CN109568359A - A kind of preparation method of angelica dahurica root dispensing granule - Google Patents
A kind of preparation method of angelica dahurica root dispensing granule Download PDFInfo
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- CN109568359A CN109568359A CN201810119001.6A CN201810119001A CN109568359A CN 109568359 A CN109568359 A CN 109568359A CN 201810119001 A CN201810119001 A CN 201810119001A CN 109568359 A CN109568359 A CN 109568359A
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- angelica dahurica
- angelica
- preparation
- root
- dispensing granule
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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)
- A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
- A61K36/232—Angelica
-
- 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
-
- 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, 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
Abstract
The invention discloses a kind of preparation method of angelica dahurica root dispensing granule, comprising steps of a, angelica root selected, shaking weeds out except impurity, be crushed；B, broken angelica dahurica decoction pieces are inputted in continuous dynamic countercurrent extractor, it is reverse that the 12-14 times of hot water measured progress continuous dynamic countercurrent extraction 1.5-2.5h is added, extracting solution is collected, the root of Dahurain angelica dregs of a decoction are discharged；C, extracting solution filters, and relative density is the clear cream of 1.02-1.05 when filtrate decompression is condensed into 65 DEG C；D, qinghuo reagent is spray-dried, and obtains dry extract, and dry extract dry granulation obtains angelica dahurica root dispensing granule.The present invention uses continuous dynamic countercurrent extraction process, angelica dahurica decoction pieces are inversely contacted with Extraction solvent, entire extraction process concentration gradient can remain at higher level, compared with traditional conventional can extraction process, not only the consumption of solvent is few, but also greatly improves the recovery rate of root of Dahurain angelica effective component, ensure that product quality, entreprise cost is reduced, industrial competition is improved.
Description
Technical field
The invention belongs to Chinese medicinal granule technical fields, and in particular to a kind of preparation method of angelica dahurica root dispensing granule.
Background technique
The root of Dahurain angelica is umbellate form section plant root of Dahurain angelica Angelica dahurica (Fisch.ex Hoffm.) Benth. et
Hook.f. or Radix angelicae dahuricae Angelica dahurica(Fisch.ex Hoffm.) Benth.et Hook.f.
Var.formosana(Boiss.) the dry root of Shan et Yuan.It is acrid in flavour and warm in nature, return stomach, large intestine, lung channel.It dehumidifies with relieve heat,
The effect of sensible analgesic, detumescence and apocenosis, is used for cold headache, pain in the supra-orbital bone, nasal obstruction, nasosinusitis, toothache, leukorrhea, sore swell and ache curative.
Chinese medicinal granule is to meet the traditional Chinese medicine medicine materical crude slice of concocted specification as raw material, extract, be concentrated through modern industry,
Dry, granulation, refined pure Chinese medicine series of products, as the new alternative prepared slices of Chinese crude drugs of medicine materical crude slice form for clinical syndrome differentiation opinion
It controls, added and subtracted with card, formula uses.Chinese medicinal granule realized in clinical use medication " highly effective and safe, it is stably and controllable,
It is convenient and healthy ".Since Chinese medicinal granule has small dosage form, good effect, quick, takes, carries, stores the features such as facilitating,
Adapt to very much the needs that modern society includes demand and fast pace life of the international community to natural drug.
Chinese medicinal granule industrialization at present is extracted mainly using the static decocting method extracted, most of traditional Chinese medicine extraction
The industrialization extraction process of object is all two pan-fried techniques, exist decoct temperature is high, decocting time is long, production efficiency is low, energy consumption at
The defects of this is big, loss of effective components is more.
Continuous dynamic countercurrent extraction is novel extraction process in recent years, it collects extraction, weight diacolation, dynamic and adverse current skill
What art was integrated has many advantages, such as that simple process, saving solvent, low energy consumption, extraction time is short, extraction efficiency is high.Currently, not yet
See the report using continuous dynamic countercurrent extraction process preparation angelica dahurica root dispensing granule.
Summary of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of preparations of angelica dahurica root dispensing granule
Method, this method are extracted using continuous dynamic countercurrent, greatly improve the recovery rate of angelica dahurica root dispensing granule, ensure that product matter
Amount.
The present invention is achieved through the following technical solutions；
A kind of preparation method of angelica dahurica root dispensing granule, includes the following steps:
A, angelica root is selected, shaking weeds out except impurity, be crushed；
B, broken angelica dahurica decoction pieces are inputted in continuous dynamic countercurrent extractor, it is reverse that the 12-14 times of hot water measured progress is added
Continuous Countercurrent Extraction 1.5-2.5h collects extracting solution, and the root of Dahurain angelica dregs of a decoction are discharged；
C, extracting solution filters, and relative density is the clear cream of 1.02-1.05 when filtrate decompression is condensed into 65 DEG C；
D, qinghuo reagent is spray-dried, and obtains dry extract, and dry extract dry granulation obtains angelica dahurica root dispensing granule.
The present invention carries out the extraction process of the root of Dahurain angelica using continuous dynamic countercurrent extractor, in continuous dynamic countercurrent extractor
Feed inlet input angelica dahurica decoction pieces enter extraction tube, and mobile to the slag-drip opening of continuous dynamic countercurrent extractor in extraction tube.?
The deslagging end of continuous dynamic countercurrent extractor is added Extraction solvent and enters extraction tube, and relative to continuous dynamic inverse in extraction tube
The leakage fluid dram of stream extractor inversely moves.In extraction tube, the flow direction of the root of Dahurain angelica and Extraction solvent is on the contrary, making the root of Dahurain angelica and extracting
Solvent comes into full contact with, and concentration gradient can remain at higher level, so that biggish mass transfer force is formed, it can be very big
Raising effective component recovery rate.
Whether the size of the broken partial size of angelica dahurica decoction pieces will affect effective component and can be fully dissolved out and extraction process object
Whether material movement is smooth, is unfavorable for solute if angelica dahurica decoction pieces partial size is excessive and quickly transmits into solvent, while existing to material
Smooth retard motion in Continuous Countercurrent Extraction, if angelica dahurica decoction pieces partial size is too small material be easy float, be unfavorable for effectively at
The abundant extraction divided, while subsequent shingle is filtered more difficult, it is preferred that in step a, the broken partial size is 0.2-
0.5cm。
Dry angelica dahurica decoction pieces are easy to appear in blanking process to get stuck, and the angelica dahurica decoction pieces after water soaks are easier blanking,
To guarantee the root of Dahurain angelica 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 in step b, after the 1-2 times of water measured wetting is first added in broken angelica dahurica decoction pieces
It is inputted in continuous dynamic countercurrent extractor again.
The present invention is to extract solvent with water, if the temperature of water is lower, may cause effective component and extracts not exclusively, if
The temperature of water is excessively high, and the heat-sensitive ingredients in angelica dahurica decoction pieces are easy loss, to extract effective component to greatest extent, preferably
, in step b, the temperature of the hot water is 60-70 DEG C.
Continuous dynamic countercurrent extractor of the invention is 10 section pipe of stage type, ensure that filling for effective component in angelica dahurica decoction pieces
Divide dissolution.
Preferably, in step b, the input speed of the broken angelica dahurica decoction pieces is 200-250kg/h, reverse that heat is added
The flow velocity of water is 2000-3250kg/h.The present invention is fed by continuous and quantitative, comes into full contact with angelica dahurica decoction pieces with Extraction solvent,
The extraction of equipment is easy to be added with certain flow velocity, constantly updates, so that angelica dahurica decoction pieces be made to locate always throughout the extraction process
It is poor in biggish concentration gradient, be conducive to being fully dissolved out for effective component, and then can greatly improve in angelica dahurica decoction pieces effectively at
The rate of transform divided.
For the recovery rate for further increasing effective component, it is preferred that in step b, by the root of Dahurain angelica dregs of a decoction through squeezing recovery section
It being then exhausted from after medical fluid, the part medical fluid of recycling merges with extracting solution, so as to further increase the rate of recovery of root of Dahurain angelica extracting solution,
Increase the rate of transform of effective component.
Contain heat-sensitive ingredients in angelica dahurica decoction pieces, in order to avoid heat-sensitive ingredients decomposition, further increases recovery rate, preferably
, it in step c, is refiltered after extracting solution is first cooled to 45-55 DEG C, to slow down the degradation of heat-sensitive ingredients.
Preferably, in step c, the filtering is filtered using centrifuge, and the revolving speed of centrifugation is 2000-3000r/min
For the decomposition for avoiding heat-sensitive ingredients, it is preferred that in step c, the temperature of the reduced pressure is 55-65 DEG C.
Preferably, in step d, the technological parameter of the spray drying are as follows: 175 DEG C ~ 185 DEG C of inlet air temperature of control, outlet air
85 DEG C ~ 95 DEG C of temperature.
Compared with prior art, the present invention having the following beneficial effects:
(1) present invention is to extract solvent with water, complies fully with what the prepared slices of Chinese crude drugs that traditional Chinese medicine theory is praised highly were used as medicine with decoction
Viewpoint, using continuous dynamic countercurrent extraction process, angelica dahurica decoction pieces are inversely contacted with Extraction solvent, entire extraction process concentration
Gradient can remain at higher level, and compared with traditional conventional can extraction process, not only the consumption of solvent is few, Er Qieji
The big recovery rate for improving root of Dahurain angelica effective component, ensure that product quality, reduces entreprise cost, improve industry competition
Power；
(2) present invention is according to the physicochemical properties of angelica dahurica decoction pieces, by process optimization, retain to greatest extent in raw material it is effective at
Point, it can be widely applied in mass production.
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 angelica dahurica root dispensing granule, includes the following steps:
A, angelica root is selected, shaking weeds out except impurity, be broken into 0.5cm particle；
B, 2 times of amount water of broken angelica dahurica decoction pieces are soaked, are inputted in the continuous dynamic countercurrent extractor of 10 section pipe of stage type,
Reverse 65 DEG C of hot water Continuous Countercurrent Extraction 2h that 11 times of amounts are added, collect extracting solution, by the root of Dahurain angelica dregs of a decoction through squeezing recoverer drug dispensing
It is then exhausted from after liquid, the part medical fluid of recycling merges with extracting solution；The input speed of the broken angelica dahurica decoction pieces is 225kg/
H, the reverse flow velocity that hot water is added are 2475kg/h；
C, centrifugal filtration after the extracting solution after merging is cooled to 50 DEG C, the revolving speed of centrifugation are 2500r/min, and filtered fluid is concentrated under reduced pressure
The clear cream for being 1.04 at relative density at 65 DEG C；
D, qinghuo reagent is spray-dried, and obtains dry extract, and dry extract dry granulation obtains angelica dahurica root dispensing granule；
The technological parameter of the spray drying are as follows: 175 DEG C ~ 185 DEG C of inlet air temperature, 85 DEG C ~ 95 DEG C of leaving air temp of control.
Embodiment 2:
A kind of preparation method of angelica dahurica root dispensing granule, includes the following steps:
A, angelica root is selected, shaking weeds out except impurity, be broken into 0.5cm particle；
B, 2 times of amount water of broken angelica dahurica decoction pieces are soaked, are inputted in the continuous dynamic countercurrent extractor of 10 section pipe of stage type,
Reverse 65 DEG C of hot water Continuous Countercurrent Extraction 2h that 11 times of amounts are added, collect extracting solution, by the root of Dahurain angelica dregs of a decoction through squeezing recoverer drug dispensing
It is then exhausted from after liquid, the part medical fluid of recycling merges with extracting solution；The input speed of the broken angelica dahurica decoction pieces is 225kg/
H, the reverse flow velocity that hot water is added are 2475kg/h；
C, the revolving speed of the extracting solution centrifugal filtration after merging, centrifugation is 2500r/min, and filtrate decompression is condensed into relatively close at 65 DEG C
The clear cream that degree is 1.04；
D, qinghuo reagent is spray-dried, and obtains dry extract, and dry extract dry granulation obtains angelica dahurica root dispensing granule；
The technological parameter of the spray drying are as follows: 175 DEG C ~ 185 DEG C of inlet air temperature, 85 DEG C ~ 95 DEG C of leaving air temp of control.
Embodiment 3:
A kind of preparation method of angelica dahurica root dispensing granule, includes the following steps:
A, angelica root is selected, shake the particle for weeding out and being broken into 0.5cm except impurity；
B, by the continuous dynamic countercurrent extractor of broken angelica dahurica decoction pieces input 10 section pipe of stage type, 13 times of reverse addition is measured
65 DEG C of hot water Continuous Countercurrent Extraction 2h, collect extracting solution, be discharged the root of Dahurain angelica dregs of a decoction；The input speed of the broken angelica dahurica decoction pieces
Degree is 225kg/h, and the reverse flow velocity that hot water is added is 2925kg/h；
C, the revolving speed of centrifugal filtration after extracting solution is cooled to 50 DEG C, centrifugation is 2500r/min, and filtrate decompression is condensed into 65 DEG C of phases
The clear cream for being 1.04 to density；
D, qinghuo reagent is spray-dried, and obtains dry extract, and dry extract dry granulation obtains angelica dahurica root dispensing granule；
The technological parameter of the spray drying are as follows: 175 DEG C ~ 185 DEG C of inlet air temperature, 85 DEG C ~ 95 DEG C of leaving air temp of control.
Embodiment 4:
A kind of preparation method of angelica dahurica root dispensing granule, includes the following steps:
A, angelica root is selected, shake the particle for weeding out and being broken into 0.4cm except impurity；
B, 1 times of amount water of broken angelica dahurica decoction pieces is soaked, is inputted in the continuous dynamic countercurrent extractor of 10 section pipe of stage type,
Reverse 70 DEG C of hot water Continuous Countercurrent Extraction 1.75h that 12 times of amounts are added, collect extracting solution, by the root of Dahurain angelica dregs of a decoction through squeezing recovery section
It is then exhausted from after medical fluid, the part medical fluid of recycling merges with extracting solution；The input speed of the broken angelica dahurica decoction pieces is
250kg/h, the reverse flow velocity that hot water is added are 3000kg/h；
C, the revolving speed of centrifugal filtration after the extracting solution after merging is cooled to 55 DEG C, centrifugation is 2650r/min, and filtrate decompression is condensed into
The clear cream that relative density is 1.05 at 65 DEG C；
D, qinghuo reagent is spray-dried, and obtains dry extract, and dry extract dry granulation obtains angelica dahurica root dispensing granule；
The technological parameter of the spray drying are as follows: 175 DEG C ~ 185 DEG C of inlet air temperature, 85 DEG C ~ 95 DEG C of leaving air temp of control.
Comparative example 1:
A kind of preparation method of angelica dahurica root dispensing granule, includes the following steps:
A, angelica root is selected, shaking weeds out except impurity；
B, angelica dahurica decoction pieces are added in Chinese medicine extracting tank, with water boiling and extraction 2 times, every time plus the water of 8 times of amounts, each 1.5h are closed
And filtrate, filtration；
C, the clear cream that relative density is 1.04 when filtrate decompression is condensed into 65 DEG C；
D, qinghuo reagent is spray-dried, and obtains dry extract, and dry extract dry granulation obtains angelica dahurica root dispensing granule；
The technological parameter of the spray drying are as follows: 175 DEG C ~ 185 DEG C of inlet air temperature, 85 DEG C ~ 95 DEG C of leaving air temp of control.
The angelica dahurica root dispensing granule that embodiment and comparative example is prepared, test its paste-forming rate, Imperatorin content and
The rate of transform of Imperatorin, the results are shown in Table 1:
1 embodiment of table is compared with comparative example extraction process
| Compare item | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 |
| Paste-forming rate % | 28.1 | 27.2 | 26.5 | 28.7 | 28.0 |
| Imperatorin content % | 0.066 | 0.061 | 0.058 | 0.065 | 0.041 |
| Imperatorin rate of transform % | 8.93 | 7.99 | 7.40 | 8.98 | 5.62 |
The present invention uses continuous dynamic countercurrent extraction process it can be seen from 1 result of table, not only molten compared with conventional can extraction process
The consumption of agent is few, and the rate of transform of paste-forming rate, Imperatorin significantly improves.Being compared by embodiment 1 and embodiment 2 can be with
Find out, extracting solution cooling is handled, can be decomposed to avoid heat-sensitive ingredients, further improve the rate of transform of Imperatorin.
Claims (10)
1. a kind of preparation method of angelica dahurica root dispensing granule, which comprises the steps of:
A, angelica root is selected, shaking weeds out except impurity, be crushed；
B, broken angelica dahurica decoction pieces are inputted in continuous dynamic countercurrent extractor, it is reverse that the 12-14 times of hot water measured progress is added
Continuous dynamic countercurrent extracts 1.5-2.5h, collects extracting solution, and the root of Dahurain angelica dregs of a decoction are discharged；
C, extracting solution filters, and relative density is the clear cream of 1.02-1.05 when filtrate decompression is condensed into 65 DEG C；
D, qinghuo reagent is spray-dried, and obtains dry extract, and dry extract dry granulation obtains angelica dahurica root dispensing granule.
2. the preparation method of angelica dahurica root dispensing granule according to claim 1, which is characterized in that described broken in step a
Partial size is 0.2-0.5cm.
3. the preparation method of angelica dahurica root dispensing granule according to claim 1, which is characterized in that, will be broken in step b
Angelica dahurica decoction pieces input in continuous dynamic countercurrent extractor again after the 1-2 times of water measured wetting is first added.
4. the preparation method of angelica dahurica root dispensing granule according to claim 1, which is characterized in that in step b, the hot water
Temperature is 60-70 DEG C；The continuous dynamic countercurrent extractor is 10 section pipe of stage type.
5. the preparation method of angelica dahurica root dispensing granule according to claim 1, which is characterized in that in step b, by the root of Dahurain angelica dregs of a decoction
It is then exhausted from after squeezing recovery section medical fluid, the part medical fluid of recycling merges with extracting solution.
6. the preparation method of angelica dahurica root dispensing granule according to claim 1, which is characterized in that in step b, it is described it is broken after
The input speeds of angelica dahurica decoction pieces be 200-250kg/h, the reverse flow velocity that hot water is added is 2000-3250kg/h.
7. the preparation method of angelica dahurica root dispensing granule according to claim 1, which is characterized in that in step c, first by extracting solution
It is refiltered after being cooled to 45-55 DEG C.
8. the preparation method of angelica dahurica root dispensing granule according to claim 1, which is characterized in that in step c, the filtering is
It is filtered using centrifuge, the revolving speed of centrifugation is 2000-3000r/min.
9. the preparation method of angelica dahurica root dispensing granule according to claim 1, which is characterized in that in step c, the decompression is dense
The temperature of contracting is 55-65 DEG C.
10. the preparation method of angelica dahurica root dispensing granule according to claim 1, which is characterized in that described spraying in step d
Dry technological parameter are as follows: 175 DEG C ~ 185 DEG C of inlet air temperature, 85 DEG C ~ 95 DEG C of leaving air temp of control.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112336757A (en) * | 2020-10-20 | 2021-02-09 | 广东一方制药有限公司 | Traditional Chinese medicine formula granule containing coumarin compound and preparation method thereof |
| CN115737569A (en) * | 2022-11-17 | 2023-03-07 | 天地恒一制药股份有限公司 | Preparation method of radix angelicae formula granules |
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|---|---|---|---|---|
| CN102058641A (en) * | 2009-12-29 | 2011-05-18 | 成都中医药大学 | Angelica dahurica extract and quality detection method |
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2018
- 2018-02-06 CN CN201810119001.6A patent/CN109568359A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102058641A (en) * | 2009-12-29 | 2011-05-18 | 成都中医药大学 | Angelica dahurica extract and quality detection method |
Non-Patent Citations (1)
| Title |
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| 邢克江等: "连续逆流提取在天然药物提取中的应用开发", 《医药工程设计》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112336757A (en) * | 2020-10-20 | 2021-02-09 | 广东一方制药有限公司 | Traditional Chinese medicine formula granule containing coumarin compound and preparation method thereof |
| CN115737569A (en) * | 2022-11-17 | 2023-03-07 | 天地恒一制药股份有限公司 | Preparation method of radix angelicae formula granules |
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Application publication date: 20190405 |