CN108836986A - Debubbling method is concentrated in ilex pubescens extracting solution - Google Patents
Debubbling method is concentrated in ilex pubescens extracting solution Download PDFInfo
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- CN108836986A CN108836986A CN201810823701.3A CN201810823701A CN108836986A CN 108836986 A CN108836986 A CN 108836986A CN 201810823701 A CN201810823701 A CN 201810823701A CN 108836986 A CN108836986 A CN 108836986A
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- ilex pubescens
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- extracting solution
- mixed fatty
- fatty glycerides
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- 235000003365 Ilex pubescens Nutrition 0.000 title claims abstract description 67
- 241001100932 Ilex pubescens Species 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000000284 extract Substances 0.000 claims abstract description 38
- 125000005456 glyceride group Chemical group 0.000 claims abstract description 31
- 238000000605 extraction Methods 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 17
- 239000006286 aqueous extract Substances 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 230000008018 melting Effects 0.000 claims abstract description 3
- 238000002844 melting Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 239000000463 material Substances 0.000 claims description 22
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- 235000011187 glycerol Nutrition 0.000 claims 1
- 150000002314 glycerols Chemical class 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000006260 foam Substances 0.000 abstract description 5
- 239000003814 drug Substances 0.000 abstract description 3
- 238000000825 ultraviolet detection Methods 0.000 description 5
- 238000001291 vacuum drying Methods 0.000 description 5
- 238000007711 solidification Methods 0.000 description 4
- 230000008023 solidification Effects 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 241000209035 Ilex Species 0.000 description 3
- 235000003325 Ilex Nutrition 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000001397 quillaja saponaria molina bark Substances 0.000 description 2
- 229930182490 saponin Natural products 0.000 description 2
- 150000007949 saponins Chemical class 0.000 description 2
- 208000010445 Chilblains Diseases 0.000 description 1
- 206010008528 Chillblains Diseases 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- 206010053615 Thermal burn Diseases 0.000 description 1
- 206010043540 Thromboangiitis obliterans Diseases 0.000 description 1
- 206010000269 abscess Diseases 0.000 description 1
- 235000010358 acesulfame potassium Nutrition 0.000 description 1
- 206010000891 acute myocardial infarction Diseases 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 229930182486 flavonoid glycoside Natural products 0.000 description 1
- 150000007955 flavonoid glycosides Chemical class 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
Classifications
-
- 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)
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
- B01D19/0404—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- 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
- 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
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
Landscapes
- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Botany (AREA)
- Microbiology (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Toxicology (AREA)
- Medical Informatics (AREA)
- Medicinal Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mycology (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to technical field of extraction of Chinese traditional medicine, are specifically related to a kind of ilex pubescens extracting solution concentration debubbling method.Specifically mixed fatty glycerides will be added in Aqueous extracts, carries out being heated to mixed fatty glycerides melting completely；Acquired solution is carried out ilex pubescens medicinal extract is concentrated under reduced pressure to obtain；Ilex pubescens medicinal extract is let cool, and is removed by filtration mixed fatty glycerides, and low temperature drying obtains Ilex pubescens extract.The present invention can effectively eliminate foam when being concentrated under reduced pressure, save the production time, improve the yield of Ilex pubescens extract, reduce production cost by the way that a certain proportion of mixed fatty glycerides are added.
Description
Technical field
The invention belongs to technical field of extraction of Chinese traditional medicine, are specifically related to a kind of ilex pubescens extracting solution concentration debubbling method.
Background technique
Ilex pubescens extract is that the one kind extracted from the root of holly plant ilex pubescens contains flavonoid glycoside, saponin(e, phenols
Etc. the extract of a variety of chemical components, there is the effects of clearing heat and detoxicating, promoting blood circulation and removing obstruction in channels.It is used clinically for treatment anemopyretic cold,
Lung heat cough and asthma, abscess of throat；Coronary arteriosclerotic cardiopathy, acute myocardial infarction AMI, Buerger's disease；External curing
Burn and scald, pernio etc..With the extensive use of Ilex pubescens extract clinically, the demand of Ilex pubescens extract also increasingly increases
It is more.
China's ilex pubescens resource is very rich, and medical value is big, and therefore, research and development extract from RADIX ILICIS PUBESCENTIS and obtain hair
Ilex extract carries out purifies and separates, the method for preparation, not only contributes to sufficiently and reasonably increase and produce using ilex pubescens resource
The added value of product, and for realizing the modernization of Chinese medicine, it realizes that tcm product goes to the world and has very important significance.
About the extraction of Ilex pubescens extract, mostly with water mention with alcohol extracting based on, due to ethyl alcohol extract there are security protection with
The disadvantages of at high cost.For this purpose, most domestic manufacturing enterprise is all using water as Extraction solvent.
Contain saponin component in RADIX ILICIS PUBESCENTIS, when Aqueous extracts are concentrated, a large amount of foam, foam after decompression can be generated
Can be more serious, cause feed liquid to be lost, yield reduces.For this phenomenon, the method for reducing vacuum degree is mostly used to reduce foam,
But thickening efficiency reduces after reducing vacuum degree, increases concentration time, increases cost.
Summary of the invention
The purpose of the present invention is overcome the deficiencies of the prior art and provide a kind of ilex pubescens extracting solution concentration debubbling method.It should
Method has the advantages that security performance is high, environmentally friendly, at low cost, simple process, while saving the production time, improves ilex pubescens
The yield of extract, reduces production cost.
Debubbling method is concentrated in ilex pubescens extracting solution of the present invention, specifically includes following steps：
(1) mixed fatty glycerides will be added in Aqueous extracts, carries out being heated to mixed fatty glycerides melting completely；
(2) step (1) acquired solution is carried out that ilex pubescens medicinal extract is concentrated under reduced pressure to obtain；
(3) ilex pubescens medicinal extract is let cool, and is removed by filtration mixed fatty glycerides, and low temperature drying obtains Ilex pubescens extract.
Wherein：
The quality that mixed fatty glycerides are added described in step (1) accounts for the 0.1%-0.5% of Aqueous extracts quality.
Aqueous extracts described in step (1) are that ilex pubescens medicinal material is taken to add water to cook twice, and decocting amount of water for the first time is hair
10 times of Chinese ilex quality of medicinal material, extraction time are 4 hours, and it is 8 times of ilex pubescens quality of medicinal material that second, which decocts amount of water, is extracted
Time 2 h, extraction terminate, combined extract, obtain ilex pubescens Aqueous extracts.
Mixed fatty glycerides described in step (1) are that 34 type mixed fatty glycerides, 36 type fatty acid mixeds are sweet
One of grease or 38 type mixed fatty glycerides.
When reduced pressure described in step (2), vacuum degree is -0.07Mpa, and temperature is 50-80 DEG C, is concentrated into relatively close
Degree is 1.1-1.15.
Filtering described in step (3) is to be removed by filtration mixed fatty glycerides with the stainless steel filtering net of 100-200 mesh.
Low temperature drying temperature described in step (3) is 50-80 DEG C, and drying is to loss on drying less than 1.0%.
Mixed fatty glycerides are not soluble in water and density ratio water is small, under heated condition, swim in the surface of water, form one
The uniform film of layer, hinders bubble formation, to solve blistering and slug phenomenon.
Compared with prior art, the present invention having the advantages that：
(1) present invention can effectively be disappeared by the way that a certain proportion of mixed fatty glycerides are added when being concentrated under reduced pressure
Foam-expelling saves the production time, improves the yield of Ilex pubescens extract, reduces production cost.
(2) ilex pubescens extracting solution of the present invention concentration debubbling method has that security performance is high, environmentally friendly, at low cost, work
The advantages that skill is simple.
Specific embodiment
The invention will be further described with reference to embodiments.
Embodiment 1
It takes ilex pubescens medicinal material 200g to add water to cook twice, decocts 10 times that amount of water is ilex pubescens quality of medicinal material for the first time,
Extraction time is 4 hours, and it is 8 times of ilex pubescens quality of medicinal material that second, which decocts amount of water, and extraction time 2 hours, extraction terminated,
Combined extract obtains extracting solution 2500ml.Extracting solution is concentrated under reduced pressure after 0.1%36 type mixed fatty glycerides are added,
Temperature is 55 DEG C, vacuum degree -0.07MPa, and being concentrated into relative density is 1.11, used time 4.5h.Ilex pubescens medicinal extract let cool after with 120
Mesh filter screen filters out the mixed fatty glycerides of solidification, and low-temperature vacuum drying is carried out at 55 DEG C, and drying to loss on drying is less than
1.0%, Ilex pubescens extract 23g is obtained, UV detection, content 31.5% are carried out.The concentration process does not have blistering and slug existing
As.
Embodiment 2
It takes ilex pubescens medicinal material 200g to add water to cook twice, decocts 10 times that amount of water is ilex pubescens quality of medicinal material for the first time,
Extraction time is 4 hours, and it is 8 times of ilex pubescens quality of medicinal material that second, which decocts amount of water, and extraction time 2 hours, extraction terminated,
Combined extract obtains extracting solution 2500ml.Extracting solution is concentrated under reduced pressure after 0.2%36 type mixed fatty glycerides are added,
Vacuum degree -0.07MPa, temperature are 60 DEG C, and being concentrated into relative density is 1.11, used time 4.3h.Ilex pubescens medicinal extract let cool after with 120
Mesh filter screen filters out the mixed fatty glycerides of solidification, and low-temperature vacuum drying is carried out at 60 DEG C, and drying to loss on drying is less than
1.0%, Ilex pubescens extract 22.5g is obtained, UV detection, content 30.7% are carried out.The concentration process does not have blistering and slug
Phenomenon.
Embodiment 3
It takes ilex pubescens medicinal material 200g to add water to cook twice, decocts 10 times that amount of water is ilex pubescens quality of medicinal material for the first time,
Extraction time is 4 hours, and it is 8 times of ilex pubescens quality of medicinal material that second, which decocts amount of water, and extraction time 2 hours, extraction terminated,
Combined extract obtains extracting solution 2500ml.Extracting solution is concentrated under reduced pressure after 0.2%38 type mixed fatty glycerides are added,
Vacuum degree -0.07MPa, temperature are 70 DEG C, and being concentrated into relative density is 1.11, used time 4.7h.Ilex pubescens medicinal extract let cool after with 120
Mesh filter screen filters out the mixed fatty glycerides of solidification, and low-temperature vacuum drying is carried out at 70 DEG C, and drying to loss on drying is less than
1.0%, Ilex pubescens extract 25g is obtained, UV detection, content 32.2% are carried out.The concentration process does not have blistering and slug existing
As.
Embodiment 4
It takes ilex pubescens medicinal material 30kg to add water to cook twice, decocts 10 times that amount of water is ilex pubescens quality of medicinal material for the first time,
Extraction time is 4 hours, and it is 8 times of ilex pubescens quality of medicinal material that second, which decocts amount of water, and extraction time 2 hours, extraction terminated,
Combined extract obtains extracting solution 370L.Extracting solution is concentrated under reduced pressure after 0.3%34 type mixed fatty glycerides are added, very
Reciprocal of duty cycle -0.07MPa, temperature are 80 DEG C, and being concentrated into relative density is 1.12, used time 32h.Ilex pubescens medicinal extract let cool after with 120 mesh
Strainer filters out the mixed fatty glycerides of solidification, and low-temperature vacuum drying is carried out at 80 DEG C, and drying to loss on drying is less than
1.0%, Ilex pubescens extract 3.6kg is obtained, UV detection, content 29.95% are carried out.The concentration process does not have blistering and slug
Phenomenon.
Comparative example 1
It takes ilex pubescens medicinal material 200g to add water to cook twice, decocts 10 times that amount of water is ilex pubescens quality of medicinal material for the first time,
Extraction time is 4 hours, and it is 8 times of ilex pubescens quality of medicinal material that second, which decocts amount of water, and extraction time 2 hours, extraction terminated,
Combined extract obtains extracting solution 2500ml.Extracting solution is directly concentrated under reduced pressure, vacuum degree -0.07MPa, and blistering is serious, has been had
Bubble and slug phenomenon, being concentrated into relative density is 1.11, used time 4.2h.Ilex pubescens medicinal extract puts low-temperature vacuum drying and obtains ilex pubescens
Extract 13g carries out UV detection, content 30.3%.
Through the comparison of embodiment 1 and comparative example 1 it is found that in the case where not adding fatty glyceride, when concentration, material
Liquid forms foam, is taken away by vacuum, and loss is big, and yield is low, and this point is confirmed from the rewinding amount of Ilex pubescens extract, right
The rewinding amount of ilex pubescens is about the half in embodiment 1 in ratio 1.
Claims (7)
1. debubbling method is concentrated in a kind of ilex pubescens extracting solution, it is characterised in that：Specifically include following steps：
(1) mixed fatty glycerides will be added in Aqueous extracts, carries out being heated to mixed fatty glycerides melting completely；
(2) step (1) acquired solution is carried out that ilex pubescens medicinal extract is concentrated under reduced pressure to obtain；
(3) ilex pubescens medicinal extract is let cool, and is removed by filtration mixed fatty glycerides, and low temperature drying obtains Ilex pubescens extract.
2. debubbling method is concentrated in ilex pubescens extracting solution according to claim 1, it is characterised in that：Described in step (1)
The quality that mixed fatty glycerides are added accounts for the 0.1%-0.5% of Aqueous extracts quality.
3. debubbling method is concentrated in ilex pubescens extracting solution according to claim 1, it is characterised in that：Described in step (1)
Aqueous extracts are that ilex pubescens medicinal material is taken to add water to cook twice, decoct 10 times that amount of water is ilex pubescens quality of medicinal material for the first time, extract
Time is 4 hours, and it is 8 times of ilex pubescens quality of medicinal material that second, which decocts amount of water, and extraction time 2 hours, extraction terminated, and merged
Extracting solution obtains ilex pubescens Aqueous extracts.
4. debubbling method is concentrated in ilex pubescens extracting solution according to claim 1, it is characterised in that：It is mixed described in step (1)
Closing fatty glyceride is 34 type mixed fatty glycerides, 36 type mixed fatty glycerides or 38 type mixing-in fat acid glycerols
One of ester.
5. debubbling method is concentrated in ilex pubescens extracting solution according to claim 1, it is characterised in that：Described in step (2)
When reduced pressure, vacuum degree is -0.07Mpa, and temperature is 50-80 DEG C, and being concentrated into relative density is 1.1-1.15.
6. debubbling method is concentrated in ilex pubescens extracting solution according to claim 1, it is characterised in that：Described in step (3)
Filtering is to be removed by filtration mixed fatty glycerides with the stainless steel filtering net of 100-200 mesh.
7. debubbling method is concentrated in ilex pubescens extracting solution according to claim 1, it is characterised in that：Described in step (3)
Low temperature drying temperature is 50-80 DEG C, and drying is to loss on drying less than 1.0%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810823701.3A CN108836986A (en) | 2018-07-25 | 2018-07-25 | Debubbling method is concentrated in ilex pubescens extracting solution |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810823701.3A CN108836986A (en) | 2018-07-25 | 2018-07-25 | Debubbling method is concentrated in ilex pubescens extracting solution |
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| CN108836986A true CN108836986A (en) | 2018-11-20 |
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| CN201810823701.3A Pending CN108836986A (en) | 2018-07-25 | 2018-07-25 | Debubbling method is concentrated in ilex pubescens extracting solution |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112870376A (en) * | 2021-01-27 | 2021-06-01 | 上海硕方医药科技有限公司 | Traditional Chinese medicine extracting solution concentrating and defoaming method and application thereof |
Citations (2)
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|---|---|---|---|---|
| CN1686362A (en) * | 2005-03-28 | 2005-10-26 | 北京正大绿洲医药科技有限公司 | Hairy holly root drip pill and its preparation method |
| CN102351924A (en) * | 2011-09-05 | 2012-02-15 | 江南大学 | Condensation method of tea saponin extract |
-
2018
- 2018-07-25 CN CN201810823701.3A patent/CN108836986A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1686362A (en) * | 2005-03-28 | 2005-10-26 | 北京正大绿洲医药科技有限公司 | Hairy holly root drip pill and its preparation method |
| CN102351924A (en) * | 2011-09-05 | 2012-02-15 | 江南大学 | Condensation method of tea saponin extract |
Non-Patent Citations (3)
| Title |
|---|
| 侯海云: "《表面活性剂物理化学基础》", 31 August 2014, 西安交通大学出版社 * |
| 张媛: "《中药制剂技术》", 31 August 2012, 河南科学技术出版社 * |
| 杨红梅等: "毛冬青溶液的制备及质量标准研究 ", 《中国药房》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112870376A (en) * | 2021-01-27 | 2021-06-01 | 上海硕方医药科技有限公司 | Traditional Chinese medicine extracting solution concentrating and defoaming method and application thereof |
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