CN109568366A - A kind of preparation method of Inula britannica chinensis or sweet Inula britannica chinensis granule - Google Patents
A kind of preparation method of Inula britannica chinensis or sweet Inula britannica chinensis granule Download PDFInfo
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- 241000253121 Inula britannica Species 0.000 title claims abstract description 198
- 235000009508 confectionery Nutrition 0.000 title claims abstract description 74
- 239000008187 granular material Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 238000000605 extraction Methods 0.000 claims abstract description 135
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 72
- 239000003814 drug Substances 0.000 claims abstract description 63
- 239000000463 material Substances 0.000 claims abstract description 55
- 239000000284 extract Substances 0.000 claims abstract description 45
- 238000007908 dry granulation Methods 0.000 claims abstract description 24
- 238000001694 spray drying Methods 0.000 claims abstract description 21
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- 230000001954 sterilising effect Effects 0.000 claims abstract description 15
- 238000004659 sterilization and disinfection Methods 0.000 claims abstract description 11
- 239000000706 filtrate Substances 0.000 claims abstract description 7
- 238000002203 pretreatment Methods 0.000 claims abstract description 5
- 238000004090 dissolution Methods 0.000 claims abstract description 3
- 239000012530 fluid Substances 0.000 claims description 32
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 30
- 229920002774 Maltodextrin Polymers 0.000 claims description 28
- 239000005913 Maltodextrin Substances 0.000 claims description 28
- 229940035034 maltodextrin Drugs 0.000 claims description 28
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- 239000012535 impurity Substances 0.000 claims description 18
- 239000003153 chemical reaction reagent Substances 0.000 claims description 16
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- 238000009835 boiling Methods 0.000 claims description 11
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- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 8
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 claims description 7
- 239000008101 lactose Substances 0.000 claims description 7
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- PZIRUHCJZBGLDY-UHFFFAOYSA-N Caffeoylquinic acid Natural products CC(CCC(=O)C(C)C1C(=O)CC2C3CC(O)C4CC(O)CCC4(C)C3CCC12C)C(=O)O PZIRUHCJZBGLDY-UHFFFAOYSA-N 0.000 description 2
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- 235000001368 chlorogenic acid Nutrition 0.000 description 1
- 229940074393 chlorogenic acid Drugs 0.000 description 1
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- QAIPRVGONGVQAS-UHFFFAOYSA-N cis-caffeic acid Natural products OC(=O)C=CC1=CC=C(O)C(O)=C1 QAIPRVGONGVQAS-UHFFFAOYSA-N 0.000 description 1
- 235000001671 coumarin Nutrition 0.000 description 1
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- 238000000354 decomposition reaction Methods 0.000 description 1
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- 229930003935 flavonoid Natural products 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
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- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 description 1
- 150000002596 lactones Chemical class 0.000 description 1
- LRDGATPGVJTWLJ-UHFFFAOYSA-N luteolin Natural products OC1=CC(O)=CC(C=2OC3=CC(O)=CC(O)=C3C(=O)C=2)=C1 LRDGATPGVJTWLJ-UHFFFAOYSA-N 0.000 description 1
- IQPNAANSBPBGFQ-UHFFFAOYSA-N luteolin Chemical compound C=1C(O)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(O)C(O)=C1 IQPNAANSBPBGFQ-UHFFFAOYSA-N 0.000 description 1
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- 239000002245 particle Substances 0.000 description 1
- 150000007965 phenolic acids Chemical class 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- RXHIKAIVEMAPRU-JRIGQVHBSA-N sequiterpene Natural products C1=C(C)[C@@H](OC(C)=O)[C@H](O)[C@@]2(O)[C@H](C)CC[C@@H](C(C)=C)[C@H]21 RXHIKAIVEMAPRU-JRIGQVHBSA-N 0.000 description 1
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- 150000003432 sterols Chemical class 0.000 description 1
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Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/28—Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1605—Excipients; Inactive ingredients
- A61K9/1611—Inorganic compounds
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1605—Excipients; Inactive ingredients
- A61K9/1629—Organic macromolecular compounds
- A61K9/1652—Polysaccharides, e.g. alginate, cellulose derivatives; Cyclodextrin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1682—Processes
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/13—Preparation or pretreatment of starting material involving cleaning, e.g. washing or peeling
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Public Health (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Pharmacology & Pharmacy (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Veterinary Medicine (AREA)
- Epidemiology (AREA)
- Inorganic Chemistry (AREA)
- Alternative & Traditional Medicine (AREA)
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Abstract
The invention discloses a kind of Inula britannica chinensis or the preparation methods of sweet Inula britannica chinensis granule, comprising: a, by the pre-treatment of Inula britannica chinensis medicinal material or processing；B, the extraction pipe that Inula britannica chinensis or sweet Inula britannica chinensis medicine materical crude slice are continuously inputted to Continuous Countercurrent Extraction machine in the end of extraction pipes at different levels continues that hot water is inversely added, and 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 to obtain the final product.The present invention uses Continuous Countercurrent Extraction, high-temperature short-time sterilization, reduced pressure, spray drying, dry granulation production technology, and various process parameters are studied, to enable active constituent content in granule sustainedly and stably to reach higher level, ensure that the active constituent rate of transform and standard decoction reach the product quality for unanimously improving Inula britannica chinensis or sweet Inula britannica chinensis granule.
Description
Technical field
The invention belongs to Chinese medicinal granule technical fields, and in particular to a kind of Inula britannica chinensis or sweet Inula britannica chinensis granule
Preparation method.
Background technique
Inula britannica chinensis is compositae plant Inula britannica chinensisInula japonicaOr Inula britannica Thunb.Inula britannicaL. dry capitulum has effects that sending down abnormally ascending, dissolving phlegm, Hang Shui, preventing or arresting vomiting, is used for cough due to wind-cold evil, and phlegm retention stores
Knot, chest diaphragm ruffian is bored, dyspnea and cough with excessive sputum, vomits gas, epigastric fullness and rigidity.The main component of Inula britannica chinensis is flavonoids, phenolic acid class, sequiterpene
Lactone, sterols and Coumarins chemical component, including chlorogenic acid, caffeic acid, 3,5-OTwo-caffeoyl quinic acid, 1,5-OThe ingredients such as two-caffeoyl quinic acid, luteolin.3,5- in Inula britannica chinensis standard decoctionOTwo-caffeoyl quinic acid content
It is higher, it can be used as the quality control composition of Inula britannica chinensis medicinal material and standard decoction, 3,5-OTwo-caffeoyl quinic acid is typical
Higher with heating temperature, the time is longer by thermally labile component, content reduction 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.
Inula britannica chinensis or the existing production technology of sweet Inula britannica chinensis Chinese medicinal granule are mainly using the static extraction side decocted twice
Method, flos materia medica extraction process Chinese medicine is light, easily floats liquid level, and decoction is insufficient, easily causes the waste of resource, medicine after decoction
Slag water swelling, difficulty that drawing liquid amount is few, drawing liquid is slagged tap, causes production efficiency low, and static decoct has decoction temperature height, decocts
The defects of time is long, production efficiency is low, energy consumption is at high cost, active ingredient loss is more.Main active 3,5-O- two coffees
Acyl group quininic acid is typical thermally labile component, i.e., water mention decoction, the sterilizing of clear cream ingredient, in wet granulation drying course by
The influence of long-time high temperature is easily degraded, thus causes the ingredient rate of transform low, and 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 water extraction process preparation Inula britannica chinensis or sweet Inula britannica chinensis granule.
Summary of the invention
In order to overcome above-mentioned the problems of the prior art, the purpose of the present invention is to provide a kind of Inula britannica chinensis or sweet Inula britannica chinensis
The preparation method of granule, this method is using Continuous Countercurrent Extraction, high temperature, short time sterilizing, reduced pressure, instantaneous spray drying
With dry granulation production technology, enable in Inula britannica chinensis or sweet Inula britannica chinensis granule active constituent content sustainedly and stably reach compared with
High level, it is ensured that the rate of transform of active constituent reaches Inula britannica chinensis or sweet Inula britannica chinensis mark in Inula britannica chinensis or sweet Inula britannica chinensis granule
Quasi- decoction technical requirements range.
The present invention is achieved through the following technical solutions；
The preparation method of a kind of Inula britannica chinensis or sweet Inula britannica chinensis granule, includes the following steps:
A, by the pre-treatment of Inula britannica chinensis medicinal material or processing, Inula britannica chinensis or sweet Inula britannica chinensis medicine materical crude slice are obtained；
B, the extraction pipe that Inula britannica chinensis or sweet Inula britannica chinensis medicine materical crude slice are continuously inputted to Continuous Countercurrent Extraction machine by feed inlet, in extraction pipe
Material is continuously pushed to forward extraction pipe slag-drip opening by a set of helical structure to slag tap, is continued in the end of extraction pipes at different levels inverse
To be added 10~30 times amount hot water, preferably 15~20 times amount, continuous dynamic countercurrent extract 0.25~3.0h, preferably 0.5
~2h collects extracting solution, and the dregs of a decoction are discharged；
C, extracting solution filters, ultra high temperature short time sterilization, and filtrate is concentrated under reduced pressure into relative density as 1.01 at 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 Inula britannica chinensis or sweet Inula britannica chinensis granule.
The present invention carries out the extraction process of Inula britannica chinensis or sweet Inula britannica chinensis using continuous dynamic countercurrent extractor, and described is continuous
Countercurrent extraction machine is 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 dynamic countercurrent extraction, continuous slag charge squeezes, continuous slag-liquid separation and mistake automatically
The features such as filter, realizes whole serialization, automatic control, fast low temperature extraction.It extracts principle are as follows: Inula britannica chinensis or honey is sheathed
Flower medicine materical crude slice is continuously added to the extraction pipe of Continuous Countercurrent Extraction machine by feed inlet (front end), passes through a set of helical structure in extraction pipe
Material is continuously pushed to forward to extraction pipe slag-drip opening (end) to slag tap, and water-soluble matchmaker then persistently adds in the end of extraction pipes at different levels
Enter, with material in liquid is brought out before reverse flow to feed inlet end or extraction pipe at different levels, material comes into full contact with Extraction solvent, makes
The concentration gradient of solute remains at higher level, so as to greatly improve the extraction rate of transform of effective component, simultaneously
By controlling the Extracting temperature of extraction pipes at different levels, reduces the degradation of heat-sensitive ingredients at high temperature and destroy.
In step a, the pre-treatment is that Inula britannica chinensis medicinal material is removed stalk, leaf and impurity；The processing is by sheathed anther
Material removes stalk, leaf and impurity, is added and uses the diluted refined honey of boiling water, bored, tack-free with being fried with slow fire, and obtains sweet Inula britannica chinensis medicine materical crude slice.
Dry Inula britannica chinensis or sweet Inula britannica chinensis medicine materical crude slice are easy to appear in blanking process and get stuck, and the wet granular after water soaks is more
It is easy blanking, to guarantee material can be made to come into full contact with Extraction solvent, while being conducive in material with the blanking of continuous and quantitative
Transfer is quickly extracted after effective component blanking, it is preferred that in step b, Inula britannica chinensis or sweet Inula britannica chinensis medicine materical crude slice are first added 1~5
It is inputted in continuous dynamic countercurrent extractor again after the water wetting of amount again.
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℃ |
| 3,5- in Inula britannica chinensisOThe two-caffeoyl quinic acid rate of transform (%) | 28.5 | 31.1 | 34.8 | 34.5 | 32.3 | 29.5 |
| 3,5- in sweet Inula britannica chinensisOThe two-caffeoyl quinic acid rate of transform (%) | 40.0 | 43.7 | 49.1 | 48.6 | 45.3 | 40.2 |
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
Spend height, 3,5-OThe heat-sensitive ingredients such as two-caffeoyl quinic acid are easy to happen chemical degradation in aqueous solution, it is preferred that step
In rapid b, the temperature of the hot water is 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 |
| 3,5- in Inula britannica chinensisOThe two-caffeoyl quinic acid rate of transform (%) | 27.6 | 32.0 | 34.1 | 35.0 | 29.2 |
| 3,5- in sweet Inula britannica chinensisOThe two-caffeoyl quinic acid rate of transform (%) | 39.4 | 46.7 | 48.1 | 49.3 | 38.6 |
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, when solvent amount reaches 20 times of amounts, 3,5-OThe two-caffeoyl quinic acid rate of transform reaches most
Peak value, if solvent amount is excessive, not only energy consumption is improved, but also extracting solution also accordingly extends in concentration time, makes ingredient dense
Contracting section is degraded, so that 3,5- can be reducedOThe rate of transform of two-caffeoyl quinic acid.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 to be optimized, concrete outcome is as follows:
| Extraction time | 0.25h | 0.5h | 1h | 2h | 3h | 5h |
| 3,5- in Inula britannica chinensisOThe two-caffeoyl quinic acid rate of transform (%) | 30.6 | 33.4 | 34.9 | 32.8 | 28.2 | 26.5 |
| 3,5- in sweet Inula britannica chinensisOThe two-caffeoyl quinic acid rate of transform (%) | 43.8 | 48.9 | 49.4 | 45.5 | 40.0 | 35.1 |
If extraction time is short it can be seen from the above results, active constituent physical transfer is incomplete, if extraction time mistake
It is long, 3,5-OTwo-caffeoyl quinic acid chemical degradation rate is high, while reducing production efficiency.Preferably, in step b, Inula britannica chinensis
Or sweet Inula britannica chinensis medicine materical crude slice extraction time in continuous dynamic countercurrent extraction is 0.25~3.0h, preferably 0.5 ~ 2h.
For the rate of transform for further increasing effective component, it is preferred that in step b, by Inula britannica chinensis or sweet Inula britannica chinensis dregs of a decoction warp
It is then exhausted from after squeezing recovery section medical fluid, the part medical fluid of recycling merges with extracting solution, so as to further increase Inula britannica chinensis
Or the rate of recovery of sweet Inula britannica chinensis extracting solution, increase the rate of transform of effective component.
Preferably, in step b, the coarse grained input speed is 100-200kg/h, and the reverse flow velocity that hot water is added is
1000-5000kg/h.The present invention is fed by continuous and quantitative, comes into full contact with material with Extraction solvent, and the extraction of equipment is easy
It is added, is constantly updated with certain flow velocity, so that it is poor so that material is constantly in biggish concentration gradient throughout the extraction process,
Be conducive to being fully dissolved out for effective component, and then the rate of transform of effective component in Inula britannica chinensis or sweet Inula britannica chinensis can be greatly improved.
Contain heat-sensitive ingredients in Inula britannica chinensis or sweet Inula britannica chinensis medicine materical crude slice, in order to avoid heat-sensitive ingredients decomposition, further mentions
The high rate of transform, the present invention will first refilter after the extracting solution cooling in step c, and the present invention has further carried out cooling temperature excellent
Change, concrete outcome is as follows:
| Cool down temperature | 25℃ | 40℃ | 55℃ | 70℃ | 80℃ |
| 3,5- in Inula britannica chinensisOThe two-caffeoyl quinic acid rate of transform (%) | 35.4 | 34.7 | 35.0 | 32.1 | 30.5 |
| 3,5- in sweet Inula britannica chinensisOThe two-caffeoyl quinic acid rate of transform (%) | 48.8 | 49.2 | 48.7 | 47.4 | 45.0 |
By can effectively avoid 3,5- after extracting solution cooling it can be seen from the above resultsOThe thermal degradation of two-caffeoyl quinic acid,
Be conducive to its content to retain and improve the rate of transform.When being cooled to 25~55 DEG C of temperature ranges, 3,5-O- two coffee acyl quinines
Acid heat degradation is less and tend towards stability, the temperature being concentrated in combination with extracting solution after cooling in 50~80 DEG C of temperature ranges,
To reduce heating energy consumption when extracting solution concentration, it is preferred that 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 3,5-OChemistry drop occurs in sterilization process for two-caffeoyl quinic acid
Solution, it is preferred that in step c, the ultra high temperature short time sterilization be by filtrate in supper high temperature instant sterilizer at 100~200 DEG C
Sterilizing 2~60 seconds.
Ingredient is degraded in heat-sensitive ingredients material wet granulation drying course, is preferably suitable for dry granulation, to improve
Material viscosity, mobility meet granule melting requirement to adapt to dry granulation, are added in clear cream spray drying ingredient
Relevant auxiliary materials, and take 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；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.
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 3,5-OTwo-caffeoyl quinic acid physics during the extraction process dissolves out the rate of transform, while can be with
The continuous extraction of temperature leaching is carried out with lower temperature, 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 3,5-ODegradation of the two-caffeoyl quinic acid in spray drying blending process,
And preferably various granulation auxiliary materials carry out dry granulation, prevent active constituent from crossing in kind in preparation and change.
(3) present invention combines Continuous Countercurrent Extraction, ultra high temperature short time sterilization, reduced pressure, spray drying, dry granulation raw
Production. art, and various process parameters are studied, to make Inula britannica chinensis and its process medicine materical crude slice Chinese medicinal granule 3,5-O- two
Caffeoyl quinic acid content can sustainedly and stably reach higher level, it is ensured that living in Inula britannica chinensis and sweet Inula britannica chinensis granule
Property the ingredient rate of transform reach unanimously with Inula britannica chinensis or sweet Inula britannica chinensis standard decoction, improve Inula britannica chinensis or honey Inula britannica chinensis granule
Product quality.
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 Inula britannica chinensis granule, includes the following steps:
A, Inula britannica chinensis medicinal material is removed into stalk, leaf and impurity and obtains Inula britannica chinensis medicine materical crude slice；
B, 2 times of amount water of Inula britannica chinensis medicine materical crude slice are soaked, spiral Continuous Countercurrent Extraction machine (stage type 10 is continuously inputted by feed inlet
Save pipe structure) extraction pipe, extraction pipe in by a set of helical structure by material continuously forward push to extraction pipe slag-drip opening
It slags tap, continues 95 DEG C of hot water Continuous Countercurrent Extraction 1h that 20 times of amounts are inversely added in the end of extraction pipes at different levels, collect extracting solution,
The Inula britannica chinensis dregs of a decoction are then exhausted from after squeezing recovery section medical fluid, the part medical fluid of recycling merges with extracting solution；The Inula britannica chinensis
The input speed of medicine materical crude slice is 100kg/h, and the reverse flow velocity that hot water is added is 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 Inula britannica chinensis granule.
Embodiment 2:
A kind of preparation method of Inula britannica chinensis granule, includes the following steps:
A, Inula britannica chinensis medicinal material is removed into stalk, leaf and impurity and obtains Inula britannica chinensis medicine materical crude slice；
B, 2 times of amount water of Inula britannica chinensis medicine materical crude slice are soaked, spiral Continuous Countercurrent Extraction machine (stage type 10 is continuously inputted by feed inlet
Save pipe structure) extraction pipe, extraction pipe in by a set of helical structure by material continuously forward push to extraction pipe slag-drip opening
It slags tap, continues 95 DEG C of hot water Continuous Countercurrent Extraction 1h that 20 times of amounts are inversely added in the end of extraction pipes at different levels, collect extracting solution,
The Inula britannica chinensis dregs of a decoction are then exhausted from after squeezing recovery section medical fluid, the part medical fluid of recycling merges with extracting solution；The Inula britannica chinensis
The input speed of medicine materical crude slice is 100kg/h, and the reverse flow velocity that hot water is added is 2000L/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 Inula britannica chinensis granule.
Embodiment 3:
A kind of preparation method of Inula britannica chinensis granule, includes the following steps:
A, Inula britannica chinensis medicinal material is removed into stalk, leaf and impurity and obtains Inula britannica chinensis medicine materical crude slice；
B, 2 times of amount water of Inula britannica chinensis medicine materical crude slice are soaked, spiral Continuous Countercurrent Extraction machine (stage type 10 is continuously inputted by feed inlet
Save pipe structure) extraction pipe, extraction pipe in by a set of helical structure by material continuously forward push to extraction pipe slag-drip opening
It slags tap, continues 80 DEG C of hot water Continuous Countercurrent Extraction 1h that 18 times of amounts are inversely added in the end of extraction pipes at different levels, collect extracting solution,
The Inula britannica chinensis dregs of a decoction are then exhausted from after squeezing recovery section medical fluid, the part medical fluid of recycling merges with extracting solution；The Inula britannica chinensis
The input speed of medicine materical crude slice is 100kg/h, and the reverse flow velocity that hot water is added is 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 Inula britannica chinensis granule.
Embodiment 4:
A kind of preparation method of Inula britannica chinensis granule, includes the following steps:
A, Inula britannica chinensis medicinal material is removed into stalk, leaf and impurity and obtains Inula britannica chinensis medicine materical crude slice；
B, Inula britannica chinensis medicine materical crude slice is continuously inputted to the leaching of spiral Continuous Countercurrent Extraction machine (10 section pipe structure of stage type) by feed inlet
Pipe is mentioned, material is continuously pushed to forward by extraction pipe slag-drip opening by a set of helical structure in extraction pipe and is slagged tap, in leachings at different levels
The end for mentioning pipe continues 80 DEG C of hot water Continuous Countercurrent Extraction 1h that 18 times of amounts are inversely added, and extracting solution is collected, by the Inula britannica chinensis dregs of a decoction
Discharge；The input speed of the Inula britannica chinensis medicine materical crude slice is 100kg/h, and the reverse flow velocity that hot water is added is 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 Inula britannica chinensis granule.
Embodiment 5:
A kind of preparation method of Inula britannica chinensis granule, includes the following steps:
A, Inula britannica chinensis medicinal material is removed into stalk, leaf and impurity and obtains Inula britannica chinensis medicine materical crude slice；
B, 2.5 times of amount water of Inula britannica chinensis medicine materical crude slice are soaked, spiral Continuous Countercurrent Extraction machine (stage type is continuously inputted by feed inlet
10 section pipe structures) extraction pipe, extraction pipe in by a set of helical structure by material continuously forward push to extraction pipe deslagging
Mouth is slagged tap, and continues 70 DEG C of hot water Continuous Countercurrent Extraction 1.5h that 16 times of amounts are inversely added in the ends of extraction pipes at different levels, and collection mentions
Liquid is taken, the Inula britannica chinensis dregs of a decoction are then exhausted from after squeezing recovery section medical fluid, the part medical fluid of recycling merges with extracting solution；It is described broken
The input speed of Inula britannica chinensis after broken is 50kg/h, and 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 Inula britannica chinensis granule.
Comparative example 1: Chinese medicine extracting tank is used
A kind of preparation method of Inula britannica chinensis granule, includes the following steps:
A, Inula britannica chinensis medicinal material is removed into stalk, leaf and impurity and obtains Inula britannica chinensis medicine materical crude slice；
B, Inula britannica chinensis 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 12 times of amounts is heated and decocted
0.5h, the water heating of second plus 8 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 Inula britannica chinensis granule.
Comparative example 2: pot group type countercurrent extraction machine is used
A kind of preparation method of Inula britannica chinensis granule, includes the following steps:
A, Inula britannica chinensis medicinal material is removed into stalk, leaf and impurity and obtains Inula britannica chinensis 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 Inula britannica chinensis granule.
The Inula britannica chinensis granule that embodiment and comparative example is prepared, measurement 3,5-OTwo-caffeoyl quinic acid contains
Amount calculates paste-forming rate, rate of transform situation, and the results are shown in Table 1:
1 Inula britannica chinensis 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 heat-sensitive ingredients 3,5-OTwo-caffeoyl quinic acid content, hence it is evident that mention
The high rate of transform, shows that the present invention is substantially better than common extractor currently on the market using Continuous Countercurrent Extraction technology and extracts skill
Art.
By embodiment 1 compared with 2 result of comparative example it is found that compared with pot group type countercurrent extraction machine, the continuous flow upstream of use
Extractive technique either paste-forming rate or heat-sensitive ingredients 3,5-OTwo-caffeoyl quinic acid content and the rate of transform are mentioned
Height, the i.e. present invention are better than pot group type countercurrent extraction machine using Continuous Countercurrent Extraction technology.
By embodiment 1, it is found that the present invention is used, by extracting solution, cooling is handled rapidly compared with 2 result of embodiment, can be kept away
Exempt from the degradation 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
Significantly improve heat-sensitive ingredients 3,5-OTwo-caffeoyl quinic acid content and the rate of transform, and then improve 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,
For a kind of novel extracting mode of economical and energy saving.
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.
Embodiment 6:
A kind of preparation method of honey Inula britannica chinensis granule, includes the following steps:
A, Inula britannica chinensis medicinal material is removed into stalk, leaf and impurity, is added and uses the diluted refined honey of boiling water, it is bored, it is tack-free with being fried with slow fire,
Obtain sweet Inula britannica chinensis medicine materical crude slice；
B, 2 times of amount water of sweet Inula britannica chinensis medicine materical crude slice are soaked, spiral Continuous Countercurrent Extraction machine (stage type is continuously inputted by feed inlet
10 section pipe structures) extraction pipe, extraction pipe in by a set of helical structure by material continuously forward push to extraction pipe deslagging
Mouth is slagged tap, and continues 95 DEG C of hot water Continuous Countercurrent Extraction 1h that 20 times of amounts are inversely added in the ends of extraction pipes at different levels, and collection is extracted
The sweet Inula britannica chinensis dregs of a decoction are then exhausted from by liquid after squeezing recovery section medical fluid, and the part medical fluid of recycling merges with extracting solution；The honey
The input speed of Inula britannica chinensis medicine materical crude slice is 100kg/h, and the reverse flow velocity that hot water is added is 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 sweet Inula britannica chinensis granule.
Embodiment 7:
A kind of preparation method of honey Inula britannica chinensis granule, includes the following steps:
A, Inula britannica chinensis medicinal material is removed into stalk, leaf and impurity, is added and uses the diluted refined honey of boiling water, it is bored, it is tack-free with being fried with slow fire,
Obtain sweet Inula britannica chinensis medicine materical crude slice；
B, 2 times of amount water of sweet Inula britannica chinensis medicine materical crude slice are soaked, spiral Continuous Countercurrent Extraction machine (stage type is continuously inputted by feed inlet
10 section pipe structures) extraction pipe, extraction pipe in by a set of helical structure by material continuously forward push to extraction pipe deslagging
Mouth is slagged tap, and continues 95 DEG C of hot water Continuous Countercurrent Extraction 1h that 20 times of amounts are inversely added in the ends of extraction pipes at different levels, and collection is extracted
The sweet Inula britannica chinensis dregs of a decoction are then exhausted from by liquid after squeezing recovery section medical fluid, and the part medical fluid of recycling merges with extracting solution；The honey
The input speed of Inula britannica chinensis medicine materical crude slice is 100kg/h, and the reverse flow velocity that hot water is added is 2000L/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 sweet Inula britannica chinensis granule.
Embodiment 8:
A kind of preparation method of honey Inula britannica chinensis granule, includes the following steps:
A, Inula britannica chinensis medicinal material is removed into stalk, leaf and impurity, is added and uses the diluted refined honey of boiling water, it is bored, it is tack-free with being fried with slow fire,
Obtain sweet Inula britannica chinensis medicine materical crude slice；
B, 2 times of amount water of sweet Inula britannica chinensis medicine materical crude slice are soaked, spiral Continuous Countercurrent Extraction machine (stage type is continuously inputted by feed inlet
10 section pipe structures) extraction pipe, extraction pipe in by a set of helical structure by material continuously forward push to extraction pipe deslagging
Mouth is slagged tap, and continues 80 DEG C of hot water Continuous Countercurrent Extraction 1h that 18 times of amounts are inversely added in the ends of extraction pipes at different levels, and collection is extracted
The sweet Inula britannica chinensis dregs of a decoction are then exhausted from by liquid after squeezing recovery section medical fluid, and the part medical fluid of recycling merges with extracting solution；The honey
The input speed of Inula britannica chinensis medicine materical crude slice is 100kg/h, and the reverse flow velocity that hot water is added is 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 sweet Inula britannica chinensis granule.
Embodiment 9:
A kind of preparation method of honey Inula britannica chinensis granule, includes the following steps:
A, Inula britannica chinensis medicinal material is removed into stalk, leaf and impurity, is added and uses the diluted refined honey of boiling water, it is bored, it is tack-free with being fried with slow fire,
Obtain sweet Inula britannica chinensis medicine materical crude slice；
B, sweet Inula britannica chinensis medicine materical crude slice is continuously inputted to spiral Continuous Countercurrent Extraction machine (10 section pipe structure of stage type) by feed inlet
Material is continuously pushed to forward extraction pipe slag-drip opening by a set of helical structure in extraction pipe and slagged tap, at different levels by extraction pipe
The end of extraction pipe continues 80 DEG C of hot water Continuous Countercurrent Extraction 1h that 18 times of amounts are inversely added, and extracting solution is collected, by sweet Inula britannica chinensis
Dregs of a decoction discharge；The input speed of the honey Inula britannica chinensis medicine materical crude slice is 100kg/h, and the reverse flow velocity that hot water is added is 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 sweet Inula britannica chinensis granule.
Embodiment 10:
A kind of preparation method of honey Inula britannica chinensis granule, includes the following steps:
A, Inula britannica chinensis medicinal material is removed into stalk, leaf and impurity, is added and uses the diluted refined honey of boiling water, it is bored, it is tack-free with being fried with slow fire,
Obtain sweet Inula britannica chinensis medicine materical crude slice；
B, 2.5 times of amount water of sweet Inula britannica chinensis medicine materical crude slice are soaked, spiral Continuous Countercurrent Extraction machine (twin-stage is continuously inputted by feed inlet
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 continued 70 DEG C of hot water Continuous Countercurrent Extraction 1.5h that 16 times of amounts are inversely added in the end of extraction pipes at different levels, is collected
The sweet Inula britannica chinensis dregs of a decoction are then exhausted from by extracting solution after squeezing recovery section medical fluid, and the part medical fluid of recycling merges with extracting solution；Institute
The input speed for stating broken sweet Inula britannica chinensis is 50kg/h, and 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, and dry granulation obtains sweet Inula britannica chinensis formula
Grain.
Comparative example 3: Chinese medicine extracting tank is used
A kind of preparation method of honey Inula britannica chinensis granule, includes the following steps:
A, Inula britannica chinensis medicinal material is removed into stalk, leaf and impurity, is added and uses the diluted refined honey of boiling water, it is bored, it is tack-free with being fried with slow fire,
Obtain sweet Inula britannica chinensis medicine materical crude slice；
B, sweet Inula britannica chinensis medicine materical crude slice is added in Chinese medicine extracting tank, with water boiling and extraction 2 times, for the first time plus the heating of the water of 12 times of amounts is decocted
0.5h is boiled, the water heating of second plus 8 times amount decocts 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 sweet Inula britannica chinensis granule.
Comparative example 4: pot group type countercurrent extraction machine is used
A kind of preparation method of honey Inula britannica chinensis granule, includes the following steps:
A, Inula britannica chinensis medicinal material is removed into stalk, leaf and impurity, is added and uses the diluted refined honey of boiling water, it is bored, it is tack-free with being fried with slow fire,
Obtain sweet Inula britannica chinensis 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 sweet Inula britannica chinensis granule.
The sweet Inula britannica chinensis granule that embodiment and comparative example is prepared, measurement 3,5-OTwo-caffeoyl quinic acid
Content calculates paste-forming rate, rate of transform situation, and the results are shown in Table 1:
The sweet Inula britannica chinensis granule embodiment of table 1 is compared with comparative example result
。
Claims (10)
1. the preparation method of a kind of Inula britannica chinensis or sweet Inula britannica chinensis granule, which comprises the steps of:
A, by the pre-treatment of Inula britannica chinensis medicinal material or processing, Inula britannica chinensis or sweet Inula britannica chinensis medicine materical crude slice are obtained；
B, the extraction pipe that Inula britannica chinensis or sweet Inula britannica chinensis medicine materical crude slice are continuously inputted to Continuous Countercurrent Extraction machine by feed inlet, in extraction pipe
Material is continuously pushed to forward extraction pipe slag-drip opening by a set of helical structure to slag tap, is continued in the end of extraction pipes at different levels inverse
To be added 10~30 times amount hot water, preferably 15~20 times amount, continuous dynamic countercurrent extract 0.25~3.0h, preferably 0.5
~2h collects extracting solution, and the dregs of a decoction are discharged；
C, extracting solution filters, ultra high temperature short time sterilization, and filtrate is concentrated under reduced pressure into relative density as 1.01 at 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 Inula britannica chinensis or sweet Inula britannica chinensis granule.
2. the preparation method of Inula britannica chinensis according to claim 1 or sweet Inula britannica chinensis granule, which is characterized in that step a
In, the pre-treatment is that Inula britannica chinensis medicinal material is removed stalk, leaf and impurity；It is described processing be by Inula britannica chinensis medicinal material remove stalk, leaf and
Impurity is added and uses the diluted refined honey of boiling water, bored, tack-free with being fried with slow fire, and obtains sweet Inula britannica chinensis medicine materical crude slice.
3. the preparation method of Inula britannica chinensis according to claim 1 or sweet Inula britannica chinensis granule, which is characterized in that step b
In, it is inputted in continuous dynamic countercurrent extractor again after the water wetting of 1~5 times of amount is first added in Inula britannica chinensis or sweet Inula britannica chinensis medicine materical crude slice.
4. the preparation method of Inula britannica chinensis according to claim 1 or sweet Inula britannica chinensis granule, which is characterized in that step b
In, the Continuous Countercurrent Extraction machine is spiral Continuous Countercurrent Extraction machine, is 10 section pipe structure of stage type.
5. the preparation method of Inula britannica chinensis according to claim 1 or sweet Inula britannica chinensis granule, which is characterized in that step b
In, the temperature of the hot water is 40~95 DEG C, preferably 70~85 DEG C.
6. the preparation method of Inula britannica chinensis according to claim 1 or sweet Inula britannica chinensis granule, which is characterized in that step b
In, the dregs of a decoction are then exhausted from after squeezing recovery section medical fluid, the part medical fluid of recycling merges with extracting solution.
7. the preparation method of Inula britannica chinensis according to claim 1 or sweet Inula britannica chinensis granule, which is characterized in that step b
In, the coarse grained input speed is 100~200kg/h, and the reverse flow velocity that hot water is added is 1000~5000kg/h.
8. the preparation method of Inula britannica chinensis according to claim 1 or sweet Inula britannica chinensis granule, which is characterized in that step c
In, it is refiltered after extracting solution is first cooled to 40~55 DEG C；The ultra high temperature short time sterilization is that filtrate is instantaneously gone out in superhigh temperature
It sterilizes 2~30 seconds at 100~150 DEG C in bacterium device.
9. the preparation method of Inula britannica chinensis according to claim 1 or sweet Inula britannica chinensis granule, which is characterized in that step d
In, the auxiliary material is one or more of maltodextrin, dextrin, starch, lactose or beta-cyclodextrin；The work of the spray drying
Skill parameter are as follows: 140 DEG C~200 DEG C of inlet air temperature, 50 DEG C~95 DEG C of leaving air temp of control.
10. the preparation method of Inula britannica chinensis according to claim 1 or sweet Inula britannica chinensis granule, which is characterized in that step e
In, the pharmaceutical adjunct is the mixing of one or more of maltodextrin, silica or magnesium stearate, and dosage is dry extract
The 0.01~0.5% of powder weight.
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| CN106990182A (en) * | 2017-04-06 | 2017-07-28 | 广州市香雪制药股份有限公司 | The characteristic spectrum of Inula britannica chinensis granule is set up and detection method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106990182A (en) * | 2017-04-06 | 2017-07-28 | 广州市香雪制药股份有限公司 | The characteristic spectrum of Inula britannica chinensis granule is set up and detection method |
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| 广西壮族自治区食品药品监督管理局: "《广西壮族自治区中药配方颗粒质量标准.第一卷》", 30 November 2016, 广西科学技术出版社 * |
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Application publication date: 20190405 |