, the motor includes being used for
Control the main motor (2) of charging and the auxiliary motor (1) for controlling differential mechanism (3).
By horizontal helical type slag remover, liquid enters filtering type solid-liquid separating machine out, and the effect of filtering type solid-liquid separating machine is logical
Partial size difference is crossed to separate, filter a small amount of impurity so that filtrate can satisfy the requirement of disc separator feed liquor.In this hair
Filtering type solid-liquid separating machine is wet type shaking screen T-3 in a bright specific embodiment, and wet type shaking screen is relative to routine
Filter plant, what is taken due to wet type shaking screen is dynamic filtration, avoids a large amount of fine powders blocking opening of sieves, and treating capacity
Greatly, it can be achieved that continuous production.
The effect of the second-order separation machine of the invention is to remove pulp and impurity and most of impurity for being gathered in sediment area,
The main effect for playing refined filtration, preferably sedimentation-type centrifuge, separate in the specific embodiment of the present invention for disc-type
Machine T-6.For disc separator for the tube centrifuge of same type, production capacity is bigger and is able to achieve continuous production.Consider
It is variant to the processing capacity between disc separator and the solid-liquid separating equipment of preceding second level, preferably it is separated by solid-liquid separation in filtering type
Intermediate storage tank 1T-4 and high-order intermediate storage tank 2T-5 are set between machine and the second-order separation machine, to adapt to disc centrifuge top
The operating mode of portion's feed liquor.
The second-order separation machine needs successively to be used in combination and could reach with above-mentioned first-stage centrifugal machine and filtering type solid-liquid separating machine
To high efficiency and the separating resulting of good separating effect.If horizontal helical type slag remover is used alone, separating effect is bad, extracting solution
Turbidity is high, if wet type shaking screen is used alone, solid bulky grain is easy blocking sieve screen apertures, if disc separator is used alone,
Also due to melt cinder partial size is big, impurity level is big, cannot exclude in time, is easy to happen blocking.If only combination horizontal helical type slag remover and
Wet type shaking screen, no refined filtration step can clarity to product and melting have large effect.In addition, three separation of solid and liquid
Equipment is because of its effect and is separated by solid-liquid separation principle and production capacity difference, and the sequence of three is specific in the present invention, only successively
It is just able to achieve good separating effect of the present invention by three solid-liquid separating equipments, if connected using different order
It will affect its treating capacity and separative efficiency, while being also easy to that equipment is caused to block.
<Chinese medicine of the effective component containing thermal sensitivity automates extraction separation method>
Separator, the Chinese medicine automation of the effective component of the invention containing thermal sensitivity are extracted based on above-mentioned Chinese medicine automation
Extraction separation method includes Dynamic Extraction and the separation of solid and liquid that is arranged in after Dynamic Extraction.
Wherein Dynamic Extraction is to extract raw material by solvent (water) minute-pressure, and the form of feeding intake of raw material to be extracted need to meet material
It can be recycled together with solvent, therefore the present invention needs to control the particle size range of raw material to be extracted, the partial size model of raw material to be extracted
< 1.0cm is enclosed, preferably < 0.8cm can be realized by the pretreatment to raw material, if partial size is excessive, will be unfavorable for adequately strong
System circulation, while subsequent separation process is adversely affected.
The Chinese medicine automation extraction separation method key step of the effective component of the present invention containing thermal sensitivity is as follows:
(1) it feeds intake:
The raw material to be extracted for extracting raw material, that is, specified particle diameter effective component containing thermal sensitivity is moved at feeding port, first
It opens solvent and adds control valve, start to measure the solvent being added into extractor body, the additive amount of solvent using electromagnetic flowmeter
The inventory of the raw material to be extracted of generally 10~25 times of the effective component containing thermal sensitivity, when solvent amount reaches predetermined process setting
After value, raw material to be extracted is from feeding port investment extractor T-1.Solvent adding too much then increases system circulating load, increases
Production cost, solvent additive amount is too low, extract to meeting to thermal sensitivity effective component with being unable to fully, and influences going out for product
Cream rate and the index components rate of transform.The raw material to be extracted of the effective component of the present invention containing thermal sensitivity be selected from honeysuckle, chrysanthemum,
One of Radix Angelicae Sinensis, rheum officinale, Radix Salviae Miltiorrhizae, rhizome of chuanxiong, glutinous rehmannia, polygonum cuspidate, caulis lonicerae, pyrrosia lingua, paniculate swallowwort or stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice are a variety of, commonly
Solvent is one of water, the alcohols solvent of C1-6, halogenated hydrocarbons or a variety of, and preferably water or ethyl alcohol, solvent can be according to medicinal materials
Dissolubility is selected.
(2) Dynamic Extraction:
After the completion of click feeds intake, automatically turning on steam control valve makes to start to be passed through steam in extractor heating jacket, to tank
Interior raw material and solvent is heated;While extractor heating jacket T-N3 heating, by being mounted on mentioning for tank body side bottom
The temperature of thermometer real-time online Detection and Extraction liquid in tank tank is taken, and PLC program is according to the mesh of temperature in steam pressure, extractor
Scale value is controlled the aperture of extractor jacket steam regulating valve TQRV-1 by PID regulative mode, made on the temperature plateau of extracting solution
It rises, when thermometer reaches the temperature of technique initialization in extractor tank and is maintained at technique initialization temperature value, heating rate 0.5
DEG C/min~4 DEG C/min, heat-sensitive ingredients are degraded by heat damage in order to prevent, to be shortened heating as far as possible and be extracted heated
Time, while it is also contemplated that the heating-up time too short effective dissolution for being unfavorable for heat-sensitive ingredients, therefore can raising heating appropriate
Rate shortens the heating-up time, preferably 2~3 DEG C/min of heating rate range, and set temperature is 60~80 DEG C, preferred range
70 DEG C ± 5 DEG C, temperature is excessively high to destroy thermal sensitivity effective component, and temperature is too low, will affect extraction quality.
The circulating pump T-M2 in fluid circulation is extracted in starting while heating, to extracting solution forced circulation, constantly
The liquid in extractor from pot bottom is extracted, extractor is returned from the top of extractor from newly by pipeline with pump, passes through liquid
Body circulates, and enhances the contact between solid-liquid two-phase, and enhancing effective component dissolves out inside medicinal material.Circulating pump T-M2 is logical
The flow of frequency converter frequency control circulation fluid is crossed to reach corresponding cycle-index, cycle-index is 5~20 times per hour;Simultaneously
Dynamic extraction pot stirring motor T-M1 variable frequency starting is stirred solvent to reach the concentration of pharmaceutical decocting piece surface effective component
Difference.The pressure inside the tank of dynamic extraction pot is normal pressure.
In addition, PLC program can automatically record the setting time extracted and decocted, it is however generally that decocting time (decocts heat preservation
Time) it is 15~150 minutes, preferably decocting time range 30~90 minutes.After extraction, which decocts setting time, to be reached, closing is mentioned
Tank jacket steam regulating valve is taken, extracting terminates and start liquid out.It can effectively be solved by automatically accurate recording decocting time
The problem of certainly artificial too short medicinal material yield of decocting time is low, and decocting time is long, thermal sensitivity effective component is more easily damaged.
During taking liquid to go out liquid, be first turned on extracting solution liquid control valve T-N4, by extracting solution circulating pump T-M2 into
Enter to be separated by solid-liquid separation, after determining feed liquid emptying by detection dynamic extraction pot liquid level detecting switch, extractor circulating pump T-M2, extract
Tank stirring motor T-M1 is shut down, and closes corresponding control valve.Extracting solution can also be derived during going out liquid using program inner equation
The extraction yield of this batch materials and compared with setting empirical value in the past, inside program under automatic fine tuning batch materials Dynamic Extraction throwing
Doses, amount of water, temperature, time parameter.
(3) combined solid-liquid separates:
It is successively preferably wet using first-stage centrifugal machine or the preferred horizontal helical type slag remover T-2 of slag remover, filtering type solid-liquid separating machine
The formula shaking screen T-3 and preferred disc separator T-6 of the second-order separation machine is combined formula to extracting solution and the dregs of a decoction and is separated by solid-liquid separation.
In order to preferably carry out the effective component containing thermal sensitivity Chinese medicine extract and the dregs of a decoction separation, need to control level-one from
The feed speed and screw speed of scheming or slag remover, the vibration grit number of wet type shaking screen and the second-order separation machine revolving speed,
The technological parameters such as deslagging gap.The inventors discovered that separating excellent effect when using following parameter: first-stage centrifugal machine or slag remover
Liquid inlet volume is set as 4~6T/ hours, and 2300~2600 revs/min of main motor revolving speed, 1500~1900 revs/min of auxiliary-motor revolving speed
Clock, may be implemented out that liquid slag inclusion is few, the dregs of a decoction are dry;The vibration grit number of wet type shaking screen can both guarantee to locate when being 100~250 mesh
Reason amount can remove the dregs of a decoction of greater particle size again;The liquid inlet volume of the second-order separation machine is set as 3-4T/ hours, the deslagging period:
150-300 seconds, the deslagging time 0.1-1 seconds, it help to obtain clear filtrate.
In a preferred embodiment of the present invention, after the completion of Dynamic Extraction step, software is automatically according to assigning
Instruction sheet judges whether to need to be implemented program of clearing out a gathering place automatically: the alkali after cleaning and whether needing replacing batch, kind including hot water
Cleaning heating water cleaning;After program is cleared out a gathering place in entrance automatically, setting has been subjected to the control ginseng of verifying in CIP on-line cleaning program
Count up to the automatic cleaning of pairs of equipment, pipeline.
The control parameter includes the washing time of dynamic extraction pot, cleaning feed liquor time, clean cycle time, cleaning row
Discharge into delay time;Delay time is completed in pipeline-cleaning feed liquor time, pipeline-cleaning discharge;First-stage centrifugal machine or slag remover,
The washing time of filtering type solid-liquid separating machine and sedimentation-type centrifuge, pipeline-cleaning feed liquor time;When extracting the flushing of liquid storage tank
Between, cleaning the feed liquor time, cleaning discharge complete delay time.
In general the extraction separator of prior art Chinese medicine has no the CIP on-line cleaning stream of independent alkali cleaning heating water
Cheng Chengxu, the general separator that extracts clear out a gathering place program also according to former extraction and separation process process program, in production server system
It can be inquired in system without corresponding cleaning record.The invention introduces CIP on-line cleaning process program, can be individually right
Equipment, pipeline alkali cleaning or hot water wash are selected, and cleaning and drain time etc. can be separately provided.
Respectively cleared out a gathering place the time according to what is had verified that, the present invention using automation control program complete each equipment (dynamic extraction pot,
Horizontal helical type centrifuge, wet type shaking screen, disc centrifuge etc.), the purpose of clearing out a gathering place of each process pipeline, automatically complete to closing
Formula equipment and pipeline ensure that each process equipment meets with pipeline without dead angle, no manual intervention, requirement of clearing out a gathering place online at regular time and quantity
The online site requirement of GMP.
<the granule preparation method of the Chinese medicine of the effective component containing thermal sensitivity>
Chinese medicinal granule is made of the extracted concentration of the prepared slices of Chinese crude drugs, for the particle of tcm clinical practice formula.It is
It based on the clinical use of traditional Chinese herbal decoction, is used under instruction of Chinese Medicine theory, but compared with traditional traditional Chinese herbal decoction, it has
Convenient to take, easy storage, Portable belt, it is quality controllable the features such as.The present invention also provides in a kind of effective component containing thermal sensitivity
Medicine composition preparation method of granules, this method include present invention automation extraction separation method above-mentioned and concentration, drying and system
Grain step.This method is especially suitable for Chinese medicine one-component formulation particle manufacture.
The clear filtrate pump of gained will be separated by solid-liquid separation to be used as medicine liquid storage tank, then drawing liquid is to concentration tank, in order to farthest subtract
Few loss to thermal sensitivity effective component, the present invention are concentrated using single-effect concentrator, and thickening temperature can be effectively reduced, dense
The vacuum pressure of contracting is -0.09~-0.08MPa, and thickening temperature is 60 DEG C ± 5 DEG C.Clear cream, then drawing liquid are obtained by vacuum concentration
To spray drying tower, 165~195 DEG C and 80~105 DEG C of leaving air temp of the inlet air temperature of concentrate, material stops in the high temperature environment
Stay time 15-20 second;Or clear cream is dry through vacuum bag, and dry materials temperature is 30~70 DEG C, drying time is 0.5~
2.5 hours, a possibility that heat-sensitive ingredients destruction, is reduced.Material after drying is crushed, and xeraphium is directly made
Necessary auxiliary material is added in grain in spray dried powder;It pelletizes to obtain one-component formulation particle.Auxiliary material can be carbohydrate auxiliary material, such as
Starch, soluble starch, dextrin, sucrose or mannitol.These auxiliary materials can be used alone, and several can also be used in mixed way, with
Improve the mouthfeel of particle.Method of granulating of the present invention includes dry pressing granulation and fluidized bed granulation.
Using this method simple production process, it is possible to reduce the loss of thermal sensitivity effective component, the formula being prepared
Grain melting is good, clarity is high after dissolution.
Embodiment
Carry out the technical solution during the present invention is further explained below with reference to specific embodiment.Under it should be understood that
Column embodiment is only used for the explanation and illustration present invention, and the protection scope being not intended to restrict the invention.
Embodiment 1
The present embodiment is related to the preparation of honeysuckle one-component formulation particle.It uses Chinese medicine automation shown in FIG. 1 to extract
Separator carries out automation and extracts separation.
(1) it feeds intake:
Honeysuckle is pre-processed, partial size < 1cm is cut to;
The honeysuckle 100KG of partial size < 1cm is moved at feeding port, solvent (water) addition control valve, benefit are first turned on
Start metering to 3M with electromagnetic flowmeter3Dynamic extraction pot body in the solvent that is added, the additive amount of water is 20 times of honeysuckles
Inventory is put into extractor T-1 after solvent amount reaches predetermined process setting value from feeding port by honeysuckle.
(2) Dynamic Extraction:
After the completion of click feeds intake, automatically turning on steam control valve makes to start to be passed through steam in extractor heating jacket, to tank
Interior honeysuckle and water is heated;While extractor heating jacket T-N3 heating, by being mounted on mentioning for tank body side bottom
The temperature of thermometer real-time online Detection and Extraction liquid in tank tank is taken, and PLC program is according to the mesh of temperature in steam pressure, extractor
Scale value is controlled the aperture of extractor jacket steam regulating valve TQRV-1 by PID regulative mode, made on the temperature plateau of extracting solution
It rises, when thermometer reaches the temperature of technique initialization in extractor tank and is maintained at technique initialization temperature value, heating rate 2
DEG C/min, set temperature is 70 DEG C.
The circulating pump T-M2 in fluid circulation is extracted in starting while heating, to extracting solution forced circulation.Circulating pump
T-M2 is reached by the flow of frequency converter frequency control circulation fluid to be recycled 16 times per hour;Dynamic extraction pot stirring motor simultaneously
T-M1 variable frequency starting is stirred solvent to reach the concentration difference of pharmaceutical decocting piece surface effective component.Dynamic extraction pot is using normal
Pressure decocts.
PLC program automatically records the setting time extracted and decocted, decocting time 1h.Reach when extracting decoction setting time
Afterwards, extractor jacket steam regulating valve is closed, extracting terminates and start liquid out.
During extracting solution goes out liquid, it is first turned on extracting solution liquid control valve T-N4, passes through extracting solution circulating pump T-M2
It extractor circulating pump T-M2, is mentioned after determining feed liquid emptying by detection dynamic extraction pot liquid level detecting switch into separation of solid and liquid
It takes tank stirring motor T-M1 to shut down, closes corresponding control valve.
(3) combined solid-liquid separates:
Extracting solution in extractor is imported combined solid-liquid separation assembly to be separated by solid-liquid separation, is successively removed by horizontal helical type
Slag machine T-2, wet type shaking screen T-3, disc separator T-6.
Extracting solution in extractor is pumped into horizontal helical type slag remover, and liquid inlet volume is set as 4T/ hours, the setting of main motor revolving speed
2500 revs/min, auxiliary-motor revolving speed sets 1600 revs/min, and the extracting solution after slagging-off passes through wet type shaking screen, vibrates grit number
For 100 mesh, then it is pumped into relay reservoir, flows into disc separator afterwards, liquid inlet volume is set as 2.5T/ hours, the deslagging period: 300
Second, the deslagging time: 0.3 second.
(4) it is concentrated, dry and granulation
The clear filtrate pump of gained after disc separator is used as medicine liquid storage tank, then drawing liquid is to concentration tank, concentration
Vacuum pressure is -0.09~-0.08MPa, and concentration time 1.5h, thickening temperature is 60 DEG C, and being concentrated in vacuo to specific gravity is 1.08
85 DEG C of~1.12 clear cream, then drawing liquid is to spray drying tower, 175 DEG C~195 DEG C of spray drying EAT and leaving air temp~
95 DEG C, it is dry after material crushed, honeysuckle can be obtained by adding the auxiliary materials such as maltodextrin and carrying out granulation
One-component formulation particle.
Embodiment 2
The present embodiment is related to the preparation of chrysanthemum one-component formulation particle.It is also extracted using Chinese medicine shown in FIG. 1 automation
Separator.
(1) it feeds intake:
Chrysanthemum is pre-processed, partial size < 1cm is cut to;
The chrysanthemum 100KG of partial size < 1cm is moved at feeding port, solvent (water) addition control valve is first turned on, utilizes
Electromagnetic flowmeter starts metering to 3M3Dynamic extraction pot body in the solvent that is added, the additive amount of water is feeding intake for 20 times of chrysanthemums
Amount is put into extractor T-1 after solvent amount reaches predetermined process setting value from feeding port by chrysanthemum.
(2) Dynamic Extraction:
After the completion of click feeds intake, automatically turning on steam control valve makes to start to be passed through steam in extractor heating jacket, to tank
Interior chrysanthemum and water is heated;While extractor heating jacket T-N3 heating, by the extraction for being mounted on tank body side bottom
The temperature of thermometer real-time online Detection and Extraction liquid in tank tank, and PLC program is according to the target of temperature in steam pressure, extractor
Value is controlled the aperture of extractor jacket steam regulating valve TQRV-1 by PID regulative mode, made on the temperature plateau of extracting solution
It rises, when thermometer reaches the temperature of technique initialization in extractor tank and is maintained at technique initialization temperature value, heating rate 2
DEG C/min, set temperature is 70 DEG C.
The circulating pump T-M2 in fluid circulation is extracted in starting while heating, to extracting solution forced circulation.Circulating pump
T-M2 is reached by the flow of frequency converter frequency control circulation fluid to be recycled 16 times per hour;Dynamic extraction pot stirring motor simultaneously
T-M1 variable frequency starting is stirred solvent to reach the concentration difference of pharmaceutical decocting piece surface effective component.Dynamic extraction pot is normal pressure
It decocts.
PLC program automatically records the setting time extracted and decocted, and decocting time is 45 minutes.Setting time is decocted when extracting
After reaching, extractor jacket steam regulating valve is closed, extracting terminates and start liquid out.
During extracting solution goes out liquid, it is first turned on extracting solution liquid control valve T-N4, passes through extracting solution circulating pump T-M2
It extractor circulating pump T-M2, is mentioned after determining feed liquid emptying by detection dynamic extraction pot liquid level detecting switch into separation of solid and liquid
It takes tank stirring motor T-M1 to shut down, closes corresponding control valve.
(3) combined solid-liquid separates:
Extracting solution in extractor is imported combined solid-liquid separation assembly to be separated by solid-liquid separation, is successively removed by horizontal helical type
Slag machine T-2, wet type shaking screen T-3, disc separator T-6.
Extracting solution in extractor is pumped into horizontal helical type slag remover, and liquid inlet volume is set as 4T/ hours, the setting of main motor revolving speed
2500 revs/min, auxiliary-motor revolving speed sets 1600 revs/min, and the extracting solution after slagging-off passes through wet type shaking screen, vibrates grit number
For 100 mesh, then it is pumped into relay reservoir, flows into disc separator afterwards, liquid inlet volume is set as 2.5T/ hours, the deslagging period: 250
Second, the deslagging time: 0.3 second.
(4) it is concentrated, dry and granulation
The clear filtrate pump of gained after disc separator is used as medicine liquid storage tank, then drawing liquid, to concentration tank, concentration is true
Pneumatics power be -0.09~-0.08MPa, concentration time 1.5h, thickening temperature be 60 DEG C, be concentrated in vacuo to specific gravity be 1.08~
1.12 clear cream, then drawing liquid is to spray drying tower, 175 DEG C~195 DEG C of spray drying EAT and leaving air temp 85 DEG C~95
DEG C, it is dry after material crushed, chrysanthemum single group can be obtained by adding the auxiliary materials such as maltodextrin and carrying out granulation
Divide granule.
Comparative example 1
This comparative example is related to honeysuckle one-component formulation particle preparation same as Example 1, and raw material inventory is identical, molten
Matchmaker is water.Difference is using conventional 3M3Multi-function extractor and conventional solid-liquid separating equipment PD1250 hanging bag discharging from
Scheming.Specifically, honeysuckle is put into multi-function extractor, extracting in water is secondary, adds 14 times of medicine materical crude slice amount of water for the first time,
100 DEG C of temperature extractions take 1 hour;Second plus 12 times of medicine materical crude slice amount of water, 100 DEG C of temperature extractions take 0.5 hour, utilize PD1250 hanging bag
Conveyer centrifugal carries out centrifugal filtration, carries out concentration, drying and granulation as described in 1 step of embodiment (4) later, obtains gold and silver
Flower granule.
Comparative example 2
This comparative example is related to honeysuckle one-component formulation particle preparation same as Example 1, and raw material inventory is identical, molten
Matchmaker is water.Difference is using conventional 3M3Multi-function extractor and 200 mesh bag filters.Specifically, honeysuckle is thrown
Enter multi-function extractor, extracting in water is secondary, adds 14 times of medicine materical crude slice amount of water for the first time, and 70 DEG C of temperature extractions take 1 hour;Add for the second time
The water that 12 times of medicine materical crude slice amount, 70 DEG C of temperature extractions take 0.5 hour, and extracting solution crosses 200 mesh bag filters, carries out such as embodiment 1 later
Concentration, drying and granulation described in step (4) obtain honeysuckle dispensing granule.
Comparative example 3
This comparative example is related to honeysuckle one-component formulation particle preparation same as Example 1, and raw material inventory is identical, molten
Matchmaker is water.Difference is that the Extracting temperature of step (2) is 50 DEG C.
Comparative example 4
This comparative example is related to honeysuckle one-component formulation particle preparation same as Example 1, and raw material inventory is identical, molten
Matchmaker is water.Difference is that the Extracting temperature of step (2) is 85 DEG C.
Comparative example 5
This comparative example is related to honeysuckle one-component formulation particle preparation same as Example 1, and raw material inventory is identical, molten
Matchmaker is water.Difference is that the heating rate of step (2) is 5 DEG C/min.
Comparative example 6
This comparative example is related to honeysuckle one-component formulation particle preparation same as Example 1, and raw material inventory is identical, molten
Matchmaker is water.Difference is that the heating rate of step (2) is 0.2 DEG C/min.
Comparative example 7
This comparative example is related to honeysuckle one-component formulation particle preparation same as Example 1, and raw material inventory is identical, molten
Matchmaker is water.Dynamic Extraction equipment and technique and subsequent concentration, drying and granulating process are same as Example 1, difference be by
Step (3) is only with second level solid-liquid separating equipment (horizontal helical type slag remover+disc centrifuge).Horizontal helical type slag remover and disc-type
The job parameter and embodiment 1 of centrifuge are consistent.
Comparative example 8
This comparative example is related to honeysuckle one-component formulation particle preparation same as Example 1, and raw material inventory is identical, molten
Matchmaker is water.Dynamic Extraction equipment and technique and subsequent concentration, drying and granulating process are same as Example 1, difference be by
Step (3) is only with second level solid-liquid separating equipment (horizontal helical type slag remover+wet type shaking screen).Horizontal helical type slag remover and wet type oscillation
The job parameter and embodiment 1 of sieve are consistent.
Comparative example 9
This comparative example is related to honeysuckle one-component formulation particle preparation same as Example 1, and raw material inventory is identical, molten
Matchmaker is water.Dynamic Extraction equipment and technique and subsequent concentration, drying and granulating process are same as Example 1, difference be by
The horizontal helical type slag remover of step (3) is changed to slag dumping filter centrifugal under 3-foot, and disc centrifuge is changed to tubular type clarification type
Ultracentrifuge adjusts the equipment of slag dumping filter centrifugal and tubular type clarification type ultracentrifuge ginseng under 3-foot according to practical
Number.The job parameter and embodiment 1 of wet type shaking screen are consistent.
To the embodiment of the present invention 1, embodiment 2, the production efficiency of the technique of comparative example 1 to comparative example 9 and energy consumption and production
The meltings of product, clarity, chlorogenic acid rate of transform etc. carry out comprehensive analysis, and concrete outcome is shown in Table 1.
The content of prepared Honegsukle flower P.E Content of Chlorogenic Acid in embodiment 1 according to the present invention and comparative example 1~9
Using high effective liquid chromatography for measuring, method particularly includes: using octadecylsilane chemically bonded silica as filler;With acetonitrile 0-.4%
Phosphoric acid solution (13: 87) is mobile phase;Detection wavelength is 327nm.Flow velocity is 1.0ml/min, and test sample sample volume is 10 μ l, green
Ortho acid reference substance sample volume is 5 μ l.
The content of the chrysanthemum extract Content of Chlorogenic Acid of embodiment 2 according to the present invention is surveyed using high performance liquid chromatography
It is fixed, method particularly includes: using octadecylsilane chemically bonded silica as filler;Using -0.1% phosphoric acid solution of acetonitrile as mobile phase;Inspection
Survey wavelength is 348nm.Flow velocity is 1.0ml/min, and test sample sample volume is 10 μ l, and chlorogenic acid reference substance sample volume is 5 μ l.
It is green in the extract Content of Chlorogenic Acid rate of transform (%)=paste-forming rate (%) × extract Content of Chlorogenic Acid (%)/medicine materical crude slice
Determination of Chlorogenic Acid (%).
The other production technology of the different groups of table 1 and product quality compare
By the comparison of table 1 it is found that the technique that the multi-function extractor conventional compared to use is repeatedly decocted, this hair
Bright to produce by using Dynamic Extraction and three-level solid-liquid separation process, paste-forming rate, the chlorogenic acid rate of transform, the finished product of product are clear and bright
The quality index such as degree, melting are greatly improved, and the economic indicators such as amount of water also have more than 20% improvement compared with original process.This
Invention can improve chlorogenic acid content while obtaining higher paste-forming rate by the control to Extracting temperature and heating rate
And the rate of transform.It compares and is separated by solid-liquid separation only with second level, the solid-liquid separating equipment that the present invention is applied in combination three kinds may be implemented to connect
Continuous production, the chlorogenic acid rate of transform does not decline but extract rushes molten rear clarity height;Compared to other three-level separation methods, this hair
The total amount that feed intake tomorrow is big, the high production efficiency and chlorogenic acid rate of transform is relatively higher.
In addition to the implementation, all to use equivalent transformation or equivalent replacement the invention also includes there is an other embodiments
The technical solution that mode is formed should all be fallen within the scope of the hereto appended claims.
Claims (10)
1. a kind of automation extraction separation method of the Chinese medicine of effective component containing thermal sensitivity, it is characterised in that: this method includes such as
Lower step,
(1) it feeds intake:
The raw material to be extracted of solvent and the effective component containing thermal sensitivity is sequentially added by metering into dynamic extraction pot body;
(2) Dynamic Extraction:
After the completion of feeding intake, open in tank raw material and solvent heat, heating rate be 0.5 DEG C/min~4 DEG C/min, preferably
Heating rate is 2 DEG C~3 DEG C/min, sets Extracting temperature as 60 DEG C~80 DEG C, 65~75 DEG C of preferable temperature;
Open stirring in the forced circulation and tank of dynamic extraction pot;While dynamic extraction pot heating, program automatically begins to remember
The setting time decocted is extracted in record, after extraction, which decocts setting time, to be reached, is closed extractor heating, is extracted end and out liquid;
(3) combined solid-liquid separates:
Successively flowed using first-stage centrifugal machine or slag remover, filtering type solid-liquid separating machine and the second-order separation machine to out of dynamic extraction pot
Extracting solution and the dregs of a decoction out is combined formula separation of solid and liquid.
2. the automation extraction separation method of the Chinese medicine of the effective component according to claim 1 containing thermal sensitivity, feature exist
In:
Decocting time is set as 15~150 minutes, preferably decocting time is 30~90 minutes.
3. the automation extraction separation method of the Chinese medicine of the effective component according to claim 1 or 2 containing thermal sensitivity, feature
It is:
The first-stage centrifugal machine or slag remover are sedimentation-type centrifuge or slag remover, preferably horizontal helical type slag remover;The filtering
Formula solid-liquid separating machine is wet type shaking screen;The second-order separation machine is sedimentation-type centrifuge, preferably disc separator.
4. the automation extraction separation method of the Chinese medicine of the effective component according to claim 3 containing thermal sensitivity, feature exist
In:
The first-stage centrifugal machine or slag remover liquid inlet volume are set as 4-6T/ hours, first-stage centrifugal machine or slag remover main motor revolving speed
It is 2300-2600 revs/min, auxiliary-motor revolving speed is 1500-1900 revs/min.
5. the automation extraction separation method of the Chinese medicine of the effective component according to claim 3 or 4 containing thermal sensitivity, feature
It is:
The vibration grit number of the wet type shaking screen is 100 mesh~250 mesh;The liquid inlet volume of the second-order separation machine is set as 3-
4T/ hours, the deslagging period: 150-300 seconds, the deslagging time 0.1-1 seconds.
6. the automation extraction separation method of the Chinese medicine of the effective component according to claim 1-5 containing thermal sensitivity,
It is characterized by:
After the completion of the Dynamic Extraction step, software judges whether to need to be implemented automatically according to the instruction sheet assigned clears out a gathering place automatically
Program: the alkali cleaning heating water cleaning after cleaning and whether needing replacing batch, kind including hot water;When the automatic journey of clearing out a gathering place of entrance
After sequence, the control parameter that setting has been subjected to verifying in CIP on-line cleaning program completes the automatic cleaning to equipment, pipeline.
7. the automation extraction separation method of the Chinese medicine of the effective component according to claim 1-6 containing thermal sensitivity,
It is characterized by:
The raw material to be extracted of the effective component containing thermal sensitivity be selected from honeysuckle, chrysanthemum, Radix Angelicae Sinensis, rheum officinale, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong, glutinous rehmannia,
One of polygonum cuspidate, caulis lonicerae, pyrrosia lingua, paniculate swallowwort or stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice are a variety of, and the solvent is water.
8. the automation extraction separation method of the Chinese medicine of any one of -6 effective component containing thermal sensitivity according to claim 1, special
Sign is:
The inventory of the raw material to be extracted for the effective component containing thermal sensitivity that the additive amount of the solvent is 10~25 times;Control
Particle size range < the 1.0cm, preferably < 0.8cm of the raw material to be extracted for the effective component containing thermal sensitivity that step (1) is added.
9. a kind of Chinese medicinal granule preparation method of effective component containing thermal sensitivity, it is characterised in that: this method includes such as right
It is required that the described in any item automation extraction separation methods of 1-8 and concentration, drying and granulation step.
10. a kind of Chinese medicinal granule preparation method of effective component containing thermal sensitivity according to claim 9, feature exist
In: the vacuum pressure of the concentration is -0.09~-0.08MPa, and thickening temperature is 60 DEG C ± 5 DEG C, and the drying is selected from spraying dry
Dry or vacuum bag is dry, and wherein material residence time in spray drying tower body hot environment is 15- in spray drying step
20 seconds, the control of dry materials temperature was in 30~70 DEG C when vacuum bag is dry.
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| CN111875664A (en) * | 2020-07-31 | 2020-11-03 | 程红梅 | Small molecule peptide separation device |
| CN112249712A (en) * | 2020-11-16 | 2021-01-22 | 常州常衡德宇粉体集成系统有限公司 | Pneumatic conveying device and working method for negative pressure anti-blocking material of water-containing material |
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| CN112755580A (en) * | 2020-12-28 | 2021-05-07 | 南京安农汇科技有限公司 | Chinese herbal medicine separation filtration system |
| CN116440002A (en) * | 2023-06-16 | 2023-07-18 | 云南艾柯生物科技有限公司 | Rhinitis spray preparation method based on traditional Chinese medicine composition |
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