CN105481872B - A kind of method of constant temperature gradient series connection extraction active components of plants - Google Patents
A kind of method of constant temperature gradient series connection extraction active components of plants Download PDFInfo
- Publication number
- CN105481872B CN105481872B CN201510858904.2A CN201510858904A CN105481872B CN 105481872 B CN105481872 B CN 105481872B CN 201510858904 A CN201510858904 A CN 201510858904A CN 105481872 B CN105481872 B CN 105481872B
- Authority
- CN
- China
- Prior art keywords
- extraction
- extractor
- series connection
- extract solution
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/02—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains two hetero rings
- C07D493/04—Ortho-condensed systems
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G99/00—Subject matter not provided for in other groups of this subclass
Abstract
A kind of method of constant temperature gradient series connection extraction active components of plants, it is to take 35 extractors series connection, by plant material by being respectively implanted after tank number decile in each extractor；Extractant is added in the first extractor, heating and thermal insulation extracts, the extract solution of the first extractor is drawn into the second extractor as Extraction solvent again, it is heated to previous extraction temperature, insulation extraction same time, the rest may be inferred, until last extractor is incubated extraction same time, obtained extract solution centrifugal filtration under foregoing extraction temperature；Then extractant repeatedly series connection extraction 12 times, obtained extract solution centrifugal filtration under foregoing extraction temperature by preceding method is added in the material residue of the first extractor, merges the filtrate of each time.It is in this way, of the invention by extraction equipment in Conventional solvents extraction method（Extractor）Series connection, extraction raw material is more, and extractor number is more, and recovery rate is higher；Reagent at least 30 50% is saved than traditional solvent extraction method, the workload at least 30% of subsequent processing concentration and recovery can be mitigated.
Description
Technical field
The present invention relates to a kind of method that active component is extracted from plant, is carried more particularly, to a kind of series connection of constant temperature gradient
The method for taking active components of plants.
Background technology
Solvent extraction method is most basic, most widely used method in plant extract active component technology, and it is according to plant
The property of various active ingredient solubility in thing, a kind of extraction that required active component is dissolved out out of medicinal material tissue
Method.This method equipment production cost is low, and technology is very ripe, most commonly water extraction and organic solvent extraction.Such as Publication No.
CN101190258 application be it is a kind of from yulan leaf and/spend it is middle extraction rich in parithenolide total sesquiterpene lactone class chemical combination
The method of thing, it is first to be soaked with deionized water, then is extracted with lower alcohol multi-reflow.For another example Publication No. CN103524520A
Patent is by Magnoliacea plant material dry, crushed, carbon dioxide supercritical extraction.But single tank in solvent extraction method production
Raw material repeatedly puts into reagent respectively, and reagent consumption is big in heating for multiple times, extraction time, heat time length, takes equipment time length,
Low production efficiency.
The content of the invention
The technical problems to be solved by the invention are：For above-mentioned the deficiencies in the prior art, there is provided a kind of constant temperature gradient string
Connection extraction active components of plants method, using extractor connect method, at a certain temperature extract solution repeatedly utilize, gradient
Extraction, to improve extraction efficiency, reduce production cost.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：A kind of constant temperature gradient series connection extraction is planted
The method of thing active component, this method are to take 3-5 extractor series connection, and the plant material for being intended to be extracted is by tank number decile
After be respectively implanted in each extractor, add extractant in the first extractor, heating and thermal insulation extraction, then proposing the first extractor
Take liquid to be drawn into the second extractor and be used as Extraction solvent, be heated to previous Extracting temperature（Extraction temperature in first extractor）
Insulation extraction same time（Extraction time in first extractor）, the extract solution of the second extractor is then drawn into the 3rd and carried
Take and Extraction solvent is used as in tank, be heated to previous Extracting temperature（Extraction temperature in second extractor）Insulation extraction same time
（Extraction time in second extractor）, the rest may be inferred, until last extractor more than an extractor extract solution in
Previous Extracting temperature（Extraction temperature in a upper extractor）Lower insulation extraction same time（Extraction in a upper extractor
Time）, obtained extract solution centrifugal filtration；Then extractant is added in the material residue of the first extractor by preceding method foregoing
Extracting temperature and repeatedly series connection extraction 1-2 times, obtained extract solution centrifugal filtration under extraction time, merge the filtrate of each time.Its
In, the above-mentioned filtering referred to is using tripodia centrifugation cloth bag 200 mesh filtering.
Such as, active component parithenolide is extracted from wide yulan fresh leaf：It is first to be beaten wide yulan fresh leaf to crush, by 1g
Leaf slurry plus 2mL volumetric concentrations are the ratio of 80%-95% polarity organic reagent, and polarity organic reagent, normal temperature are added in leaf slurry
Lower cold soaking steeps 12-24h, then carries out decile by series can number, is added separately in each series can, standby；Wherein, polarity is organic
Reagent is methanol, ethanol or amylalcohol.The extractant added in the wide yulan fresh leaf slurry or material residue of first extractor is 80%-95% bodies
Methanol, ethanol or the amylalcohol of product concentration, the addition of the extractant is to add 8ml extractants by the wide yulan fresh leaf slurry/material residues of 1g
Ratio adds, and Extracting temperature is 65-70 DEG C, extraction time 20-30min.
Or, green tea polyphenols is extracted from green tea：After green tea is aliquoted into extractor, in green tea/material residue of the first extractor
The extractant of addition is deionized water, and deionized water adds the ratio of 8ml deionized waters to add in 1g green tea/material residue, Extracting temperature
For 85 DEG C -90 DEG C, extraction time 45-50min.
In actual production, material residue can carry out 4-5 times and repeat to extract, and after 2-3 times repeats to extract, can be carried first
Take the material residue in tank to be replaced by new raw material, using the second extractor as initial extraction tank, add new extractant, extract successively, now,
Extraction order is changed into the second extractor and extracted at first, and successively up to last extractor, and the first extractor finally extracts.Press
Same principle changes raw material, extractant and extraction order, can be carried out continuously production.
Extractor is series under constant temperature by the present invention to be extracted, and the tank connected is more（It can be the extraction of more than 3
Tank is connected, but must not be less than 3）, extracting times are more, and gradient is incremented by the concentration of active ingredient step by step in extract solution, finally makes
The concentration of active ingredient reaches highest level in extract solution.Compared with the traditional handicraft that each tank extracts respectively, equivalent is being used
In the case of extractant, extraction efficiency can be effectively improved, and continuous production is good, subsequent concentration, evaporate recycling design
Efficiency will also improve, and can effectively reduce production cost.Active component can be also effectively improved in plant by this method in extract solution
In concentration, simplify subsequent purification difficulty so that the higher production of purity need not can be obtained using complicated procedures of forming in subsequent technique
Product.
In this way, the constant temperature gradient series connection of the present invention is extracted extraction equipment in Conventional solvents extraction method（Extractor）Series connection,
Extraction raw material is more, and extractor number is more, and recovery rate is higher；Reagent at least 30-50% is saved than traditional solvent extraction method, can be subtracted
The workload at least 30% of light subsequent processing concentration and recovery.
Embodiment
Embodiment 1 extracts parithenolide from wide yulan fresh leaf
4 extractor series connection are taken, the wide yulan fresh leaf mashing of 50kg is weighed and crushes, leaf slurry is divided into 4 parts, every part of 12.5kg,
It is respectively placed in the methanol that 25L volumetric concentrations are 90%, cold soaking steeps 20h under normal temperature.Leaf slurry after 4 parts of cold soaking bubbles is put respectively
In 4 extractors, the methanol that 100L volumetric concentrations are 90% is added in the first extractor, 65-70 DEG C is heated up to and keeps
The temperature, the extract solution that the first extractor is extracted after 30min are used as extractant into the second extractor, heated in the second extractor
To 65-70 DEG C and the temperature is kept, the extract solution that the second extractor is extracted after 30min is used as extractant into the 3rd extractor,
65-70 DEG C is heated up in 3rd extractor and keeps the temperature, the extract solution that the 3rd extractor is extracted after 30min extracts to the 4th
Extractant is used as in tank, 65-70 DEG C is heated up in the 4th extractor and keeps temperature 30min, obtained extract solution is through tripodia
Centrifuge Bag filter（200 mesh）；The methanol that 100L volumetric concentrations are 90% is added in remaining material residue in the first extractor,
It is heated up to 65-70 DEG C and keeps the temperature, the extract solution that the first extractor is extracted after 30min is used as extraction into the second extractor
Agent, 65-70 DEG C being heated up in the second extractor and keeps the temperature, the extract solution of the second extractor is extracted after 30min to the 3rd
Extractant is used as in extractor, 65-70 DEG C is heated up in the 3rd extractor and keeps the temperature, the 3rd extraction is extracted after 30min
The extract solution of tank is used as Extraction solvent into the 4th extractor, and 65-70 DEG C is heated up in the 4th extractor and keeps the temperature
30min, obtained extract solution centrifuge Bag filter through tripodia（200 mesh）, merge 2 filtrates.Filtrate is returned through vacuum-concentrcted
Methanol is received, carries out subsequent handling by prior art, parithenolide content is 95.1% to last products obtained therefrom after testing.
Comparison example 1
By the mixed solvent for extracting water-soluble portion, again with methanol and water from wide yulan fresh leaf using deionized water at present
The method for extracting parithenolide crude product is carried out.The wide yulan fresh leaf deciles of 50kg, loaded on 4 extraction do not connected list tanks
In, parithenolide is extracted from wide yulan fresh leaf using this 4 single tanks of extraction, is showed after extraction and by same as Example 1
There is technology to carry out subsequent handling, products obtained therefrom parithenolide content is 81.3%.Than the series connection extraction method of the application, deionization
Water multi-purpose 30%, Extraction solvent multi-purpose 30%, concentration and recovery workload is high by more than 30%.
Embodiment 2 extracts green tea polyphenols from green tea
3 extractor series connection are taken, 300kg green tea materials are divided into 3 equal portions（100kg/ parts）, this 3 strings are dosed into respectively
Join in extractor.800kg deionized waters are heated to 85 DEG C, are extracted into the first extractor and are used as extractant, in 85 DEG C of extractions
45min；The extract solution of first extractor is extracted into the second extractor as extractant, is heated to previous 85 DEG C of guarantors of Extracting temperature
Temperature extraction 45min, the extract solution of the second extractor is extracted into the 3rd tank extractor, is heated to 85 DEG C, insulation, at such a temperature
45min is extracted, obtained extract solution centrifuges Bag filter through tripodia（200 mesh）.Then 1g is pressed in the material residue of the first extractor
Material residue adds the ratio of 8ml deionized waters to add deionized water, in 85 DEG C of insulation extraction 45min, by the extract solution of the first extractor
It is drawn into the second extractor and is used as extractant, the is extracted into 85 DEG C of insulation extraction 45min, then by the extract solution of the second extractor
Extractant, 85 DEG C of insulation extraction 45min are used as in three extractors, obtained extract solution centrifuges Bag filter through tripodia（200 mesh）.
Then the ratio for adding 8ml deionized waters in 1g material residues in the material residue of the first extractor adds deionized water, by preceding method
Extracted again, obtained extract solution centrifuges the mesh of cloth bag 200 through tripodia and filtered, and merges 3 filtrates, is carried out by prior art
Subsequent handling.The raw material leaching rate of this method is 32%, and Tea Polyphenols detection level extracts solvent up to 43%（Deionized water）It is no more than
2000kg reaches 3% with regard to that can reach extraction effect, extract solution solid content.
Comparison example 2
The water extraction technology mainly used by current green tea polyphenols is carried out.By 300kg green tea materials trisections, respectively loaded on 3
In the individual extraction list tank do not connected, the ratio of 8ml deionized waters is added to be separately added into deionized water extraction 3 in each tank in 1g raw materials
It is secondary, 85 DEG C of Extracting temperature, each 45-60 minutes.Extract solution centrifugal filtration, merging filtrate, by existing skill same as Example 2
Art carries out subsequent handling, and for extract solution solid content below 1.8%, raw material leaching rate is 24%, and detection polyphenol content is
33%.The deionized water of addition need to all be heated to 85 DEG C from normal temperature, and energy resource consumption is too many, relative to this method, deionized water consumption
More 30% is at least wanted, concentration and recovery workload also increases by more than 30%.
Claims (4)
- A kind of 1. method of constant temperature gradient series connection extraction active components of plants, it is characterised in that this method is to take 3-5 extractor Series connection, the plant material for being intended to be extracted are respectively implanted in each extractor by tank number decile；Added in the first extractor Extractant, heating and thermal insulation extraction, then the extract solution of the first extractor is drawn into the second extractor as Extraction solvent, heating To previous extraction temperature, insulation extraction same time, the rest may be inferred, until last extractor is protected under foregoing extraction temperature Temperature extraction same time, obtained extract solution centrifugal filtration；Then extractant is added in the material residue of the first extractor by foregoing Method repeats series connection extraction 1-2 times, obtained extract solution centrifugal filtration, the filtrate that merging is each time under foregoing extraction temperature；Wherein, above-mentioned plant material is wide yulan fresh leaf, and active component is parithenolide, the extraction added in the first extractor Agent is methanol, ethanol or the amylalcohol of 80%-95% volumetric concentrations, and extractant adds 8ml extractants by the wide yulan fresh leaf slurry/material residues of 1g Ratio add, Extracting temperature be 65-70 DEG C, extraction time 20-30min.
- 2. the method for a kind of constant temperature gradient series connection extraction active components of plants as claimed in claim 1, it is characterised in that described Wide yulan fresh leaf is inserted in extractor again after being handled as follows：The mashing of wide yulan fresh leaf is broken, by 1g leaves slurry plus 2mL volumes Concentration is the ratio of 80%-95% polarity organic reagent, and polarity organic reagent is added in leaf slurry, and cold soaking steeps 12- under normal temperature 24h。
- 3. the method for a kind of constant temperature gradient series connection extraction active components of plants as claimed in claim 2, it is characterised in that described Polarity organic reagent is methanol, ethanol or amylalcohol.
- 4. the method for a kind of constant temperature gradient series connection extraction active components of plants as claimed in claim 1, it is characterised in that described Filtering is using tripodia centrifugation cloth bag 200 mesh filtering.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510858904.2A CN105481872B (en) | 2015-12-01 | 2015-12-01 | A kind of method of constant temperature gradient series connection extraction active components of plants |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510858904.2A CN105481872B (en) | 2015-12-01 | 2015-12-01 | A kind of method of constant temperature gradient series connection extraction active components of plants |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105481872A CN105481872A (en) | 2016-04-13 |
| CN105481872B true CN105481872B (en) | 2018-01-09 |
Family
ID=55669186
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510858904.2A Active CN105481872B (en) | 2015-12-01 | 2015-12-01 | A kind of method of constant temperature gradient series connection extraction active components of plants |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105481872B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109609277A (en) * | 2019-01-24 | 2019-04-12 | 河北省农林科学院经济作物研究所 | A kind of continuous extracting device and technique |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1472932B1 (en) * | 2002-02-05 | 2008-04-23 | Kao Corporation | Process for producing green tea polyphenol |
| US20060222722A1 (en) * | 2005-03-30 | 2006-10-05 | Roberts Stephen C | Sublingual methods of treatment to alleviate or prevent arthritis |
| US20110117070A1 (en) * | 2005-04-19 | 2011-05-19 | Aurora Sheena K | Compositions and methods for treating headache |
| CN101190258A (en) * | 2007-05-30 | 2008-06-04 | 北京星昊医药股份有限公司 | Total sesquiterpene lactone extract containing rich parthenolide and preparation method and application thereof |
| CN102863452B (en) * | 2011-07-06 | 2015-05-20 | 天津尚德药缘科技有限公司 | Method for preparing parthenolide originated from magnolia delavayi, magnolia liliiflora and magnolia denudate |
| CN103170157A (en) * | 2013-03-07 | 2013-06-26 | 康宝莱蕾硕（湖南）天然产物有限公司 | Continuous countercurrent extraction technology, and extraction tanks and extraction system thereof |
| CN103920305B (en) * | 2014-04-23 | 2015-12-02 | 柳秦桥 | A kind of method of pot group type counter-flow extraction Chinese caterpillar fungus |
| CN103999975A (en) * | 2014-05-22 | 2014-08-27 | 青海阿如拉藏医药研究开发有限公司 | Preparation method for instant Tibetan tea |
-
2015
- 2015-12-01 CN CN201510858904.2A patent/CN105481872B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN105481872A (en) | 2016-04-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104231281B (en) | A kind of method extracting separation gutta-percha | |
| CN102219810B (en) | Process method for preparing high-purity tannin from walnut green husk | |
| CN102002089B (en) | Process for extracting tea saponin from tea seed cakes or meal | |
| CN102100875B (en) | Process method for microwave assistant supercritical extraction of active ingredients of curcuma | |
| CN106993789B (en) | Method for extracting high-quality propolis by using subcritical multi-component mixed solvent | |
| CN101914097A (en) | Technological method for extracting caffeine and tea polyphenol mixture from tea step by step | |
| CN101524138B (en) | Preparation process for extracting active ingredient of natural plant by supersonic | |
| CN102876456A (en) | Method for extracting volatile oil and alkaloid from pepper by using subcritical fluid | |
| CN105062686A (en) | Method for extracting lavender essential oil | |
| CN102228503B (en) | Green and environment-friendly extraction method and applications of peanut shell polyphenol | |
| CN105602719B (en) | A kind of supercritical extraction method of tea oil | |
| CN102716190A (en) | Extraction method for pomiferin G/H and morusin of cortex mori radicis | |
| CN101560150B (en) | Method for extracting shikimic acid from aniseed | |
| CN100451030C (en) | Process of preparing ganoderma tricterpinyl acid and ganoderma polyose from ganoderma | |
| CN102617693A (en) | Method and device utilizing subcritical water extraction technology to extract and prepare ursolic acid from loquat leaves | |
| CN105481872B (en) | A kind of method of constant temperature gradient series connection extraction active components of plants | |
| CN104771930B (en) | The Subcritical Water Extraction agent of polyphenols and extracting process in a kind of lotus solid waste | |
| CN104193711A (en) | New method for extracting apigenin from celery | |
| CN102389510A (en) | Dioscorea nipponica Makino saponin extraction method | |
| CN105330670A (en) | Method for continuously efficiently extracting parthenolide from southern magnolia leaves | |
| CN102060858B (en) | Method for simultaneously extracting chlorophyll and protein from red clover processing waste water | |
| CN109096353A (en) | A kind of method that continuous phase transistion extracts aurantiamarin and pectin in citrus young fruit | |
| CN104231282A (en) | Method for extracting and separating eucommia seed oil and eucommia gum from eucommia samaras | |
| CN103432205A (en) | Novel method for extracting high-purity lotus leaf flavone | |
| CN103110678A (en) | Method for preparing saponin |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20180411 Address after: 415500 No. 1 Middle School Road, Lixian County, Hunan province. Patentee after: Hunan GuanYuan Biotechnology Co., Ltd. Address before: 410001 No. 1, international enterprise center, 188 environmental protection road, Yuhua District, Hunan, Changsha A301 Patentee before: Liu Hanyi |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20210514 Address after: Room 505, 5th floor, building B, Hunan Jindan science and technology venture building, 1 XIONGTIAN Road, Longping hi tech park, Furong district, Changsha City, Hunan Province, 410000 Patentee after: Changsha Huirui Bio-technology Co.,Ltd. Address before: 415500 No.1, Zhongxue Road, Guanyuan wharf neighborhood committee, Guanyuan Township, Li County, Hunan Province Patentee before: HUNAN GUANYUAN BIOTECHNOLOGY Co.,Ltd. |