CN110143854A - Method that is a kind of while extracting CBD and CBDV - Google Patents
Method that is a kind of while extracting CBD and CBDV Download PDFInfo
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- CN110143854A CN110143854A CN201910546070.XA CN201910546070A CN110143854A CN 110143854 A CN110143854 A CN 110143854A CN 201910546070 A CN201910546070 A CN 201910546070A CN 110143854 A CN110143854 A CN 110143854A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/004—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by obtaining phenols from plant material or from animal material
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/16—Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated
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Abstract
The invention discloses a kind of methods for extracting CBD and CBDV simultaneously, it is to be prepared using the leaf of industrial hemp as raw material that the method for CBD and CBDV is extracted while described, specifically includes the following steps: selection industrial hemp fresh leaf, after chopping in oxygen content be 50~80% oxygen-enriched environment under place 12~obtain material a for 24 hours;The water content of material a is regulated to 10~20% and obtains material b;It extracts the organic solvent that 3~5 times of material b volume is added in material b to obtain extracting solution c;Extracting solution c is respectively obtained into object CBD and CBDV using gradient solution crystallization.The treatment process that the present invention passes through the pre-treatment of oxygen-enriched environment, it crystallizes in conjunction with subsequent gradient solution, with the ethanol-water solution gradient crystallization of volume proportion 0:1~1:0, first crystallizes out CBDV, it is subsequent again to crystallize out CBD, and the purity of CBD and CBDV can reach 99.2% or more.
Description
Technical field
The invention belongs to chemical technology fields, and in particular to a method of CBD and CBDV are extracted simultaneously.
Background technique
Hemp (scientific name: Cannabis sativa L.) Cannabaceae, Cannabis plant, You Mingma, Chinese fiber crops, fire fiber crops, mountain silk
Seedling, second fiber crops, have important agricultural and medical value.It can be made one in hemp containing a kind of toxic component tetrahydrocannabinol (THC)
Unreal habituation is caused, drugs can be done, was once forbidden cultivating within suitable long-term.Since the economy of hemp, medical value are high, specialize in industrial
The raw material hemp on way is referred to as " industrial hemp ", and THC content does not have extraction poison less than 3/1000ths in growth period marihuana
Property ingredient THC value or sucked directly as drugs, can legal progress large-scale planting and industrialized developing utilize.Mesh
Before, people have isolated more than 500 from hemp plant and have planted substance, CBD, big wherein in cannabinol compounds at least 86
Numb terpene phenol (CBG) can influence lipid and glycometabolism, and CBDV has preferable antiepileptic activity, while again research shows that CBDV can subtract
Light nausea helps to treat gastrointestinal problems;But current extraction process is not able to satisfy the market demand, therefore develops a kind of energy
The extracting method for solving above-mentioned technical problem is very important.
Summary of the invention
The purpose of the present invention is to provide a kind of methods for extracting CBD and CBDV simultaneously.
The object of the present invention is achieved like this, and the method that CBD and CBDV is extracted while described is with industrial hemp
Leaf is prepared as raw material, specifically includes the following steps:
1) select industrial hemp fresh leaf, after chopping in oxygen content be 50~80% oxygen-enriched environment under place 12~for 24 hours
Obtain material a;
2) water content of material a is regulated to 10~20% and obtains material b;
3) it extracts the organic solvent that 3~5 times of material b volume is added in material b to obtain extracting solution c;
4) extracting solution c is respectively obtained into object CBD and CBDV using gradient solution crystallization.
The present invention is crystallized in conjunction with subsequent gradient solution, is matched with volume by the treatment process of the pre-treatment of oxygen-enriched environment
Ethanol-water solution gradient crystallization than 0:1~1:0, first crystallizes out CBDV, subsequent again to crystallize out CBD, and CBD and
The purity of CBDV can reach 99.2% or more.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated, but the present invention is limited in any way,
Based on present invention teach that it is made it is any transform or replace, all belong to the scope of protection of the present invention.
It is to be prepared using the leaf of industrial hemp as raw material that the method for CBD and CBDV is extracted while of the present invention,
Specifically includes the following steps:
1) select industrial hemp fresh leaf, after chopping in oxygen content be 50~80% oxygen-enriched environment under place 12~for 24 hours
Obtain material a;
2) water content of material a is regulated to 10~20% and obtains material b;
3) it extracts the organic solvent that 3~5 times of material b volume is added in material b to obtain extracting solution c;
4) extracting solution c is respectively obtained into object CBD and CBDV using gradient solution crystallization.
The chopping is that primary industry hemp fresh leaf is cut into (0.5~1) cm × (0.5~1) cm size.
The organic solvent is ethyl alcohol, chloroform, carbon tetrachloride or petroleum ether.
The organic solvent is ethanol solution.
The concentration expressed in percentage by volume of the ethanol solution is 20%~90%.
The concentration expressed in percentage by volume of the ethanol solution is 50~80%.
The gradient solution crystallization is the ethanol-water solution using volume proportion 0:1~1:0 in 20~30 DEG C of items of temperature
Extracting solution c is crystallized under part.
The volume proportion of the ethanol-water solution is 0:1,2:3,1:2,3:7,2:1 and 1:0.
The crystallization that the volume proportion of ethanol-water solution obtains when being 0:1 to 3:7 gradient step is CBDV;
The crystallization that the volume proportion of ethanol-water solution obtains when being 3:7 to 1:0 gradient step is CBD.
Embodiment 1
Industrial hemp fresh leaf is selected, is chopped into after 0.5cm × 0.5cm size in oxygen content as under 50% oxygen-enriched environment
Placement obtains material a for 24 hours;The water content of material a is regulated to 10% and obtains material b;5 times of material b volume will be added in material b
It is concentration expressed in percentage by volume is that 80% ethanol solution extracts to obtain extracting solution c;By extracting solution c using gradient solution crystallization point
Object CBD and CBDV are not obtained.The volume proportion of ethanol-water solution be 0:1 to 3:7 gradient step when obtained crystallization
For CBDV;The crystallization obtained when the volume proportion of ethanol-water solution is 3:7 to 1:0 gradient step is CBD;The present embodiment
The purity that the purity for the CBD being prepared is 99.7%, CBDV is 99.5%.
Embodiment 2
Industrial hemp fresh leaf is selected, being chopped into after 1cm × 1cm size in oxygen content is to place under 80% oxygen-enriched environment
12h obtains material a;The water content of material a is regulated to 20% and obtains material b;It is by 3 times of material b volume is added in material b
Concentration expressed in percentage by volume is that 50% ethanol solution extracts to obtain extracting solution c;Extracting solution c is crystallized using gradient solution and is obtained respectively
To object CBD and CBDV.The crystallization obtained when the volume proportion of ethanol-water solution is 0:1 to 3:7 gradient step is
CBDV;The crystallization obtained when the volume proportion of ethanol-water solution is 3:7 to 1:0 gradient step is CBD;The present embodiment system
The purity that the purity of standby obtained CBD is 99.3%, CBDV is 99.2%.
Embodiment 3
Industrial hemp fresh leaf is selected, is transferred after being chopped into 0.5cm × 1cm size in the oxygen-enriched environment that oxygen content is 70%
It sets 20h and obtains material a;The water content of material a is regulated to 15% and obtains material b;4 times of material b volume will be added in material b
It is that chloroform extracts to obtain extracting solution c for concentration expressed in percentage by volume;Extracting solution c is respectively obtained into target using gradient solution crystallization
Object CBD and CBDV.The crystallization obtained when the volume proportion of ethanol-water solution is 0:1 to 3:7 gradient step is CBDV;?
The crystallization that the volume proportion of ethanol-water solution obtains when being 3:7 to 1:0 gradient step is CBD;What the present embodiment was prepared
The purity that the purity of CBD is 99.8%, CBDV is 99.4%.
Claims (10)
1. a kind of method for extracting CBD and CBDV simultaneously, it is characterized in that: the method that CBD and CBDV is extracted while described be with
The leaf of industrial hemp is prepared as raw material, specifically includes the following steps:
1) select industrial hemp fresh leaf, after chopping in oxygen content be 50~80% oxygen-enriched environment under place 12~obtain for 24 hours
Material a;
2) water content of material a is regulated to 10~20% and obtains material b;
3) it extracts the organic solvent that 3~5 times of material b volume is added in material b to obtain extracting solution c;
4) extracting solution c is respectively obtained into object CBD and CBDV using gradient solution crystallization.
2. method that is according to claim 1 while extracting CBD and CBDV, it is characterized in that: the chopping is by raw material
Industrial hemp fresh leaf is cut into (0.5~1) cm × (0.5~1) cm size.
3. method that is according to claim 1 while extracting CBD and CBDV, it is characterized in that: the organic solvent is second
Alcohol, chloroform, carbon tetrachloride or petroleum ether.
4. method that is according to claim 1 or 3 while extracting CBD and CBDV, it is characterized in that: the organic solvent is
Ethanol solution.
5. method that is according to claim 4 while extracting CBD and CBDV, it is characterized in that: the body of the ethanol solution
Product percentage concentration is 20%~90%.
6. method that is according to claim 5 while extracting CBD and CBDV, it is characterized in that: the body of the ethanol solution
Product percentage concentration is 50~80%.
7. method that is according to claim 1 while extracting CBD and CBDV, it is characterized in that: the gradient solution crystallizes
It is to be crystallized under the conditions of 20~30 DEG C of temperature to extracting solution c using the ethanol-water solution of volume proportion 0:1~1:0.
8. method that is according to claim 7 while extracting CBD and CBDV, it is characterized in that: the ethanol-water solution
Volume proportion is 0:1,2:3,1:2,3:7,2:1 and 1:0.
9. method that is according to claim 8 while extracting CBD and CBDV, it is characterized in that: the volume of ethanol-water solution is matched
The crystallization obtained when than for 0:1 to 3:7 gradient step is CBDV.
10. method that is according to claim 8 while extracting CBD and CBDV, it is characterized in that: the volume of ethanol-water solution
The crystallization that proportion obtains when being 3:7 to 1:0 gradient step is CBD.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN115385780A (en) * | 2022-08-26 | 2022-11-25 | 晨光生物科技集团股份有限公司 | Sub-cannabidiol crystal polymorphic substance as well as preparation method and application thereof |
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CN106831353A (en) * | 2016-08-16 | 2017-06-13 | 云南汉素生物科技有限公司 | A kind of method that cannabidiol is extracted from hemp |
US20170349518A1 (en) * | 2016-06-01 | 2017-12-07 | Daniel Dickman | Crystalline Form of Cannabidiol |
CN108083989A (en) * | 2018-01-10 | 2018-05-29 | 烟台汉麻生物技术有限公司 | A kind of preparation method of high-purity cannabidiol |
CN109574810A (en) * | 2017-09-29 | 2019-04-05 | 汉义生物科技(北京)有限公司 | Method that is a kind of while extracting CBD and CBDV |
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- 2019-06-23 CN CN201910546070.XA patent/CN110143854A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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US20170349518A1 (en) * | 2016-06-01 | 2017-12-07 | Daniel Dickman | Crystalline Form of Cannabidiol |
CN106831353A (en) * | 2016-08-16 | 2017-06-13 | 云南汉素生物科技有限公司 | A kind of method that cannabidiol is extracted from hemp |
CN109574810A (en) * | 2017-09-29 | 2019-04-05 | 汉义生物科技(北京)有限公司 | Method that is a kind of while extracting CBD and CBDV |
CN108083989A (en) * | 2018-01-10 | 2018-05-29 | 烟台汉麻生物技术有限公司 | A kind of preparation method of high-purity cannabidiol |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN115385780A (en) * | 2022-08-26 | 2022-11-25 | 晨光生物科技集团股份有限公司 | Sub-cannabidiol crystal polymorphic substance as well as preparation method and application thereof |
CN115385780B (en) * | 2022-08-26 | 2024-02-27 | 晨光生物科技集团股份有限公司 | Secondary cannabidiol crystal polymorph and preparation method and application thereof |
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