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 PDF

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Publication number
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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China
Prior art keywords
cbdv
cbd
solution
extracting
ethanol
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Pending
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CN201910546070.XA
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Chinese (zh)
Inventor
张伟东
谢建瑞
詹志刚
李佳
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Yunnan Fengsheng Biotechnology Co Ltd
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Yunnan Fengsheng Biotechnology Co Ltd
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Priority to CN201910546070.XA priority Critical patent/CN110143854A/en
Publication of CN110143854A publication Critical patent/CN110143854A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C37/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
    • C07C37/004Preparation 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
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2601/00Systems containing only non-condensed rings
    • C07C2601/12Systems containing only non-condensed rings with a six-membered ring
    • C07C2601/16Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Botany (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

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

Method that is a kind of while extracting CBD and CBDV
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.
CN201910546070.XA 2019-06-23 2019-06-23 Method that is a kind of while extracting CBD and CBDV Pending CN110143854A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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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