CN109568432A - A kind of preparation method of cordate houttuynia granule - Google Patents
A kind of preparation method of cordate houttuynia granule Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of cordate houttuynia granule, comprising: a, is crushed or shreds to obtain cordate houttuynia medicine materical crude slice for cordate houttuynia；B, cordate houttuynia medicine materical crude slice is successively inputted in continuous dynamic countercurrent extractor, in the end of extraction pipes at different levels continues that hot water is inversely added, continuous dynamic countercurrent extracts, and collects extracting solution, and the dregs of a decoction are discharged；C, extracting solution filters, and ultra high temperature short time sterilization, filtrate decompression is condensed into clear cream；D, auxiliary material dissolution is added in clear cream, is spray-dried to obtain dry extract；E, pharmaceutical adjunct is added in dry extract, dry granulation obtains cordate houttuynia granule.The present invention uses Continuous Countercurrent Extraction, ultra 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 cordate houttuynia granule sustainedly and stably to reach higher level, ensure that the active constituent rate of transform and cordate houttuynia standard decoction reach the product quality for unanimously improving cordate houttuynia granule.
Description
Technical field
The invention belongs to Chinese medicinal granule technical fields, and in particular to a kind of preparation method of cordate houttuynia granule.
Background technique
Cordate houttuynia is saururaceae plant houttuynia cordataHouttuynia cordata Thunb. on fresh herb or dry ground
Part.Fresh goods whole year can tap, and the luxuriant flower spike of dry product summer cauline leaf is tapped when more, remove impurity, dry.This product fresh goods and dry
Product can be used as medicine, and fresh goods dosage doubles, and decocting or smash juice clothes, have clearing heat and detoxicating, the effect of the carbuncle that disappears apocenosis, inducing diuresis for treating strangurtia, use
In lung carbuncle pyemesis, phlegm heat panting cough, hot dysentery, heat gonorrhea, carbuncle sore tumefacting virus.It has been reported that one of the principle active component of cordate houttuynia
Quercitin has the pharmacological actions such as antiviral, anti-inflammatory, diuresis, consistent with its effect, therefore, matches using quercitin as cordate houttuynia
The quality control index ingredient of square particle.Experimental study shows that quercitin content under long-time high-temperature condition is on a declining curve,
Temperature is higher, heated time is longer, and decline is more obvious.
Chinese medicinal granule is to be mentioned, be concentrated through water by single medicinal material medicine materical crude slice, dried, pelletized, in 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
Process is there are huge difference, such as standard decoction is the low temperature concentration of short time, dry process, and Chinese medicinal granule must be through
Cross the concentration of long period under the conditions of certain temperature, it is dry could form the particle used for medical institutions' adjustment, it is different
The quality that equipment, technique and process control both make generates difference, at the same different kinds because its ingredient physics, change
It learns distinct, different tendency of changes or rule is presented in process of production.How by equipment and technological means, make industry
The product of change obtains and the consistent clinical effectiveness of traditional Chinese medicine decoction, is that Chinese medicinal granule studies most important purpose.
Mainly using the static extracting method decocted twice, static state decocts to be existed the existing production technology of cordate houttuynia granule
Decoct 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.Experimental study hair
Existing, quercitin in cordate houttuynia proposes decoction, the sterilizing of clear cream ingredient by thermally labile, in water, is grown in wet granulation drying course
It easily degrades under conditions of time high temperature, thus causes the ingredient rate of transform low, content deviates standard decoction technical requirements range,
And differences between batches are big, not only cause the huge waste of resource, more seriously affect product quality, influence clinical application safety,
Effectively.
Continuous dynamic countercurrent extraction is novel extraction process in recent years, it collects extraction, weight diacolation, dynamic and adverse current skill
What art was integrated has many advantages, such as that simple process, saving solvent, low energy consumption, extraction time is short, extraction efficiency is high.Currently, not yet
See the report using continuous dynamic countercurrent extraction process preparation cordate houttuynia granule.
Summary of the invention
In order to overcome above-mentioned problem of the prior art, the purpose of the present invention is to provide a kind of systems of cordate houttuynia granule
Preparation Method, this method are raw using Continuous Countercurrent Extraction, high temperature, short time sterilizing, reduced pressure, instantaneous spray drying and dry granulation
Production. art enables active constituent content in cordate houttuynia granule sustainedly and stably to reach higher level, it is ensured that cordate houttuynia is matched
The rate of transform of active constituent reaches cordate houttuynia standard decoction technical requirements range in square particle.
The present invention is achieved through the following technical solutions；
A kind of preparation method of cordate houttuynia granule, which comprises the steps of:
A, cordate houttuynia is crushed or is shredded to obtain cordate houttuynia medicine materical crude slice；
B, the extraction pipe that cordate houttuynia medicine materical crude slice is continuously inputted to Continuous Countercurrent Extraction machine by the feed inlet of front end 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, is continuously added into 10 in the end of extraction pipes at different levels
~30 times amount hot water, preferably 15~20 times amount, continuous dynamic countercurrent extract 0.5~3.0h, preferably 1~2h, hot water with
Material collects extracting solution in liquid is brought out before reverse flow to extraction pipes at different levels, and the dregs of a decoction are discharged；
C, extracting solution filters, ultra high temperature short time sterilization, and it is 1.01 that filtrate, which is concentrated under reduced pressure into relative density under the conditions of 50~80 DEG C,
~1.20 clear cream；
D, auxiliary material dissolution is added in qinghuo reagent, is spray-dried to obtain dry extract；
E, pharmaceutical adjunct is added in dry extract, dry granulation obtains cordate houttuynia granule.
The present invention carries out the extraction process of cordate houttuynia, the Continuous Countercurrent Extraction machine using continuous dynamic countercurrent extractor
For the horizontal spiral Continuous Countercurrent Extraction machine of 10 section pipe structure of stage type, compared to pot group type countercurrent extraction machine group, horizontal spiral
Continuous Countercurrent Extraction machine has agglomerated the features such as dynamic countercurrent extraction, the extruding of continuous slag charge, continuous automatic slag-liquid separation and filtering, real
Whole serialization, automatic control, fast low temperature extraction are showed.It extracts principle are as follows: by cordate houttuynia medicine materical crude slice by feed inlet (front end)
It is continuously added to the extraction pipe of Continuous Countercurrent Extraction machine, is continuously pushed to material forward by a set of helical structure in extraction pipe
Extraction pipe slag-drip opening (end) is slagged tap, and water-soluble matchmaker is then continuously added into the end of extraction pipes at different levels, is in reverse flow with material
Liquid is brought out before to feed inlet end or extraction pipe at different levels, material comes into full contact with Extraction solvent, makes the concentration gradient of solute always
It is maintained at higher level, so as to greatly improve the extraction rate of transform of effective component, while by controlling extraction pipes at different levels
Extracting temperature, reduce heat-sensitive ingredients degradation at high temperature and destroy.
Cordate houttuynia raw material is crushed or the size of the partial size of chopping will affect whether effective component can be fully dissolved out, while shadow
Ring extraction process material push forward move it is whether smooth, be unfavorable for solute if partial size is excessive and quickly transmitted into solvent,
Smooth retard motion to material in Continuous Countercurrent Extraction simultaneously, be easy to miss from spiral plate hole if partial size is too small and
It can not be successfully and be transferred to slag-drip opening, it is preferred that in step a, the partial size after described broken or chopping is 0.1~1.0cm.
Dry cordate houttuynia medicine materical crude slice is easy to appear in blanking process to get stuck, and the medicine materical crude slice after water soaks is easier blanking, from
And guarantee material can be made to come into full contact with Extraction solvent with the blanking of continuous and quantitative, while being conducive in material under effective component
Transfer is quickly extracted after material, it is preferred that in step b, input again after cordate houttuynia medicine materical crude slice to be first added to the water wetting of 1~5 times of amount
In continuous dynamic countercurrent extractor.
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 | 25℃ | 40℃ | 70℃ | 85℃ | 95℃ | 100℃ |
| The quercitin rate of transform (%) | 42.9 | 48.2 | 51.6 | 52.5 | 49.8 | 47.1 |
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 the temperature of water
Height is spent, the thermally labile components such as quercitin and organic acid are easy to happen chemical degradation, it is preferred that in step b, the hot water
Temperature be 40~95 DEG C, preferably 70~85 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 | 7 times of amounts | 10 times of amounts | 15 times of amounts | 20 times of amounts | 30 times of amounts |
| The quercitin rate of transform (%) | 42.0 | 47.4 | 52.0 | 52.5 | 45.0 |
If solvent amount is very few it can be seen from the above results, active constituent cannot reach higher in each extraction pipeline section
Concentration difference, physical transfer is incomplete, and when solvent amount reaches 20 times of amounts, the quercitin rate of transform reaches peak-peak, if solvent
Amount is excessive, and not only energy consumption improves, but also extracting solution also accordingly extends in concentration time, and ingredient is made to degrade in enriching section, from
And the rate of transform of quercitin can be reduced.Therefore, the additional amount of the hot water is 10~30 times of amounts, preferably 15~20 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 | 0.25h | 0.5h | 1h | 2h | 3h | 5h |
| The quercitin rate of transform (%) | 43.7 | 49.6 | 52.1 | 49.3 | 45.0 | 42.2 |
If extraction time is short it can be seen from the above results, active constituent physical transfer is incomplete, if extraction time mistake
Long, quercitin chemical degradation rate is high, while reducing production efficiency.Preferably, in step b, cordate houttuynia medicine materical crude slice is in continuous dynamic inverse
Extraction time is 0.25~3.0h, preferably 0.5~2.0h in stream extraction.
For the rate of transform for further increasing effective component, it is preferred that in step b, by the cordate houttuynia dregs of a decoction through squeezing recoverer
It is then exhausted from after drug dispensing liquid, the part medical fluid of recycling merges with extracting solution, realizes hoop structure in process of production, more
It is the rate of recovery for taking full advantage of herb resource, while can be further improved Herba Houttuyniae extract, increases turning for effective component
Shifting rate.
Preferably, in step b, the input speed of the cordate houttuynia medicine materical crude slice is 100~200kg/h, reverse addition hot water
Flow velocity is 1000~6000kg/h.The present invention is fed by continuous and quantitative, comes into full contact with material with Extraction solvent, equipment mentions
It tries to please and is easily added with certain flow velocity, constantly updated, so that material be made to be constantly in biggish concentration throughout the extraction process
Gradient difference is conducive to being fully dissolved out for effective component, and then can greatly improve the rate of transform of effective component in cordate houttuynia.
Contain heat-sensitive ingredients in cordate houttuynia medicine materical crude slice, in order to avoid heat-sensitive ingredients decomposition, further increases the rate of transform, this
Invention will first refilter after the extracting solution cooling in step c, and the present invention is further optimized cooling temperature, concrete outcome
It is as follows:
| Cool down temperature | 25℃ | 40℃ | 55℃ | 70℃ | 80℃ |
| The quercitin rate of transform (%) | 52.6 | 51.8 | 52.2 | 48.0 | 44.5 |
The thermal degradation that can effectively avoid quercitin after extracting solution cooling it can be seen from the above results is conducive to the reservation of its content
And improve the rate of transform.When being cooled to 25~55 DEG C of temperature ranges, quercitin thermal degradation is less and tends towards stability, in combination with drop
The temperature that extracting solution is concentrated after temperature is in 50~80 DEG C of temperature ranges, to reduce heating energy consumption when extracting solution concentration, preferably
, in step c, 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 quercitin from chemical degradation occurring in sterilization process, it is preferred that in step c,
The ultra high temperature short time sterilization is that filtrate sterilizes 2~60 seconds at 100~200 DEG C in supper high temperature instant sterilizer.
Quercitin in cordate houttuynia by thermally labile, easily degrade in wet granulation drying course, is preferably applicable in by ingredient
Dry granulation, to improve material viscosity, mobility meets granule melting requirement to adapt to dry granulation, in clear cream
Relevant auxiliary materials are added when spray drying ingredient, and takes a step forward in dry granulation and proper auxiliary materials are added adjust its mobility, compressibility.
Preferably, in step d, the auxiliary material is one or more of maltodextrin, dextrin, starch, lactose or beta-cyclodextrin；It is described
The technological parameter of spray drying are as follows: 170 DEG C~180 DEG C of inlet air temperature, 80 DEG C~90 DEG C of leaving air temp of control.
Preferably, in step e, 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 in lower temperature
The characteristics of lower extraction, improves the physics of quercitin during the extraction process and dissolves out the rate of transform, while can carry out temperature with lower temperature
Leaching is continuous to extract, and 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 quercitin in spray drying blending process, and preferably various granulations are auxiliary
Material carries out dry granulation, prevents active constituent from crossing in kind in preparation and changes.
(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 keep cordate houttuynia Chinese medicinal granule Determination of Quercitrin continual and steady
Ground reaches higher level, it is ensured that and the active constituent rate of transform and cordate houttuynia standard decoction reach unanimously in cordate houttuynia granule,
Improve the product quality of cordate houttuynia 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.
Embodiment 1:
A kind of preparation method of cordate houttuynia granule, includes the following steps:
A, Herba Houttuyniae is selected, shaking weeds out except impurity, is broken into 0.5cm particle, obtain cordate houttuynia medicine materical crude slice；
B, 2 times of amount water of broken cordate houttuynia medicine materical crude slice are soaked, spiral continuous flow upstream is continuously inputted by the feed inlet of front end
The extraction pipe of extractor (10 section pipe structure of stage type) is continuously pushed forward material by a set of helical structure in extraction pipe
It slags tap to extraction pipe slag-drip opening, is continuously added into 95 DEG C of hot water Continuous Countercurrent Extraction 1h of 20 times of amounts in the end of extraction pipes at different levels,
Hot water and material collect extracting solution in liquid is brought out before reverse flow to extraction pipes at different levels, and the cordate houttuynia dregs of a decoction are recycled through squeezing
It is then exhausted from after the medical fluid of part, the part medical fluid of recycling merges with extracting solution；The input speed of the cordate houttuynia medicine materical crude slice is 100kg/
H, the reverse flow velocity that hot water is added are 2000L/h；
C, the extracting solution after merging filters after being cooled to 80 DEG C, and filtered fluid goes out at 150 DEG C in supper high temperature instant sterilizer (UHT)
Bacterium 10 seconds, after at 60 DEG C be concentrated under reduced pressure at relative density be 1.06 clear cream；
D, 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: 170 DEG C ~ 180 DEG C of inlet air temperature, 80 DEG C ~ 90 DEG C of leaving air temp of control；
E, maltodextrin and silica is added in dry extract, is uniformly mixed, dry granulation obtains cordate houttuynia granule.
Embodiment 2:
Step 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 1.06 clear cream；
Remaining step is the same as embodiment 1.
Embodiment 3:
A kind of preparation method of cordate houttuynia granule, includes the following steps:
A, Herba Houttuyniae is selected, shaking weeds out except impurity, is broken into 0.5cm particle, obtain cordate houttuynia medicine materical crude slice；
B, 2 times of amount water of broken cordate houttuynia medicine materical crude slice are soaked, spiral continuous flow upstream is continuously inputted by the feed inlet of front end
The extraction pipe of extractor (10 section pipe structure of stage type) is continuously pushed forward material by a set of helical structure in extraction pipe
It slags tap to extraction pipe slag-drip opening, is continuously added into 80 DEG C of hot water Continuous Countercurrent Extraction 1h of 18 times of amounts in the end of extraction pipes at different levels,
Hot water and material collect extracting solution in liquid is brought out before reverse flow to extraction pipes at different levels, and the cordate houttuynia dregs of a decoction are recycled through squeezing
It is then exhausted from after the medical fluid of part, the part medical fluid of recycling merges with extracting solution；The input speed of the cordate houttuynia medicine materical crude slice is 100kg/
H, the reverse flow velocity that hot water is added are 1800L/h；
C, the extracting solution after merging filters after being cooled to 50 DEG C, and filtered fluid goes out at 150 DEG C in supper high temperature instant sterilizer (UHT)
Bacterium 10 seconds, after at 60 DEG C be concentrated under reduced pressure at relative density be 1.06 clear cream；
D, 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: 170 DEG C ~ 180 DEG C of inlet air temperature, 80 DEG C ~ 90 DEG C of leaving air temp of control；
E, maltodextrin and silica is added in dry extract, is uniformly mixed, dry granulation obtains cordate houttuynia granule.
Embodiment 4:
Step b, broken cordate houttuynia medicine materical crude slice is continuously inputted into spiral Continuous Countercurrent Extraction machine (twin-stage by the feed inlet of front end
10 section pipe structure of formula) extraction pipe, extraction pipe in by a set of helical structure by material continuously forward push to extraction pipe row
Cinder notch is slagged tap, and is continuously added into 80 DEG C of hot water Continuous Countercurrent Extraction 1h of 18 times of amounts, hot water and material in the end of extraction pipes at different levels
In liquid is brought out before reverse flow to extraction pipes at different levels, extracting solution is collected, the cordate houttuynia dregs of a decoction are discharged；The cordate houttuynia medicine materical crude slice
Input speed is 100kg/h, and the reverse flow velocity that hot water is added is 1800L/h；
Remaining step is the same as embodiment 3.
Embodiment 5:
A kind of preparation method of cordate houttuynia granule, includes the following steps:
A, Herba Houttuyniae is selected, shaking weeds out except impurity, is broken into 0.4cm particle, obtain cordate houttuynia medicine materical crude slice；
B, 2.5 times of amount water of broken cordate houttuynia medicine materical crude slice are soaked, is continuously inputted by the feed inlet of front end spiral continuous inverse
The extraction pipe for flowing extractor (10 section pipe structure of stage type), in extraction pipe by a set of helical structure by material continuously to being pushed forward
It send to extraction pipe slag-drip opening and slags tap, be continuously added into 70 DEG C of hot water Continuous Countercurrent Extractions of 16 times of amounts in the end of extraction pipes at different levels
1.5h, hot water and material collect extracting solution, by the cordate houttuynia dregs of a decoction through squeezing in liquid is brought out before reverse flow to extraction pipes at different levels
It is then exhausted from after recovery section medical fluid, the part medical fluid of recycling merges with extracting solution；The input speed of the broken cordate houttuynia
For 50kg/h, the reverse flow velocity that hot water is added is 800L/h；
C, the extracting solution after merging filters after being cooled to 45 DEG C, and filtered fluid goes out at 105 DEG C in supper high temperature instant sterilizer (UHT)
Bacterium 30 seconds, after at 75 DEG C be concentrated under reduced pressure at relative density be 1.04 clear cream；
D, qinghuo reagent is added lactose and dissolves and stir evenly, and is spray-dried, obtains dry extract, the technique of the spray drying
Parameter are as follows: 170 DEG C ~ 180 DEG C of inlet air temperature, 80 DEG C ~ 90 DEG C of leaving air temp of control；
E, lactose, silica and magnesium stearate is added in dry extract, is uniformly mixed, dry granulation obtains cordate houttuynia granule.
Comparative example 1: Chinese medicine extracting tank is used
A kind of preparation method of cordate houttuynia granule, includes the following steps:
A, Herba Houttuyniae is selected, shaking weeds out except impurity, is broken into 0.5cm particle, obtain cordate houttuynia medicine materical crude slice；
B, cordate houttuynia medicine materical crude slice is added in Chinese medicine extracting tank, with water boiling and extraction 2 times, for the first time plus the water of 11 times of amounts is heated and decocted
0.5h, the water heating of second plus 9 times amount decoct 0.5h, extracting solution filtration；
C, the clear cream that relative density is 1.06 when filtrate decompression is condensed into 60 DEG C；
D, 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: 170 DEG C ~ 180 DEG C of inlet air temperature, 80 DEG C ~ 90 DEG C of leaving air temp of control；
E, dry extract adds maltodextrin and silica, is uniformly mixed, dry granulation obtains cordate houttuynia granule.
Comparative example 2: pot group type countercurrent extraction machine is used
A kind of preparation method of cordate houttuynia granule, includes the following steps:
A, Herba Houttuyniae is selected, shaking weeds out except impurity, is broken into 0.5cm particle, obtain cordate houttuynia medicine materical crude slice；
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,
Fresh solvent is added with material-water ratio 1:20 ratio in tail tank, is extracted with 95 DEG C of each tank Extracting temperature, extraction time 1h: 5
Material in a tank 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 dregs of a decoction extracted through 3 times, warp
Fresh solvent is added in (dregs of a decoction after extracting equipped with the 4th) tank of most end by the dregs of a decoction of 4 extractions, other each tanks according to
Secondary to extract equipped with the extracting solution moved past from next stage tank transfer, final extracting solution is discharged from the tank of foremost, finally
Extractor discharge the dregs of a decoction and be packed into new medicine materical crude slice, become most preceding extractor, so circulation is reverse extracts, and collects extracting solution filtration
Merge；
C, the extracting solution after merging filters after being cooled to 50 DEG C, and filtered fluid goes out at 150 DEG C in supper high temperature instant sterilizer (UHT)
Bacterium 10 seconds, after at 60 DEG C be concentrated under reduced pressure at relative density be 1.06 clear cream；
D, 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: 170 DEG C ~ 180 DEG C of inlet air temperature, 80 DEG C ~ 90 DEG C of leaving air temp of control；
E, maltodextrin and silica is added in dry extract, is uniformly mixed, dry granulation obtains cordate houttuynia granule.
The cordate houttuynia granule that embodiment and comparative example is prepared measures Determination of Quercitrin, calculates paste-forming rate, turns
Shifting rate situation, the results are shown in Table 1:
1 cordate houttuynia granule embodiment of table is compared with comparative example result
By embodiment 1 it is found that the present invention is mentioned using Continuous Countercurrent Extraction technology with traditional extraction tank compared with 1 result of comparative example
Take technology to compare, not only solvent consumption amount is few, but also can continuous slag charge squeeze, continuous automatic slag-liquid separation, realize it is whole even
Continuousization, automatic control, fast low temperature extract, and remain by thermally labile component Determination of Quercitrin, hence it is evident that improve the rate of transform, table
The bright present invention is substantially better than common extractor extractive technique currently on the market using Continuous Countercurrent Extraction technology.
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
Extractive technique either paste-forming rate or Determination of Quercitrin and the rate of transform increase, i.e., the present invention is mentioned using continuous flow upstream
Take technology better than pot group type countercurrent extraction machine.
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 of heat-sensitive ingredients, 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
It significantly improves by thermally labile component Determination of Quercitrin and the rate of transform, and then improves the quality of product.Meanwhile continuous dynamic countercurrent
Technology can be further reduced the consumption of solvent in the case where guaranteeing paste-forming rate, component content and the rate of transform, be economical and energy saving
A kind of novel extracting mode.
By embodiment 1 ~ 5 it is found that the present invention carries out extracting solution using ultra high temperature short time sterilization technology compared with comparative example 1
Sterilizing preferably can control microorganism from source, guarantee that the microorganism of finished product is qualified.
Claims (10)
1. a kind of preparation method of cordate houttuynia granule, which comprises the steps of:
A, cordate houttuynia is crushed or is shredded to obtain cordate houttuynia medicine materical crude slice；
B, the extraction pipe that cordate houttuynia medicine materical crude slice is continuously inputted to Continuous Countercurrent Extraction machine by the feed inlet of front end 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, is continuously added into 10 in the end of extraction pipes at different levels
The hot water of~30 times of amounts, preferably 15~20 times amounts, continuous dynamic countercurrent extract 0.25~3.0h, preferably 0.5~2h, hot water
With material in liquid is brought out before reverse flow to extraction pipes at different levels, extracting solution is collected, the dregs of a decoction are discharged；
C, extracting solution filters, ultra high temperature short time sterilization, and it is 1.01 that filtrate, which is concentrated under reduced pressure into relative density under the conditions of 50~80 DEG C,
~1.20 clear cream；
D, auxiliary material dissolution is added in qinghuo reagent, is spray-dried to obtain dry extract；
E, pharmaceutical adjunct is added in dry extract, dry granulation obtains cordate houttuynia granule.
2. the preparation method of cordate houttuynia granule according to claim 1, which is characterized in that described broken in step a
Or the partial size after chopping is 0.1~1.0cm.
3. the preparation method of cordate houttuynia granule according to claim 1, which is characterized in that in step b, by cordate houttuynia
Medicine materical crude slice inputs in continuous dynamic countercurrent extractor again after the water wetting of 1~5 times of amount is first added.
4. the preparation method of cordate houttuynia granule according to claim 1, which is characterized in that described continuous in step b
Countercurrent extraction machine is spiral Continuous Countercurrent Extraction machine, is 10 section pipe structure of stage type.
5. the preparation method of cordate houttuynia granule according to claim 1, which is characterized in that in step b, the hot water
Temperature be 40~95 DEG C, preferably 70~85 DEG C.
6. the preparation method of cordate houttuynia granule according to claim 1, which is characterized in that in step b, the dregs of a decoction are passed through
It is then exhausted from after squeezing recovery section medical fluid, the part medical fluid of recycling merges with extracting solution.
7. the preparation method of cordate houttuynia granule according to claim 1, which is characterized in that in step b, the fish raw meat
The input speed of careless medicine materical crude slice is 100~200kg/h, and the reverse flow velocity that hot water is added is 1000~6000kg/h.
8. the preparation method of cordate houttuynia granule according to claim 1, which is characterized in that in step c, will first extract
Liquid refilters after being cooled to 40~55 DEG C；The ultra high temperature short time sterilization is in supper high temperature instant sterilizer at 100~200 DEG C
Sterilizing 2~60 seconds.
9. the preparation method of cordate houttuynia granule according to claim 1, which is characterized in that in step d, the auxiliary material
For one or more of maltodextrin, dextrin, starch, lactose or beta-cyclodextrin；The technological parameter of the spray drying are as follows: control
170 DEG C~180 DEG C of inlet air temperature processed, 80 DEG C~90 DEG C of leaving air temp.
10. the preparation method of cordate houttuynia granule according to claim 1, which is characterized in that in step e, the system
Agent auxiliary material is one or more of maltodextrin, dextrin, starch, lactose, beta-cyclodextrin, silica or magnesium stearate.
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| CN105878525A (en) * | 2014-12-15 | 2016-08-24 | 沈阳伟嘉牧业技术有限公司 | Method for preparing houttuynia cordata lyophilized superfine powder granules |
| CN107375510A (en) * | 2017-08-22 | 2017-11-24 | 张涛 | A kind of preparation method of cordate houttuynia particle |
| CN107441223A (en) * | 2017-08-25 | 2017-12-08 | 徐自升 | A kind of fresh preparation technology for squeezing spray-dried granules medicine materical crude slice of cordate houttuynia |
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| CN107375510A (en) * | 2017-08-22 | 2017-11-24 | 张涛 | A kind of preparation method of cordate houttuynia particle |
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