CN109568440A - A kind of preparation method of root bark of Chinese wolf-berry granule - Google Patents
A kind of preparation method of root bark of Chinese wolf-berry granule Download PDFInfo
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- CN109568440A CN109568440A CN201811301207.7A CN201811301207A CN109568440A CN 109568440 A CN109568440 A CN 109568440A CN 201811301207 A CN201811301207 A CN 201811301207A CN 109568440 A CN109568440 A CN 109568440A
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- 244000241872 Lycium chinense Species 0.000 title claims abstract description 81
- 235000015468 Lycium chinense Nutrition 0.000 title claims abstract description 81
- 239000008187 granular material Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000000605 extraction Methods 0.000 claims abstract description 100
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- 239000000463 material Substances 0.000 claims abstract description 45
- 239000003814 drug Substances 0.000 claims abstract description 32
- 239000000284 extract Substances 0.000 claims abstract description 31
- 238000007908 dry granulation Methods 0.000 claims abstract description 15
- 239000006071 cream Substances 0.000 claims abstract description 14
- 230000001954 sterilising effect Effects 0.000 claims abstract description 13
- 230000002829 reductive effect Effects 0.000 claims abstract description 12
- 238000001694 spray drying Methods 0.000 claims abstract description 12
- 238000004659 sterilization and disinfection Methods 0.000 claims abstract description 11
- 239000000706 filtrate Substances 0.000 claims abstract description 6
- 238000004090 dissolution Methods 0.000 claims abstract description 3
- 229920002774 Maltodextrin Polymers 0.000 claims description 14
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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 14
- 229940035034 maltodextrin Drugs 0.000 claims description 14
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- 235000019359 magnesium stearate Nutrition 0.000 claims description 7
- 230000036961 partial effect Effects 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 5
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 claims description 4
- 229920000858 Cyclodextrin Polymers 0.000 claims description 4
- 229920001353 Dextrin Polymers 0.000 claims description 4
- 239000004375 Dextrin Substances 0.000 claims description 4
- 239000001116 FEMA 4028 Substances 0.000 claims description 4
- 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 4
- 229920002472 Starch Polymers 0.000 claims description 4
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims description 4
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims description 4
- 229960004853 betadex Drugs 0.000 claims description 4
- 235000019425 dextrin Nutrition 0.000 claims description 4
- 239000008101 lactose Substances 0.000 claims description 4
- 238000011084 recovery Methods 0.000 claims description 4
- 239000002893 slag Substances 0.000 claims description 4
- 239000008107 starch Substances 0.000 claims description 4
- 235000019698 starch Nutrition 0.000 claims description 4
- 238000002203 pretreatment Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 229940079593 drug Drugs 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims 2
- 239000000377 silicon dioxide Substances 0.000 claims 1
- 238000009736 wetting Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 20
- 239000000470 constituent Substances 0.000 abstract description 10
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- 239000012467 final product Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 31
- IWRAOCFRRTWUDF-UHFFFAOYSA-N Kukoamine B Chemical compound C=1C=C(O)C(O)=CC=1CCC(=O)N(CCCN)CCCCNCCCNC(=O)CCC1=CC=C(O)C(O)=C1 IWRAOCFRRTWUDF-UHFFFAOYSA-N 0.000 description 30
- 239000002904 solvent Substances 0.000 description 19
- 239000004615 ingredient Substances 0.000 description 13
- 230000015556 catabolic process Effects 0.000 description 8
- 238000006731 degradation reaction Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 241000196324 Embryophyta Species 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000002144 chemical decomposition reaction Methods 0.000 description 4
- 244000005700 microbiome Species 0.000 description 4
- 230000002411 adverse Effects 0.000 description 3
- 241001609931 bacterium 20 Species 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 230000033001 locomotion Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000011144 upstream manufacturing Methods 0.000 description 3
- 244000241838 Lycium barbarum Species 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004886 process control Methods 0.000 description 2
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- 238000005550 wet granulation Methods 0.000 description 2
- 235000015459 Lycium barbarum Nutrition 0.000 description 1
- 241000208292 Solanaceae Species 0.000 description 1
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- 241000385540 bacterium 10 Species 0.000 description 1
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- 238000002386 leaching Methods 0.000 description 1
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- 239000010703 silicon Substances 0.000 description 1
- 235000014347 soups Nutrition 0.000 description 1
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- 239000004408 titanium dioxide Substances 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)
- A61K36/81—Solanaceae (Potato family), e.g. tobacco, nightshade, tomato, belladonna, capsicum or jimsonweed
- A61K36/815—Lycium (desert-thorn)
-
- 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
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
- A61L2/0005—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor for pharmaceuticals, biologicals or living parts
- A61L2/0011—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor for pharmaceuticals, biologicals or living parts using physical methods
- A61L2/0023—Heat
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- 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
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
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- 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
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2202/00—Aspects relating to methods or apparatus for disinfecting or sterilising materials or objects
- A61L2202/20—Targets to be treated
- A61L2202/21—Pharmaceuticals, e.g. medicaments, artificial body parts
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Abstract
The invention discloses a kind of preparation methods of root bark of Chinese wolf-berry granule, comprising: a, by root bark of Chinese wolf-berry medicine materical crude slice is carried out broken or is chopped into coarse granule；B, coarse granule is continuously inputted to Continuous Countercurrent Extraction machine, 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, clear cream dissolution is added in auxiliary material, 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 root bark of Chinese wolf-berry granule.
Description
Technical field
The invention belongs to Chinese medicinal granule technical fields, and in particular to a kind of preparation method of root bark of Chinese wolf-berry granule.
Background technique
The root bark of Chinese wolf-berry is matrimony vine of solanaceae plant Lycium chinense Mill. or lycium barbarum Lycium barbarum L.
Dry root skin.Root is excavated at the beginning of spring or after autumn, is cleaned, is stripped root skin, dry.
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, most of Chinese medicine mentions the existing production technology of root bark of Chinese wolf-berry Chinese medicinal granule
The industrialization extraction process for taking object is all two pan-fried techniques, and since root bark of Chinese wolf-berry medicinal material is light, when decoction swims in liquid level, it is difficult to sufficiently
It decocts, production efficiency is low, and temperature is high, decocting time is long, production efficiency is low, energy consumption is at high cost, the root bark of Chinese wolf-berry is active in the presence of decocting
The defects of component damages are more.Ground bone main active is soluble easily in water, if extraction process is insufficient, clear cream ingredient sterilize,
It is influenced to degrade by long-time high temperature in wet granulation drying course, thus causes the rate of transform low, content deviates standard soup
Agent technical requirements range, influences clinical application safely, 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 that root bark of Chinese wolf-berry granule is prepared using continuous dynamic countercurrent water extraction process.
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 root bark of Chinese wolf-berry granules
Preparation method, this method is using Continuous Countercurrent Extraction, high temperature, short time sterilizing, reduced pressure, instantaneous spray drying and dry granulation
Production technology enables active constituent content in root bark of Chinese wolf-berry granule sustainedly and stably to reach higher level, it is ensured that the root bark of Chinese wolf-berry
The rate of transform of active constituent reaches root bark of Chinese wolf-berry standard decoction technical requirements range in granule.
The present invention is achieved through the following technical solutions；
A kind of preparation method of root bark of Chinese wolf-berry granule, includes the following steps:
A, by root bark of Chinese wolf-berry medicinal material pre-treatment, root bark of Chinese wolf-berry medicine materical crude slice is obtained, then carry out broken or is chopped into coarse granule；
B, the extraction pipe that the coarse granule after broken or chopping is continuously inputted to Continuous Countercurrent Extraction machine by the feed inlet of front end, is soaking
It mentions and material is continuously pushed to forward by extraction pipe slag-drip opening by a set of helical structure in pipe slags tap, in the ends of extraction pipes at different levels
Be continuously added into 10~24 times amount hot water, preferably 12~20 times amount, continuous dynamic countercurrent extract 0.5~3.0h, preferably 1~
2h, hot water and material collect 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 filtrate is concentrated under reduced pressure into relative density as 1.00 at 55~65 DEG C~
1.10 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 root bark of Chinese wolf-berry granule.
The present invention carries out the extraction process of the root bark of Chinese wolf-berry, 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 root bark of Chinese wolf-berry 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.
The pre-treatment is to sort root bark of Chinese wolf-berry medicinal material, remove impurity, obtains root bark of Chinese wolf-berry medicine materical crude slice.
The size of the broken partial size of raw material will affect whether effective component can be fully dissolved out, while influence extraction process object
Whether push movement is smooth forward for material, is unfavorable for solute if partial size is excessive and quickly transmits into solvent, while existing to material
Smooth retard motion in Continuous Countercurrent Extraction is easy to miss from spiral plate hole and can not be successfully transmission if partial size is too small
To slag-drip opening, it is preferred that in step a, described broken or chopping partial size is 0.3~1.5cm.
Dry root bark of Chinese wolf-berry medicine materical crude slice is easy to appear in blanking process to get stuck, and the wet granular after water soaks is easier blanking,
To guarantee material can be made to come into full contact with Extraction solvent with the blanking of continuous and quantitative, while being conducive to effective component in material
Transfer is quickly extracted after blanking, it is preferred that defeated again after the water that 2~3 times of amounts are first added in root bark of Chinese wolf-berry medicine materical crude slice is soaked in step b
Enter 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℃ | 50℃ | 75℃ | 85℃ | 95℃ | 100℃ |
| The kukoamine B rate of transform (%) | 23.26 | 36.18 | 42.85 | 43.17 | 41.52 | 34.28 |
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 ingredients such as kukoamine B are easy to happen chemical degradation in aqueous solution, it is preferred that in step b, the temperature of the hot water
Degree is 50~95 DEG C, preferably 75~95 DEG C.
Solvent amount also directly influences the extraction and degradation of active constituent, and the present invention has further carried out solvent amount excellent
Change, concrete outcome is as follows:
| Solvent amount | 8 times of amounts | 10 times of amounts | 12 times of amounts | 16 times of amounts | 20 times of amounts | 24 times of amounts |
| The kukoamine B rate of transform (%) | 25.56 | 35.72 | 38.89 | 44.25 | 41.28 | 36.64 |
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 16 times of amounts, the kukoamine B 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 dropped in each process
Solution, so that the rate of transform of kukoamine B can be reduced.Therefore, the additional amount of the hot water is measured for 10~24 times, preferably 12~
20 times of 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 | 1.5h | 2h | 3h |
| The kukoamine B rate of transform (%) | 26.04 | 35.59 | 43.25 | 44.82 | 40.58 | 36.36 |
If extraction time is short it can be seen from the above results, active constituent physical transfer is incomplete, if extraction time mistake
Long, kukoamine B chemical degradation rate is high, while reducing production efficiency.Preferably, in step b, root bark of Chinese wolf-berry medicine materical crude slice is continuously being moved
Extraction time is 0.5~3.0h, preferably 1 ~ 2h in state adverse current extraction.
For the rate of transform for further increasing effective component, it is preferred that in step b, by the root bark of Chinese wolf-berry 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, so as to further increase returning for root bark of Chinese wolf-berry extracting solution
Yield increases the rate of transform of effective component.
Preferably, in step b, the coarse grained input speed is 100~250kg/h, the reverse flow velocity that hot water is added
For 1000~6000kg/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 held
It is easily added, is constantly updated, so that material be made to be constantly in biggish concentration gradient throughout the extraction process with certain flow velocity
Difference is conducive to being fully dissolved out for effective component, and then can greatly improve the rate of transform of effective component in the root bark of Chinese wolf-berry.
Root bark of Chinese wolf-berry medicine materical crude slice index components are soluble easily in water, in order to reduce component damages, further increase the rate of transform, the present invention is first
It will be refiltered after extracting solution cooling in step c, the present invention is further optimized cooling temperature, and concrete outcome is as follows:
| Cool down temperature | 30℃ | 45℃ | 55℃ | 65℃ | 75℃ |
| The kukoamine B rate of transform (%) | 34.25 | 45.34 | 44.86 | 42.32 | 38.78 |
The thermal degradation that can effectively avoid kukoamine B after extracting solution cooling it can be seen from the above results, is conducive to its content
Retain and improves the rate of transform.When being cooled to 30~65 DEG C of temperature ranges, kukoamine B thermal degradation is less and tends towards stability, together
When the temperature that is concentrated in conjunction with extracting solution after cooling in 55~65 DEG C of temperature ranges, to reduce heating energy when extracting solution concentration
Consumption, it is preferred that in step c, refiltered after extracting solution is first cooled to 45~55 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 kukoamine B from chemical degradation occurring in sterilization process, it is preferred that step
In c, the ultra high temperature short time sterilization is that filtrate sterilizes 2~30 seconds at 100~150 DEG C in supper high temperature instant sterilizer.
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: 160 DEG C~185 DEG C of inlet air temperature, 80 DEG C~100 DEG C of leaving air temp of control.
Preferably, in step e, the pharmaceutical adjunct is maltodextrin, dextrin, starch, lactose, beta-cyclodextrin, titanium dioxide
The mixing of one or more of silicon or magnesium stearate, dosage are the 0.01~0.5% of dry extract weight.
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 kukoamine B physics during the extraction process and dissolves out the rate of transform, at the same can with lower temperature into
Row temperature leaching is continuous to extract, and reduces the degradation of heat-sensitive ingredients at high temperature and destroys.
(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 kukoamine B in spray drying blending process, and preferably various systems
Grain 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 enable root bark of Chinese wolf-berry medicine materical crude slice Chinese medicinal granule kukoamine B content
Sustainedly and stably reach higher level, it is ensured that the active constituent rate of transform and root bark of Chinese wolf-berry standard decoction reach one in granule
It causes, improves the product quality of root bark of Chinese wolf-berry 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 root bark of Chinese wolf-berry granule, includes the following steps:
A, root bark of Chinese wolf-berry medicinal material is selected, shaking weeds out except impurity, obtains root bark of Chinese wolf-berry medicine materical crude slice, be then broken into the thick of 1.0cm with crusher
Particle；
B, 2 times of amount water of coarse granule are soaked, spiral Continuous Countercurrent Extraction machine (stage type is continuously inputted by the feed inlet of front end
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 is continuously added into 16 times of 90 DEG C of hot water Continuous Countercurrent Extraction 2h in the ends of extraction pipes at different levels, hot water is with material in inverse
Liquid is brought out to flowing to before extraction pipes at different levels, extracting solution is collected, the root bark of Chinese wolf-berry dregs of a decoction is arranged again after squeezing recovery section medical fluid
Out, the part medical fluid of recycling merges with extracting solution；The input speed of the root bark of Chinese wolf-berry medicine materical crude slice is 100kg/h, and hot water is inversely added
Flow velocity be 1600L/h；
C, the extracting solution after merging filters after being cooled to 55 DEG C, and filtered fluid goes out at 105 DEG C in supper high temperature instant sterilizer (UHT)
Bacterium 20 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: 160 DEG C ~ 175 DEG C of inlet air temperature, 80 DEG C ~ 90 DEG C of leaving air temp of control；
E, maltodextrin and magnesium stearate is added in dry extract, is uniformly mixed, dry granulation obtains root bark of Chinese wolf-berry granule.
Embodiment 2:
In step c, the extracting solution after merging does not cool down, and directly sterilizes 20 at 105 DEG C in supper high temperature instant sterilizer (UHT)
Second, after at 60 DEG C be concentrated under reduced pressure at relative density be 1.06 clear cream；
Remaining is the same as embodiment 1.
Embodiment 3:
It is in step b, coarse granule is nonwetting, spiral Continuous Countercurrent Extraction machine (stage type is continuously inputted by the feed inlet of front end
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 is continuously added into 16 times of 90 DEG C of hot water Continuous Countercurrent Extraction 2h in the ends of extraction pipes at different levels, hot water is with material in inverse
Liquid is brought out to flowing to before extraction pipes at different levels, extracting solution is collected, the root bark of Chinese wolf-berry dregs of a decoction is discharged；The input of the root bark of Chinese wolf-berry medicine materical crude slice
Speed is 100kg/h, and the reverse flow velocity that hot water is added is 1600L/h；
Remaining is the same as embodiment 1.
Embodiment 4:
A kind of preparation method of root bark of Chinese wolf-berry granule, includes the following steps:
A, root bark of Chinese wolf-berry medicinal material is selected, shaking weeds out except impurity, obtains root bark of Chinese wolf-berry medicine materical crude slice, be then broken into 1.0cm thick with crusher
Grain；
B, 2 times of amount water of coarse granule are soaked, spiral Continuous Countercurrent Extraction machine (stage type is continuously inputted by the feed inlet of front end
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 is continuously added into 18 times of 85 DEG C of hot water Continuous Countercurrent Extraction 1.5h in the ends of extraction pipes at different levels, hot water is with material in inverse
Liquid is brought out to flowing to before extraction pipes at different levels, extracting solution is collected, the root bark of Chinese wolf-berry dregs of a decoction is arranged again after squeezing recovery section medical fluid
Out, the part medical fluid of recycling merges with extracting solution；The input speed of the root bark of Chinese wolf-berry medicine materical crude slice is 100kg/h, and hot water is inversely added
Flow velocity be 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 65 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: 175 DEG C ~ 185 DEG C of inlet air temperature, 90 DEG C ~ 100 DEG C of leaving air temp of control；
E, maltodextrin and magnesium stearate is added in dry extract, is uniformly mixed, dry granulation obtains root bark of Chinese wolf-berry granule.
Embodiment 5:
A kind of preparation method of root bark of Chinese wolf-berry granule, includes the following steps:
A, root bark of Chinese wolf-berry medicinal material is selected, shaking weeds out except impurity, obtains root bark of Chinese wolf-berry medicine materical crude slice, be then broken into the thick of 1.0cm with crusher
Particle；
B, 2 times of amount water of coarse granule are soaked, spiral Continuous Countercurrent Extraction machine (stage type is continuously inputted by the feed inlet of front end
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 is continuously added into 20 times of 75 DEG C of hot water Continuous Countercurrent Extraction 1.5h in the ends of extraction pipes at different levels, hot water is with material in inverse
Liquid is brought out to flowing to before extraction pipes at different levels, extracting solution is collected, the root bark of Chinese wolf-berry dregs of a decoction is arranged again after squeezing recovery section medical fluid
Out, the part medical fluid of recycling merges with extracting solution；The input speed of the root bark of Chinese wolf-berry medicine materical crude slice is 60kg/h, reverse addition hot water
Flow velocity is 1200L/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 20 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: 175 DEG C ~ 185 DEG C of inlet air temperature, 90 DEG C ~ 100 DEG C of leaving air temp of control；
E, maltodextrin and magnesium stearate is added in dry extract, is uniformly mixed, dry granulation obtains root bark of Chinese wolf-berry granule.
Comparative example 1: Chinese medicine extracting tank is used
A kind of preparation method of root bark of Chinese wolf-berry granule, includes the following steps:
A, root bark of Chinese wolf-berry medicinal material is selected, shaking weeds out except impurity, obtains root bark of Chinese wolf-berry medicine materical crude slice, be then broken into the thick of 1.0cm with crusher
Particle；
B, root bark of Chinese wolf-berry 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 9 times of amounts is heated and decocted
1h, the water heating of second plus 7 times amount decoct 1h, 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: 160 DEG C ~ 175 DEG C of inlet air temperature, 80 DEG C ~ 90 DEG C of leaving air temp of control；
E, dry extract adds maltodextrin and magnesium stearate, is uniformly mixed, dry granulation obtains root bark of Chinese wolf-berry granule.
Comparative example 2: pot group type countercurrent extraction machine is used
A kind of preparation method of root bark of Chinese wolf-berry granule, includes the following steps:
A, root bark of Chinese wolf-berry medicinal material is selected, shaking weeds out except impurity, obtains root bark of Chinese wolf-berry medicine materical crude slice, be then broken into the thick of 1.0cm with crusher
Particle；
B, medicine materical crude slice is put into the series connection extractor group formed with 5 end to end extractors by the following arrangement mode that feeds intake,
Fresh solvent is added with material-water ratio 1:16 ratio in tail tank, is extracted with 90 DEG C of each tank Extracting temperature, extraction time 2.0h:
Material in 5 tanks be successively new medicine materical crude slice, through 1 time extract after the dregs of a decoction, through 2 times extract the dregs of a decoction, through 3 times extract the dregs of a decoction,
Fresh solvent is added in (dregs of a decoction after extracting equipped with the 4th) tank of most end, other each tanks by the dregs of a decoction extracted through 4 times
It is sequentially arranged with from the extracting solution that next stage tank transfer moves past and extracts, final extracting solution is discharged from the tank of foremost, most
Extractor afterwards is discharged the dregs of a decoction and is packed into new medicine materical crude slice, becomes most preceding extractor, and so circulation is reverse extracts, collection extracting solution filter
Cross merging；
C, the extracting solution after merging filters after being cooled to 55 DEG C, and filtered fluid goes out at 105 DEG C in supper high temperature instant sterilizer (UHT)
Bacterium 20 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: 160 DEG C ~ 175 DEG C of inlet air temperature, 80 DEG C ~ 90 DEG C of leaving air temp of control；
E, maltodextrin and magnesium stearate is added in dry extract, is uniformly mixed, dry granulation obtains root bark of Chinese wolf-berry granule.
The root bark of Chinese wolf-berry granule that embodiment and comparative example is prepared measures kukoamine B content, calculates cream
Rate, rate of transform situation, the results are shown in Table 1:
1 root bark of Chinese wolf-berry 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, embodiment 1 can continuous slag charge squeeze, continuous automatic slag-liquid separation, realize whole serialization, automatic control,
Fast low temperature extracts, and remains index components content, hence it is evident that improves the rate of transform, shows the present invention using Continuous Countercurrent Extraction skill
Art is substantially better than common extractor extractive technique currently on the market.
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 index components content and the rate of transform increase, i.e., the present invention uses continuous flow upstream
Extractive technique is 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
Index components and the rate of transform are significantly improved, and then improves the quality of product.Meanwhile continuous dynamic countercurrent technology is guaranteeing cream out
In the case where rate, component content and the rate of transform, it can be further reduced the consumption of solvent, be a kind of novel extraction side of economical and energy saving
Formula.
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 root bark of Chinese wolf-berry granule, which comprises the steps of:
A, by root bark of Chinese wolf-berry medicinal material pre-treatment, root bark of Chinese wolf-berry medicine materical crude slice is obtained, then carry out broken or is chopped into coarse granule；
B, the extraction pipe that the coarse granule after broken or chopping is continuously inputted to Continuous Countercurrent Extraction machine by the feed inlet of front end, is soaking
It mentions and material is continuously pushed to forward by extraction pipe slag-drip opening by a set of helical structure in pipe slags tap, in the ends of extraction pipes at different levels
Be continuously added into 10~24 times amount hot water, preferably 12~20 times amount, continuous dynamic countercurrent extract 0.5~3.0h, preferably 1~
2h, hot water and material collect 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 1.00~1.10 that filtrate, which is concentrated under reduced pressure into relative density at 55-65 DEG C,
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 root bark of Chinese wolf-berry granule.
2. the preparation method of root bark of Chinese wolf-berry granule according to claim 1, which is characterized in that in step a, locate before described
Reason is to sort root bark of Chinese wolf-berry medicinal material, remove impurity, obtains root bark of Chinese wolf-berry medicine materical crude slice；Described broken or chopping partial size is 0.3-1.5cm.
3. the preparation method of root bark of Chinese wolf-berry granule according to claim 1, which is characterized in that in step b, by the root bark of Chinese wolf-berry
Medicine materical crude slice inputs in continuous dynamic countercurrent extractor again after the water wetting of 2~3 times of amounts is first added.
4. the preparation method of root bark of Chinese wolf-berry 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 root bark of Chinese wolf-berry granule according to claim 1, which is characterized in that in step b, the hot water
Temperature be 50~95 DEG C, preferably 75~95 DEG C.
6. the preparation method of root bark of Chinese wolf-berry 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 root bark of Chinese wolf-berry granule according to claim 1, which is characterized in that in step b, described thick
The input speed of grain is 100~250kg/h, and the reverse flow velocity that hot water is added is 1000~6000kg/h.
8. the preparation method of root bark of Chinese wolf-berry granule according to claim 1, which is characterized in that in step c, will first extract
Liquid refilters after being cooled to 45~55 DEG C；The ultra high temperature short time sterilization be by filtrate 100 in supper high temperature instant sterilizer~
It sterilizes 2~30 seconds at 150 DEG C.
9. the preparation method of root bark of Chinese wolf-berry 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
160 DEG C~185 DEG C of inlet air temperature processed, 80 DEG C~100 DEG C of leaving air temp.
10. the preparation method of root bark of Chinese wolf-berry granule according to claim 1, which is characterized in that in step e, the system
Agent auxiliary material is the mixed of one or more of maltodextrin, dextrin, starch, lactose, beta-cyclodextrin, silica or magnesium stearate
It closes, dosage is the 0.01~0.5% of dry extract weight.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110974901A (en) * | 2019-12-21 | 2020-04-10 | 江西济民可信金水宝制药有限公司 | Preparation method of heat-clearing and detoxifying granules |
| CN111557984A (en) * | 2020-06-15 | 2020-08-21 | 劲牌持正堂药业有限公司 | Preparation method of cortex lycii radicis extract for improving hygroscopicity |
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2018
- 2018-11-02 CN CN201811301207.7A patent/CN109568440A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110974901A (en) * | 2019-12-21 | 2020-04-10 | 江西济民可信金水宝制药有限公司 | Preparation method of heat-clearing and detoxifying granules |
| CN111557984A (en) * | 2020-06-15 | 2020-08-21 | 劲牌持正堂药业有限公司 | Preparation method of cortex lycii radicis extract for improving hygroscopicity |
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