CN109745348A - A kind of preparation method of bupleurum formulation particle - Google Patents
A kind of preparation method of bupleurum formulation particle Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of bupleurum formulation particle, comprising the following steps: (1) to dried firewood recklessly water spray infiltration, it is cut into sheet, it is dry, and obtain radix bupleuri medicine materical crude slice；(2) step (1) radix bupleuri medicine materical crude slice is added into 5-10 times of water refluxing extraction 2-3 times, collects each secondary extracting solution；(3) step (2) extracting solution is put into dual-effect concentrator and is concentrated under reduced pressure, obtain concentrate；(4) dextrin of concentrate weight 1-3% will be added in step (3) concentrate, be dried in vacuo after stirring evenly, crush, obtain dry powder；(5) it is separately added into dextrin and ethyl alcohol in step (4) dry powder, mixes, is pelletized with oscillating granulator, be sieved, drying, whole grain obtains bupleurum formulation particle.Preparation method of the present invention effectively reduces the loss of the volatilization of volatile oil and saikoside in radix bupleuri, and gained bupleurum formulation particle active principle content is high, and preparation method is simple, low in cost, has good application value.
Description
Technical field
The invention belongs to technical field of traditional Chinese medicines, and in particular to a kind of preparation method of bupleurum formulation particle.
Background technique
Radix bupleuri is bitter in taste, slightly cold, returns liver, gallbladder channel, has in inducing diaphoresis, the effect of soothing the liver rising Yang, is used for cold, fever, fever and chills
Contact, malaria, liver depression and qi stagnation, chest and rib distending pain, rectal prolapse, uterine prolapse, irregular menstruation.Radix bupleuri is extracted preparation by the prior art
It at bupleurum formulation particle, is shared with other Chinese medicinal granules, for catching a cold, the infection of the upper respiratory tract, malaria, fevers and chills alternate, costalgia, liver
Gallbladder inflammation can be used for regulating menstruation in gynaecology and not wither, rectal prolapse can be then treated in urological department.
The Chinese patent application of Publication No. CN106511925A discloses a kind of plus taste Xiao Chai Hu granules and its preparation side
Method and application should add taste Xiao Chai Hu granules, and the component including following weight percent: bupleurum Chinense volatile oil 2-10% adds the small radix bupleuri of taste
Particle extract powder 20-70%, dextrin 20-70% have the advantages that easy to carry, effective component is high, are conducive to absorb；The small radix bupleuri of taste should be added
The preparation method of particle includes: the extraction Step 1: bupleurum Chinense volatile oil, Step 2: the preparation of inclusion compound, Step 3: plus taste it is small
The preparation of bupleurum particles extract powder, Step 4: granulation, which can preferably purify small radix bupleuri drug ingedient, and make
The particle obtained is easy to carry；It should add taste Xiao Chai Hu granules can be in preparation treatment peptic ulcer, unrestrained property gastritis complication medicine
Application, further improve application range of the Xiao Chai Hu granules in taste drug.But the patent uses kinds of traditional Chinese medicines material
It prepares extract powder, higher cost, and volatile oil and extract powder to prepare using different process, processing step is cumbersome.
Notification number is that the Chinese patent of CN102349993B discloses a kind of new Xiao Chai Hu granules preparation and its preparation side
Method.The basic prescription of the invention derives from Xiao Chaihu Tang.In the preparation process of original Xiao Chaihu Tang and Xiao Chai Hu granules preparation
Basis on, related process technologies are adjusted and have been improved, so that the new Xiao Chai Hu granules preparation made is controlled
Therapeutic effect significantly improves.But the patent is decocted using simple water and carries out effective component extraction to radix bupleuri, subsequent processing is only adopted
With concentration and fluidized bed prilling, extract yield is low, and effective component is easy loss.
Summary of the invention
To overcome drawbacks described above, the purpose of the present invention is to provide a kind of preparation methods of bupleurum formulation particle.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of preparation method of bupleurum formulation particle, comprising the following steps:
(1) it sprays water recklessly to dried firewood, to consistent inside and outside moisture, softening is cut into sheet without the dry heart for infiltration, and it is dry to water content≤10%,
Obtain radix bupleuri medicine materical crude slice；
(2) step (1) radix bupleuri medicine materical crude slice is added into 5-10 times of water refluxing extraction 2-3 times, extracts 50-100min every time, collected each time and mention
Take liquid；
(3) step (2) extracting solution is put into dual-effect concentrator, in 50-60 DEG C of temperature, pressure-0.03-- 0.06MPa condition
Under be concentrated under reduced pressure into relative density 1.22-1.26g/mL, obtain concentrate；
(4) dextrin of concentrate weight 1-3% will be added in step (3) concentrate, be dried in vacuo after stirring evenly, crush, done
Powder；
60-70 DEG C of vacuum drying temperature described in step (4), pressure-0.05-- 0.08MPa, time 40-60h；
(5) dextrin of 0.6-0.9 times of dry powder weight and the second of 0.9-1.3 times of dry powder weight are separately added into step (4) dry powder
Alcohol is mixed, is pelletized with oscillating granulator, is sieved, and drying, whole grain obtains bupleurum formulation particle.
Preferably, sheet described in step (1) with a thickness of 2-5mm.
Preferably, the partial size of dry powder described in step (4) is 60-100 mesh.
Preferably, the partial size of sieving sieve described in step (5) is 16-20 mesh.
Preferably, the volumetric concentration of ethyl alcohol described in step (5) is 90-98%.
Preferably, drying temperature described in step (5) is 50-55 DEG C, time 4-6h.
Positive beneficial effect of the invention:
1. the present invention uses water refluxing extraction, wherein effective component volatile oil and saikoside are sufficiently extracted, and are then extracted
Liquid is concentrated under reduced pressure in dual-effect concentrator, in concentrate be added dextrin stir evenly after be dried in vacuo, dextrin by concentrate respectively at
It is point evenly dispersed, it is convenient for drying, significantly shortens compared with the vacuum drying time 72h in conventional method, and is concentrated under reduced pressure and vacuum
Dry temperature is lower, while dextrin has effectively included the readily volatilized ingredient such as volatile oil, reduces the loss of effective component, very
Yield >=26% of extract after sky is dry, water content≤4%, saikoside content >=4.3% in final bupleurum formulation particle contain
Water≤6.7%；When step (2) reflux is replaced with decocting method by comparative example 1 of the present invention；Comparative example 2 is by step
(4) dextrin, which omits, uses, and vacuum drying time needs 72h；The temperature that step (3) is concentrated under reduced pressure comparative example 3 is by 55 DEG C
Replace with 70 DEG C, step (4) vacuum drying temperature by 65 DEG C replace with 75 DEG C；In comparative example preparation method radix bupleuri effectively
Ingredient has loss, and extract yield (dry powder weight/dried firewood Hu Chongliang) decline is obvious, and saponin content is also bright in bupleurum formulation particle
Aobvious decline.Therefore, preparation method of the present invention effectively reduces the loss of the volatilization of volatile oil and saikoside in radix bupleuri, gained bavin
Hu granule active constituent content is high, and preparation method is simple, low in cost, has good application value.
Specific embodiment
Below with reference to some specific embodiments, the present invention is further described.
Embodiment 1
A kind of preparation method of bupleurum formulation particle, comprising the following steps:
(1) it sprays water recklessly to dried firewood, infiltration softens without the dry heart, is cut into sheet to consistent inside and outside moisture, dry to containing with a thickness of 2mm
Water≤10% obtains radix bupleuri medicine materical crude slice；
(2) step (1) radix bupleuri medicine materical crude slice is added into 6 times of water refluxing extractions 2 times, extracts 60min every time, collect each secondary extracting solution；
(3) step (2) extracting solution is put into dual-effect concentrator, is concentrated under reduced pressure under the conditions of temperature 60 C, pressure -0.03MPa
To relative density 1.22g/mL, concentrate is obtained；
(4) dextrin of concentrate weight 1.5% will be added in step (3) concentrate, be dried in vacuo after stirring evenly, crush, done
Powder, the partial size of dry powder are 60 mesh；
65 DEG C of vacuum drying temperature, pressure -0.05MPa, time 40h described in step (4)；
(5) 0.9 times of dry powder weight of dextrin and 0.9 times of dry powder weight of ethyl alcohol are separately added into step (4) dry powder, ethyl alcohol
Volumetric concentration is 90%, mixes, is pelletized with oscillating granulator, crosses 16 meshes, dries 4h under the conditions of 55 DEG C of temperature, whole grain obtains
Bupleurum formulation particle.
Embodiment 2
A kind of preparation method of bupleurum formulation particle, comprising the following steps:
(1) it sprays water recklessly to dried firewood, infiltration softens without the dry heart, is cut into sheet to consistent inside and outside moisture, dry to containing with a thickness of 3mm
Water≤10% obtains radix bupleuri medicine materical crude slice；
(2) step (1) radix bupleuri medicine materical crude slice is added into 7 times of water refluxing extractions 3 times, extracts 60min every time, collect each secondary extracting solution；
(3) step (2) extracting solution is put into dual-effect concentrator, is concentrated under reduced pressure under the conditions of 55 DEG C of temperature, pressure -0.05MPa
To relative density 1.23g/mL, concentrate is obtained；
(4) dextrin of concentrate weight 1% will be added in step (3) concentrate, be dried in vacuo after stirring evenly, crush, obtain dry powder,
The partial size of dry powder is 80 mesh；
60 DEG C of vacuum drying temperature, pressure -0.08MPa, time 45h described in step (4)；
(5) 0.6 times of dry powder weight of dextrin and 1.0 times of dry powder weight of ethyl alcohol are separately added into step (4) dry powder, ethyl alcohol
Volumetric concentration is 90%, mixes, is pelletized with oscillating granulator, crosses 18 meshes, dries 6h under the conditions of temperature 50 C, whole grain obtains
Bupleurum formulation particle.
Embodiment 3
A kind of preparation method of bupleurum formulation particle, comprising the following steps:
(1) it sprays water recklessly to dried firewood, infiltration softens without the dry heart, is cut into sheet to consistent inside and outside moisture, dry to containing with a thickness of 3mm
Water≤10% obtains radix bupleuri medicine materical crude slice；
(2) step (1) radix bupleuri medicine materical crude slice is added into 6 times of water refluxing extractions 3 times, extracts 60min every time, collect each secondary extracting solution；
(3) step (2) extracting solution is put into dual-effect concentrator, is concentrated under reduced pressure under the conditions of 55 DEG C of temperature, pressure -0.04MPa
To relative density 1.25g/mL, concentrate is obtained；
(4) dextrin of concentrate weight 2% will be added in step (3) concentrate, be dried in vacuo after stirring evenly, crush, obtain dry powder,
The partial size of dry powder is 80 mesh；
65 DEG C of vacuum drying temperature, pressure -0.06MPa, time 50h described in step (4)；
(5) 0.8 times of dry powder weight of dextrin and 1.0 times of dry powder weight of ethyl alcohol are separately added into step (4) dry powder, ethyl alcohol
Volumetric concentration is 95%, mixes, is pelletized with oscillating granulator, crosses 16 meshes, dries 5h under the conditions of temperature 50 C, whole grain obtains
Bupleurum formulation particle.
Embodiment 4
A kind of preparation method of bupleurum formulation particle, comprising the following steps:
(1) it sprays water recklessly to dried firewood, infiltration softens without the dry heart, is cut into sheet to consistent inside and outside moisture, dry to containing with a thickness of 4mm
Water≤10% obtains radix bupleuri medicine materical crude slice；
(2) step (1) radix bupleuri medicine materical crude slice is added into 8 times of water refluxing extractions 2 times, extracts 70min every time, collect each secondary extracting solution；
(3) step (2) extracting solution is put into dual-effect concentrator, is concentrated under reduced pressure under the conditions of temperature 60 C, pressure -0.06MPa
To relative density 1.24g/mL, concentrate is obtained；
(4) dextrin of concentrate weight 2% will be added in step (3) concentrate, be dried in vacuo after stirring evenly, crush, obtain dry powder,
The partial size of dry powder is 90 mesh；
65 DEG C of vacuum drying temperature, pressure -0.07MPa, time 55h described in step (4)；
(5) 0.7 times of dry powder weight of dextrin and 1.1 times of dry powder weight of ethyl alcohol are separately added into step (4) dry powder, ethyl alcohol
Volumetric concentration is 95%, mixes, is pelletized with oscillating granulator, crosses 16 meshes, dries 4h under the conditions of 55 DEG C of temperature, whole grain obtains
Bupleurum formulation particle.
Embodiment 5
A kind of preparation method of bupleurum formulation particle, comprising the following steps:
(1) it sprays water recklessly to dried firewood, infiltration softens without the dry heart, is cut into sheet to consistent inside and outside moisture, dry to containing with a thickness of 5mm
Water≤10% obtains radix bupleuri medicine materical crude slice；
(2) step (1) radix bupleuri medicine materical crude slice is added into 5 times of water refluxing extractions 3 times, extracts 50min every time, collect each secondary extracting solution；
(3) step (2) extracting solution is put into dual-effect concentrator, is concentrated under reduced pressure under the conditions of 55 DEG C of temperature, pressure -0.03MPa
To relative density 1.26g/mL, concentrate is obtained；
(4) dextrin of concentrate weight 3% will be added in step (3) concentrate, be dried in vacuo after stirring evenly, crush, obtain dry powder,
The partial size of dry powder is 100 mesh；
60 DEG C of vacuum drying temperature, pressure -0.06MPa, time 50h described in step (4)；
(5) 0.8 times of dry powder weight of dextrin and 1.2 times of dry powder weight of ethyl alcohol are separately added into step (4) dry powder, ethyl alcohol
Volumetric concentration is 98%, mixes, is pelletized with oscillating granulator, crosses 20 meshes, dries 5h under the conditions of temperature 50 C, whole grain obtains
Bupleurum formulation particle.
Embodiment 6
A kind of preparation method of bupleurum formulation particle, comprising the following steps:
(1) it sprays water recklessly to dried firewood, infiltration softens without the dry heart, is cut into sheet to consistent inside and outside moisture, dry to containing with a thickness of 4mm
Water≤10% obtains radix bupleuri medicine materical crude slice；
(2) step (1) radix bupleuri medicine materical crude slice is added into 10 times of water refluxing extractions 3 times, extracts 100min every time, collect each secondary extracting solution；
(3) step (2) extracting solution is put into dual-effect concentrator, is concentrated under reduced pressure under the conditions of temperature 50 C, pressure -0.05MPa
To relative density 1.22g/mL, concentrate is obtained；
(4) dextrin of concentrate weight 2% will be added in step (3) concentrate, be dried in vacuo after stirring evenly, crush, obtain dry powder,
The partial size of dry powder is 100 mesh；
70 DEG C of vacuum drying temperature, pressure -0.05MPa, time 60h described in step (4)；
(5) 0.8 times of dry powder weight of dextrin and 1.3 times of dry powder weight of ethyl alcohol are separately added into step (4) dry powder, ethyl alcohol
Volumetric concentration is 95%, mixes, is pelletized with oscillating granulator, crosses 16 meshes, dries 5h under the conditions of 55 DEG C of temperature, whole grain obtains
Bupleurum formulation particle.
Comparative example 1
The present embodiment is substantially the same manner as Example 3, and the same thing is not repeated, somewhat different:
A kind of preparation method of bupleurum formulation particle, comprising the following steps:
(1) it sprays water recklessly to dried firewood, infiltration softens without the dry heart, is cut into sheet to consistent inside and outside moisture, dry to containing with a thickness of 3mm
Water≤10% obtains radix bupleuri medicine materical crude slice；
(2) step (1) radix bupleuri medicine materical crude slice is added into 6 times of water boiling and extractions 3 times, extracts 60min every time, collect each secondary extracting solution；
(3) step (2) extracting solution is put into dual-effect concentrator, is concentrated under reduced pressure under the conditions of 55 DEG C of temperature, pressure -0.04MPa
To relative density 1.23g/mL, concentrate is obtained；
(4) dextrin of concentrate weight 2% will be added in step (3) concentrate, be dried in vacuo after stirring evenly, crush, obtain dry powder,
The partial size of dry powder is 80 mesh；
65 DEG C of vacuum drying temperature, pressure -0.06MPa, time 50h described in step (4)；
(5) 0.8 times of dry powder weight of dextrin and 1.0 times of dry powder weight of ethyl alcohol are separately added into step (4) dry powder, ethyl alcohol
Volumetric concentration is 95%, mixes, is pelletized with oscillating granulator, crosses 16 meshes, dries 5h under the conditions of temperature 50 C, whole grain obtains
Bupleurum formulation particle.
Comparative example 2
The present embodiment is substantially the same manner as Example 3, and the same thing is not repeated, somewhat different:
A kind of preparation method of bupleurum formulation particle, comprising the following steps:
(1) it sprays water recklessly to dried firewood, infiltration softens without the dry heart, is cut into sheet to consistent inside and outside moisture, dry to containing with a thickness of 3mm
Water≤10% obtains radix bupleuri medicine materical crude slice；
(2) step (1) radix bupleuri medicine materical crude slice is added into 6 times of water refluxing extractions 3 times, extracts 60min every time, collect each secondary extracting solution；
(3) step (2) extracting solution is put into dual-effect concentrator, is concentrated under reduced pressure under the conditions of 55 DEG C of temperature, pressure -0.04MPa
To relative density 1.23g/mL, concentrate is obtained；
(4) step (3) concentrate is dried in vacuo, is crushed, obtain dry powder, the partial size of dry powder is 80 mesh；
65 DEG C of vacuum drying temperature, pressure -0.06MPa, time 72h described in step (4)；
(5) 0.8 times of dry powder weight of dextrin and 1.0 times of dry powder weight of ethyl alcohol are separately added into step (4) dry powder, ethyl alcohol
Volumetric concentration is 95%, mixes, is pelletized with oscillating granulator, crosses 16 meshes, dries 5h under the conditions of temperature 50 C, whole grain obtains
Bupleurum formulation particle.
Comparative example 3
A kind of preparation method of bupleurum formulation particle, comprising the following steps:
(1) it sprays water recklessly to dried firewood, infiltration softens without the dry heart, is cut into sheet to consistent inside and outside moisture, dry to containing with a thickness of 3mm
Water≤10% obtains radix bupleuri medicine materical crude slice；
(2) step (1) radix bupleuri medicine materical crude slice is added into 6 times of water refluxing extractions 3 times, extracts 60min every time, collect each secondary extracting solution；
(3) step (2) extracting solution is put into dual-effect concentrator, is concentrated under reduced pressure under the conditions of temperature 70 C, pressure -0.04MPa
To relative density 1.26g/mL, concentrate is obtained；
(4) dextrin of concentrate weight 2% will be added in step (3) concentrate, be dried in vacuo after stirring evenly, crush, obtain dry powder,
The partial size of dry powder is 80 mesh；
75 DEG C of vacuum drying temperature, pressure -0.06MPa, time 50h described in step (4)；
(5) 0.8 times of dry powder weight of dextrin and 1.0 times of dry powder weight of ethyl alcohol are separately added into step (4) dry powder, ethyl alcohol
Volumetric concentration is 95%, mixes, is pelletized with oscillating granulator, crosses 16 meshes, dries 5h under the conditions of temperature 50 C, whole grain obtains
Bupleurum formulation particle.
Bupleurum formulation particle prepared by 1-6 of the embodiment of the present invention and comparative example 1-3 carries out live operation test,
Test result see the table below 1.
The test result of the bupleurum formulation particle of table 1 1-6 of the embodiment of the present invention and comparative example 1-3 preparation
As shown in Table 1, step (2) reflux is replaced with decocting method by opposite embodiment 3, comparative example 1；Comparative example 2
Step (4) dextrin is omitted and is used, vacuum drying time needs 72h；The temperature that step (3) is concentrated under reduced pressure comparative example 3
By 55 DEG C replace with 70 DEG C, step (4) vacuum drying temperature by 65 DEG C replace with 75 DEG C；Comparative example preparation method is extracted
Object yield (being expressed as dry powder weight/dried firewood Hu Chongliang roughly) decline is obvious, and effective component has loss, bupleurum formulation in radix bupleuri
Saponin content is decreased obviously in grain, and especially 2 saponin content of comparative example decline is the most obvious.
Bupleurum formulation Particulate Extract (dry powder) yield >=26% of 1-6 of embodiment of the present invention preparation, high income, radix bupleuri are matched
Saponin content >=4.3% in square particle, water content≤6.7%, active constituent content are high.
Claims (6)
1. a kind of preparation method of bupleurum formulation particle, which comprises the following steps:
(1) it sprays water recklessly to dried firewood, to consistent inside and outside moisture, softening is cut into sheet without the dry heart for infiltration, and it is dry to water content≤10%,
Obtain radix bupleuri medicine materical crude slice；
(2) step (1) radix bupleuri medicine materical crude slice is added into 5-10 times of water refluxing extraction 2-3 times, extracts 50-100min every time, collected each time and mention
Take liquid；
(3) step (2) extracting solution is put into dual-effect concentrator, in 50-60 DEG C of temperature, pressure-0.03-- 0.06MPa condition
Under be concentrated under reduced pressure into relative density 1.22-1.26g/mL, obtain concentrate；
(4) dextrin of concentrate weight 1-3% will be added in step (3) concentrate, be dried in vacuo after stirring evenly, crush, done
Powder；
60-70 DEG C of vacuum drying temperature described in step (4), pressure-0.05-- 0.08MPa, time 40-60h；
(5) dextrin of 0.6-0.9 times of dry powder weight and the second of 0.9-1.3 times of dry powder weight are separately added into step (4) dry powder
Alcohol is mixed, is pelletized with oscillating granulator, is sieved, and drying, whole grain obtains bupleurum formulation particle.
2. the preparation method of bupleurum formulation particle according to claim 1, which is characterized in that sheet described in step (1)
With a thickness of 2-5mm.
3. the preparation method of bupleurum formulation particle according to claim 1, which is characterized in that dry powder described in step (4)
Partial size be 60-100 mesh.
4. the preparation method of bupleurum formulation particle according to claim 1, which is characterized in that sieving described in step (5)
It is 16-20 mesh with the partial size of sieve.
5. the preparation method of bupleurum formulation particle according to claim 1, which is characterized in that ethyl alcohol described in step (5)
Volumetric concentration be 90-98%.
6. the preparation method of bupleurum formulation particle according to claim 1, which is characterized in that drying described in step (5)
Temperature is 50-55 DEG C, time 4-6h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116019856A (en) * | 2023-02-23 | 2023-04-28 | 河南福森药业有限公司 | New use of rhizoma corydalis pain relieving oral liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1714811A (en) * | 2004-06-30 | 2006-01-04 | 天津天士力制药股份有限公司 | Radix bupleuri dripping pill and its preparing method |
| CN106138131A (en) * | 2016-06-20 | 2016-11-23 | 广东方制药有限公司 | A kind of bupleurum particles and Chinese medicine preparation thereof |
| CN106511925A (en) * | 2016-11-10 | 2017-03-22 | 东莞市中医院 | Modified common goldenrop granules as well as preparation method and applications thereof |
| CN108619186A (en) * | 2018-07-06 | 2018-10-09 | 徐自升 | Radix bupleuri is fresh to carry spray-dried granules medicine materical crude slice |
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2019
- 2019-03-04 CN CN201910160908.1A patent/CN109745348A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1714811A (en) * | 2004-06-30 | 2006-01-04 | 天津天士力制药股份有限公司 | Radix bupleuri dripping pill and its preparing method |
| CN106138131A (en) * | 2016-06-20 | 2016-11-23 | 广东方制药有限公司 | A kind of bupleurum particles and Chinese medicine preparation thereof |
| CN106511925A (en) * | 2016-11-10 | 2017-03-22 | 东莞市中医院 | Modified common goldenrop granules as well as preparation method and applications thereof |
| CN108619186A (en) * | 2018-07-06 | 2018-10-09 | 徐自升 | Radix bupleuri is fresh to carry spray-dried granules medicine materical crude slice |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116019856A (en) * | 2023-02-23 | 2023-04-28 | 河南福森药业有限公司 | New use of rhizoma corydalis pain relieving oral liquid |
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Application publication date: 20190514 |